CN107955682B - Environment-friendly synthetic lubricating oil and preparation method thereof - Google Patents

Environment-friendly synthetic lubricating oil and preparation method thereof Download PDF

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Publication number
CN107955682B
CN107955682B CN201711288263.7A CN201711288263A CN107955682B CN 107955682 B CN107955682 B CN 107955682B CN 201711288263 A CN201711288263 A CN 201711288263A CN 107955682 B CN107955682 B CN 107955682B
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lubricating oil
environment
mixture
preparation
synthetic lubricating
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CN107955682A (en
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张连耕
张语
于盈盈
钟景熙
刘建秀
张讯
侯艳丽
段志军
钟读永
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XI'AN PETROLEUM DAJIARUN INDUSTRIAL Co.,Ltd.
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Xi'an Petroleum Dajiarun Industrial 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
    • C10M169/044Mixtures of base-materials and additives the additives being a mixture of non-macromolecular and macromolecular compounds
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    • C10M2201/00Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/14Inorganic compounds or elements as ingredients in lubricant compositions inorganic compounds surface treated with organic compounds
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    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2207/00Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/02Hydroxy compounds
    • C10M2207/023Hydroxy compounds having hydroxy groups bound to carbon atoms of six-membered aromatic rings
    • C10M2207/026Hydroxy compounds having hydroxy groups bound to carbon atoms of six-membered aromatic rings with tertiary alkyl groups
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    • C10M2207/00Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
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    • C10M2207/283Esters of polyhydroxy compounds
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    • C10M2207/00Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/28Esters
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    • C10M2207/289Partial esters containing free hydroxy groups
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    • C10M2209/00Organic macromolecular compounds containing oxygen as ingredients in lubricant compositions
    • C10M2209/02Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • C10M2209/08Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds containing monomers having an unsaturated radical bound to a carboxyl radical, e.g. acrylate type
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    • C10M2209/00Organic macromolecular compounds containing oxygen as ingredients in lubricant compositions
    • C10M2209/10Macromolecular compoundss obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • C10M2209/103Polyethers, i.e. containing di- or higher polyoxyalkylene groups
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    • C10M2209/00Organic macromolecular compounds containing oxygen as ingredients in lubricant compositions
    • C10M2209/10Macromolecular compoundss obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • C10M2209/103Polyethers, i.e. containing di- or higher polyoxyalkylene groups
    • C10M2209/108Polyethers, i.e. containing di- or higher polyoxyalkylene groups etherified
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    • C10M2215/00Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
    • C10M2215/08Amides
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    • C10M2215/086Imides
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    • C10M2217/00Organic macromolecular compounds containing nitrogen as ingredients in lubricant compositions
    • C10M2217/02Macromolecular compounds obtained from nitrogen containing monomers by reactions only involving carbon-to-carbon unsaturated bonds
    • C10M2217/022Macromolecular compounds obtained from nitrogen containing monomers by reactions only involving carbon-to-carbon unsaturated bonds containing monomers having an unsaturated radical bound to an amino group
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    • C10M2219/00Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions
    • C10M2219/04Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions containing sulfur-to-oxygen bonds, i.e. sulfones, sulfoxides
    • C10M2219/044Sulfonic acids, Derivatives thereof, e.g. neutral salts
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    • C10M2219/00Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions
    • C10M2219/08Thiols; Sulfides; Polysulfides; Mercaptals
    • C10M2219/082Thiols; Sulfides; Polysulfides; Mercaptals containing sulfur atoms bound to acyclic or cycloaliphatic carbon atoms
    • C10M2219/084Thiols; Sulfides; Polysulfides; Mercaptals containing sulfur atoms bound to acyclic or cycloaliphatic carbon atoms containing hydroxy groups; Derivatives thereof
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    • C10M2223/00Organic non-macromolecular compounds containing phosphorus as ingredients in lubricant compositions
    • C10M2223/06Organic non-macromolecular compounds containing phosphorus as ingredients in lubricant compositions having phosphorus-to-carbon bonds
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    • C10M2229/00Organic macromolecular compounds containing atoms of elements not provided for in groups C10M2205/00, C10M2209/00, C10M2213/00, C10M2217/00, C10M2221/00 or C10M2225/00 as ingredients in lubricant compositions
    • C10M2229/04Siloxanes with specific structure
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    • 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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    • C10N2030/00Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
    • C10N2030/64Environmental friendly compositions

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

Abstract

The invention discloses a preparation method of environment-friendly synthetic lubricating oil, which comprises the steps of preparing methyl methacrylate-4-vinylaniline copolymer, adding the copolymer solution prepared in the step 1) into polyether epoxy co-modified silicone oil, stirring and reacting for 5-6 hours at 70-80 ℃, then adding carboxylated fullerene, continuing to stir and react for 3-4 hours, then adding antioxidant and dispersant, stirring into a uniform mixture through a mechanical stirrer, then treating the mixture through a three-roller machine for three times, and finally transferring the mixture treated through the three-roller machine into a vacuum degassing device to remove air so as to obtain the environment-friendly synthetic lubricating oil; the invention also discloses the environment-friendly synthetic lubricating oil prepared by the preparation method; the environment-friendly synthetic lubricating oil disclosed by the invention is excellent in extrusion performance and lubricating performance, green and environment-friendly, and has excellent viscosity-temperature performance and low-temperature performance.

Description

Environment-friendly synthetic lubricating oil and preparation method thereof
Technical Field
The invention relates to the technical field of lubricating oil, in particular to environment-friendly synthetic lubricating oil and a preparation method thereof.
Background
With the acceleration of global industrialization process, environmental problems and energy problems become more prominent and become one of the main factors restricting social progress and economic development. The environment-friendly synthetic lubricating oil is one of a plurality of environment-friendly novel materials, is green and pollution-free, can relieve the problem of mineral energy shortage, is widely applied to industries such as aviation, machining, metallurgy, automobiles, transportation, coal and the like, and can effectively slow down the friction and wear of mechanical parts and reduce the energy loss, thereby stabilizing the working state of the mechanical parts and prolonging the service life of the mechanical parts.
The common lubricating oil in the market at present has no outstanding effect on the aspects of wear resistance and oxidation resistance, the common lubricating oil with better effect is generally added with fluoride, the fluoride has certain pollution to the environment, and a product which has good protection effect on mechanical parts, is environment-friendly and has long service life is lacked. The price of high-quality lubricating oil on the market is expensive, most of the lubricating oil has single effect, the using effect is not ideal, and the oil change period can not meet the basic requirements of mechanical parts such as engines.
The synthetic oil has well-arranged molecules and naturally strong ability to resist external variables, so the physique is better, and the capacities of heat stability, oxidation resistance and viscosity change resistance are naturally stronger than those of mineral oil and semi-synthetic oil.
Therefore, there is a need for an environmentally friendly synthetic lubricating oil with good lubricating effect and low price.
Disclosure of Invention
The invention mainly aims to provide the environment-friendly synthetic lubricating oil and the preparation method thereof. Has the advantages of good lubricating effect, multiple functions, good effect, wide application range and good stability.
In order to achieve the above purposes, the technical scheme adopted by the invention is as follows: a preparation method of environment-friendly synthetic lubricating oil comprises the following steps:
1) preparation of the copolymer: mixing methyl methacrylate, 4-vinylaniline and an emulsifier, putting the mixture into a radiation field in the atmosphere of nitrogen or inert gas, and radiating the mixture by adopting a cobalt 60-gamma radiation method for 40-50 minutes;
2) preparation of lubricating oil: adding the copolymer solution prepared in the step 1) into polyether epoxy co-modified silicone oil, stirring and reacting for 5-6 hours at 70-80 ℃, then adding the carboxylated fullerene, continuing stirring and reacting for 3-4 hours, then adding the antioxidant and the dispersant, stirring the mixture into a uniform mixture through a mechanical stirrer, then treating the mixture through a three-roller machine for three times, and finally transferring the mixture treated through the three-roller machine into a vacuum-pumping degassing device to remove air, thereby obtaining the environment-friendly synthetic lubricating oil.
Wherein the mass ratio of the methyl methacrylate to the 4-vinylaniline to the emulsifier in the step 1) is 3: 5: (0.1-0.2);
the emulsifier is selected from sodium dodecyl benzene sulfonate, polyoxypropylene polyethylene glycerol ether and nonylphenol polyoxyethylene ether;
the inert gas is selected from one or more of helium, argon and neon;
the mass ratio of the copolymer, the polyether epoxy co-modified silicone oil, the carboxylated fullerene, the antioxidant and the dispersant in the step 2) is 2: 1: (0.1-0.2): (0.05-0.07): (0.05-0.07);
the dispersing agent is one or more than two of triethyl hexyl phosphoric acid, vinyl distearamide, stearic acid monoglyceride, polyethylene glycol and mono-alkenyl succinimide in any proportion;
the antioxidant is one or more than two of 2, 6-tertiary butyl-4-methylphenol, bis (3, 5-tertiary butyl-4-hydroxyphenyl) thioether, tetra [ beta- (3, 5-tertiary butyl-4-hydroxyphenyl) propionic acid ] pentaerythritol ester, didodecanol ester, dimyristyl alcohol ester and dioctadecyl alcohol ester in any proportion;
an environment-friendly synthetic lubricating oil which is prepared by adopting the preparation method of the environment-friendly synthetic lubricating oil.
Due to the application of the technical scheme, compared with the prior art, the invention has the following advantages:
(1) the environment-friendly synthetic lubricating oil designed by the invention has the advantages of easily available raw materials, lower price than that of the lubricating oil in the prior art, simple and feasible preparation method and low requirement on equipment.
(2) The environment-friendly synthetic lubricating oil designed by the invention does not contain components harmful to the environment in preparation and structure, and is environment-friendly.
(3) The environment-friendly synthetic lubricating oil designed by the invention has the excellent characteristics of polyethylene, organosilicon and polyether synthetic lubricating oil, and has excellent viscosity-temperature performance and low-temperature performance. Good lubricating effect, excellent film-forming property and extreme pressure property and good stability.
(4) The environment-friendly synthetic lubricating oil designed by the invention has the advantages that the molecular chain structure contains the fullerene structure, the lubricating performance is greatly improved, the fullerene and the polymer are tightly bonded, the phase separation cannot occur, and the fullerene is uniformly dispersed.
(5) The environment-friendly synthetic lubricating oil designed by the invention does not contain halogen, acid, alkali and other components which cause corrosion to mechanical parts, and is beneficial to improving the corrosion resistance.
Detailed Description
The following description is presented to disclose the invention so as to enable any person skilled in the art to practice the invention. The preferred embodiments in the following description are given by way of example only, and other obvious variations will occur to those skilled in the art.
In the embodiment, the polyether epoxy co-modified silicone oil is DY-ETE301 polyether epoxy co-modified silicone oil which is purchased from Shandong Dai chemical industry Co., Ltd; carboxylated fullerenes were purchased from Nanjing Xiancheng nanomaterial science and technology Co., Ltd; other raw materials were purchased from the national pharmaceutical group chemical agents limited.
Example 1
A preparation method of environment-friendly synthetic lubricating oil comprises the following steps:
1) preparation of the copolymer: mixing 30g of methyl methacrylate, 50g of 4-vinylaniline and 1g of sodium dodecyl benzene sulfonate, putting the mixture into a radiation field in a nitrogen atmosphere, and radiating the mixture by adopting a cobalt 60-gamma radiation method for 40 minutes;
2) preparation of lubricating oil: adding 40g of the copolymer prepared in the step 1) into 20g of polyether epoxy co-modified silicone oil, stirring and reacting for 5 hours at 70 ℃, then adding 2g of carboxylated fullerene, continuing stirring and reacting for 3 hours, then adding 1g of 2, 6-tertiary butyl-4-methylphenol and 1g of triethylhexylphosphoric acid, stirring the mixture into a uniform mixture through a mechanical stirrer, then treating the mixture through a three-roller machine for three times, and finally transferring the mixture treated through the three-roller machine into a vacuum pumping and degassing device to remove air so as to obtain the environment-friendly synthetic lubricating oil.
An environment-friendly synthetic lubricating oil which is prepared by adopting the preparation method of the environment-friendly synthetic lubricating oil.
Example 2
A preparation method of environment-friendly synthetic lubricating oil comprises the following steps:
1) preparation of the copolymer: mixing 30g of methyl methacrylate, 50g of 4-vinylaniline and 1.2g of polyoxypropylene polyethylene glycerol ether, placing the mixture in a radiation field under the argon atmosphere, and radiating the mixture by adopting a cobalt 60-gamma radiation method for 43 minutes;
2) preparation of lubricating oil: adding 40g of the copolymer prepared in the step 1) into 20g of polyether epoxy co-modified silicone oil, stirring and reacting for 5.3 hours at 73 ℃, then adding 3g of carboxylated fullerene, continuing to stir and react for 3.3 hours, then adding 1.1g of bis (3, 5-tertiary butyl-4-hydroxyphenyl) sulfide and 1g of vinyl bis stearamide, stirring into a uniform mixture through a mechanical stirrer, then treating the mixture through a three-roller machine for three times, and finally transferring the mixture treated through the three-roller machine into a vacuum pumping and degassing device to remove air so as to obtain the environment-friendly synthetic lubricating oil.
An environment-friendly synthetic lubricating oil which is prepared by adopting the preparation method of the environment-friendly synthetic lubricating oil.
Example 3
A preparation method of environment-friendly synthetic lubricating oil comprises the following steps:
1) preparation of the copolymer: mixing 30g of methyl methacrylate, 50g of 4-vinylaniline and 1.5g of nonylphenol polyoxyethylene ether, placing the mixture in a radiation field in a neon atmosphere, and radiating the mixture by adopting a cobalt 60-gamma radiation method for 45 minutes;
2) preparation of lubricating oil: adding 40g of the copolymer prepared in the step 1) into 20g of polyether epoxy co-modified silicone oil, stirring and reacting for 5.7 hours at 77 ℃, then adding 3.2g of carboxylated fullerene, continuing to stir and react for 3.6 hours, then adding 1.3g of docosanol ester and 1.2g of glycerol monostearate, stirring the mixture into a uniform mixture through a mechanical stirrer, then treating the mixture through a three-roller machine for three times, and finally transferring the mixture treated through the three-roller machine into a vacuumizing and degassing device to remove air so as to obtain the environment-friendly synthetic lubricating oil.
An environment-friendly synthetic lubricating oil which is prepared by adopting the preparation method of the environment-friendly synthetic lubricating oil.
Example 4
A preparation method of environment-friendly synthetic lubricating oil comprises the following steps:
1) preparation of the copolymer: mixing 30g of methyl methacrylate, 50g of 4-vinylaniline and 1.8g of sodium dodecyl benzene sulfonate, putting the mixture into a radiation field in a nitrogen atmosphere, and radiating the mixture by adopting a cobalt 60-gamma radiation method for 48 minutes;
2) preparation of lubricating oil: adding 40g of the copolymer prepared in the step 1) into 20g of polyether epoxy co-modified silicone oil, stirring and reacting for 6 hours at 78 ℃, then adding 3.8g of carboxylated fullerene, continuing stirring and reacting for 4 hours, then adding 1.4g of ditetradecanol and 1.3g of polyethylene glycol, stirring into a uniform mixture through a mechanical stirrer, then treating the mixture through a three-roller machine for three times, and finally transferring the mixture treated through the three-roller machine into a vacuum-pumping degassing device to remove air so as to obtain the environment-friendly synthetic lubricating oil.
An environment-friendly synthetic lubricating oil which is prepared by adopting the preparation method of the environment-friendly synthetic lubricating oil.
Example 5
A preparation method of environment-friendly synthetic lubricating oil comprises the following steps:
1) preparation of the copolymer: mixing 30g of methyl methacrylate, 50g of 4-vinylaniline and 2g of polyoxypropylene polyethylene glycerol ether, putting the mixture into a radiation field in a nitrogen atmosphere, and radiating the mixture by adopting a cobalt 60-gamma radiation method for 50 minutes;
2) preparation of lubricating oil: adding 40g of the copolymer prepared in the step 1) into 20g of polyether epoxy co-modified silicone oil, stirring and reacting for 6 hours at 80 ℃, then adding 4g of carboxylated fullerene, continuing stirring and reacting for 4 hours, then adding 1.4g of dioctadecyl carbonate and 1.4g of monoalkenyl succinimide, stirring into a uniform mixture through a mechanical stirrer, then treating the mixture through a three-roll machine for three times, and finally transferring the mixture treated through the three-roll machine into a vacuum-pumping degassing device to remove air so as to obtain the environment-friendly synthetic lubricating oil.
An environment-friendly synthetic lubricating oil which is prepared by adopting the preparation method of the environment-friendly synthetic lubricating oil.
Comparative example
The common lubricating grease in China is purchased from Wuxi Purun science and technology Limited.
The samples obtained in the above examples 1 to 5 and comparative example were subjected to the relevant performance tests, the test results are shown in table 1, the test methods are as follows,
(1) four-ball experiment: testing according to ASTM D-2783; in the test results of the four-ball experiment, the maximum non-seizure load PB value indicates the maximum load of the steel ball without seizure in a lubricating state at a certain temperature and a certain rotating speed, and the higher the PB value is, the better the lubricating performance of the lubricating oil is. The sintering load PD value indicates that the load is increased step by step, the upper steel ball and the lower steel ball are sintered at high temperature due to the overlarge load, the equipment has to stop running, and the higher the PD value is, the better the extreme pressure lubricating performance of the lubricating oil is. The value d of the wear scar diameter represents the size of the wear scar diameter of the bearing steel spherical surface caused by friction, and the smaller the value d is, the better the anti-wear capability and lubricity of the lubricating oil is.
(2) Kinematic viscosity: testing according to GB/T265;
(3) pour point: testing according to GB/T3535-2006;
TABLE 1 Properties of samples of examples and comparative examples
Figure RE-GDA0001543340480000051
Figure RE-GDA0001543340480000061
As can be seen from the above table, the multifunctional lubricating oil disclosed in the embodiment of the invention has the maximum non-seizing load (PB) of 72-94N (kg), the sintering load (PD) of 135-160N (kg), the diameter d of the wear scar of 0.30-0.15mm, and the kinematic viscosity at 40 ℃ of 34-42mm2The lubricating oil has the advantages that the lubricating oil has a pour point of-35 to-25 ℃, and the maximum non-seizure load (PB) of the conventional lubricating oil sold in the market is 60N (kg), the sintering load (PD) is 130N (kg), the diameter of a wear scar is 0.4mm, the kinematic viscosity at 40 ℃ is 75mm2/s, and the pour point is-21 ℃, so that the multifunctional lubricating oil disclosed by the embodiment of the invention has good extreme pressure performance and lubricating performance.
The foregoing shows and describes the general principles, essential features, and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are merely illustrative of the principles of the invention, but that various changes and modifications may be made without departing from the spirit and scope of the invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.

Claims (6)

1. The preparation method of the environment-friendly synthetic lubricating oil is characterized by comprising the following steps:
1) preparation of the copolymer: mixing methyl methacrylate, 4-vinylaniline and an emulsifier, placing the mixture in a radiation field in an inert gas atmosphere, and radiating the mixture by adopting a cobalt 60-gamma radiation method for 40-50 minutes;
2) preparation of lubricating oil: adding the copolymer prepared in the step 1) into polyether epoxy co-modified silicone oil, stirring and reacting for 5-6 hours at 70-80 ℃, then adding carboxylated fullerene, continuing stirring and reacting for 3-4 hours, then adding an antioxidant and a dispersing agent, stirring the mixture into a uniform mixture through a mechanical stirrer, then treating the mixture through a three-roller machine for three times, and finally transferring the mixture treated through the three-roller machine into a vacuum-pumping degassing device to remove air to obtain the environment-friendly synthetic lubricating oil;
wherein the mass ratio of the methyl methacrylate to the 4-vinylaniline to the emulsifier in the step 1) is 3: 5: (0.1-0.2);
the mass ratio of the copolymer, the polyether epoxy co-modified silicone oil, the carboxylated fullerene, the antioxidant and the dispersant in the step 2) is 2: 1: (0.1-0.2): (0.05-0.07): (0.05-0.07).
2. The method of claim 1, wherein the emulsifier is selected from sodium dodecylbenzenesulfonate, polyoxypropylene polyethylene glycol glyceryl ether, and nonylphenol polyoxyethylene ether.
3. The method of claim 1, wherein the inert gas is selected from helium, argon, neon, or a combination thereof.
4. The method of claim 1, wherein the dispersant is one or more selected from the group consisting of triethylhexylphosphoric acid, vinyldistearamide, glyceryl monostearate, polyethylene glycol, and monoalkenylbutyldiimide at any ratio.
5. The method of claim 1, wherein the antioxidant is one or more selected from the group consisting of 2, 6-tertiary butyl-4-methylphenol, bis (3, 5-tertiary butyl-4-hydroxyphenyl) sulfide, pentaerythrityl tetrakis [ β - (3, 5-tertiary butyl-4-hydroxyphenyl) propionate ], behenyl ester, lignoceryl ester, and distearyl ester.
6. An environment-friendly synthetic lubricating oil, which is characterized by being prepared by the preparation method of the environment-friendly synthetic lubricating oil according to any one of claims 1 to 5.
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