CN112662450A - High-wear-resistance lubricating oil and preparation method thereof - Google Patents
High-wear-resistance lubricating oil and preparation method thereof Download PDFInfo
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Abstract
The invention discloses high-wear-resistance lubricating oil which is characterized by being prepared from the following components in parts by weight: 3-5 parts of benzotriazole-1-oxyl tris (dimethylamino) phosphonium hexafluorophosphate, 4-8 parts of modified boron nitride nanotube silicon nitride nanowire compound, 8-12 parts of fluorine-containing N, N' -thiodiglycolamidate/polyethylene glycol dicarboxylic acid polycondensate, 70-80 parts of base oil, 0.8-1.2 parts of a viscosity agent, 0.5-1 part of a dispersing agent and 1-2 parts of an antioxidant. The invention also discloses a preparation method of the high-wear-resistance lubricating oil. The high-wear-resistance lubricating oil disclosed by the invention has the advantages of obvious lubricating effect, good wear-resisting property, strong extreme pressure resistance and bearing capacity, good oxidation stability and long service life.
Description
Technical Field
The invention relates to the technical field of lubricating oil, in particular to high-wear-resistance lubricating oil and a preparation method thereof.
Background
With the rapid development of modern industry and the increasingly prominent energy problem, higher requirements are put forward on the aspects of reliability, service life, wear resistance and the like of lubricating oil. The traditional lubricating oil is gradually replaced by some compound lubricating oil with excellent lubricating performance, and the lubricating oil can effectively reduce the friction between objects, reduce the loss of the objects and play a role in saving energy and reducing consumption.
The lubricating oil is a liquid lubricant which is used on various automobile transmissions, mechanical equipment and precision instruments to reduce friction and protect machines and workpieces, is mainly used for reducing friction between surfaces of moving parts, and has the functions of cooling, sealing, corrosion prevention, rust prevention, insulation, power transmission, impurity cleaning and the like on the mechanical equipment. Lubricating oils are generally composed of two parts, a base oil and additives. The base oil is the main component of the lubricating oil, the basic properties of the lubricating oil are determined, the additives can make up and improve the defects in the performance aspect of the base oil, and the additives endow certain new performances, such as oxidation resistance, wear resistance, pour point depression and the like, and are important components of the lubricating oil.
In order to improve the lubricating properties of lubricating oils, various antiwear and antifriction additives are generally added to the base lubricating oil. At present, the antiwear and antifriction additives mainly fall into two categories: the first type is an oil-soluble additive such as polar group-containing oiliness agent, fatty acid ester, organic amide, amide ester, imide compound, sulfurized ester, phosphorus-containing compound, chlorine-containing compound, boric acid ester, borate, organic metal compound, organic molybdenum compound, etc.; the second type is a solid additive such as graphite-based materials having a lamellar structure, molybdenum disulfide, tungsten disulfide, boron nitride, and the like. However, the oil-soluble additives are decomposed at high temperatures, the lubricating properties are significantly reduced, and the decomposed products may cause corrosion of equipment, resulting in process contamination. The solid additive is easy to cause poor comprehensive performance of the lubricating oil due to the problem of dispersibility, and the performance stability and the wear resistance are required to be further improved.
The Chinese invention patent with the application number of 201410313292.4 discloses wear-resistant vehicle lubricating oil which is prepared from the following components in parts by weight: 25-40 parts of modified nano-diamond, 40-80 parts of base oil, 20-30 parts of organic molybdenum mixture, 10-20 parts of an antiwear agent and 20-30 parts of a preservative. The invention also discloses a preparation method of the wear-resistant vehicle lubricating oil. The antiwear agent is used in the lubricating oil for vehicles, so that the friction and the abrasion can be reduced, and the viscosity index of an oil product can be improved. Meanwhile, the invention also adds the preservative, which can prevent the metal parts from rusting and prolong the service life of the vehicle. However, the organomolybdenum mixture added thereto may gradually fail due to degradation in practical use. And the added antiwear agent contains phosphorus, sulfur and chlorine compounds, so that the antiwear agent is easy to corrode equipment, and causes environmental pollution.
Therefore, the development of the high-wear-resistance lubricating oil with remarkable lubricating effect, good wear-resistance performance, strong extreme pressure resistance and bearing capacity, good oxidation stability and long service life meets the market demand, has higher market value and application prospect, and has very important significance for promoting the development of the lubricating oil industry.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention provides high-wear-resistance lubricating oil which is characterized by being prepared from the following components in parts by weight: 3-5 parts of benzotriazole-1-oxyl tris (dimethylamino) phosphonium hexafluorophosphate, 4-8 parts of modified boron nitride nanotube silicon nitride nanowire compound, 8-12 parts of fluorine-containing N, N' -thiodiglycolamidate/polyethylene glycol dicarboxylic acid polycondensate, 70-80 parts of base oil, 0.8-1.2 parts of a viscosity agent, 0.5-1 part of a dispersing agent and 1-2 parts of an antioxidant.
Preferably, the viscous agent is at least one of hydrogenated styrene diene copolymer, polymethacrylate and ethylene propylene copolymer.
Preferably, the dispersant is one or more of triethylhexylphosphoric acid, vinyl bis stearamide, stearic acid monoglyceride, polyethylene glycol and monoalkenyl succinimide in any ratio.
Preferably, the antioxidant is at least one of 2, 6-tertiary butyl-4-methylphenol, bis (3, 5-tertiary butyl-4-hydroxyphenyl) sulfide, pentaerythritol tetrakis [ beta- (3, 5-tertiary butyl-4-hydroxyphenyl) propionate ] and bisdodecyl alcohol ester.
Preferably, the base oil is at least one of base oil HVI500, base oil HVI200 and base oil 150 BS.
Preferably, the preparation method of the modified boron nitride nanotube silicon nitride nanowire compound comprises the following steps: uniformly mixing the boron nitride nanotube and the silicon nitride nanowire, dispersing the mixture in an organic solvent, adding N, N '-bis (2-hydroxyethyl) -N, N' -bis (trimethoxysilylpropyl) ethylenediamine, stirring and reacting for 4-6 hours at the temperature of 60-80 ℃, and then removing the solvent by rotary evaporation to obtain the modified boron nitride nanotube-silicon nitride nanowire compound.
Preferably, the mass ratio of the boron nitride nanotube to the silicon nitride nanowire to the organic solvent to the N, N '-bis (2-hydroxyethyl) -N, N' -bis (trimethoxysilylpropyl) ethylenediamine is 1 (1-2) to 10-16 to 0.1-0.3; the organic solvent is any one of ethanol, dichloromethane and acetone.
Preferably, the preparation method of the boron nitride nanotube is described in the first specific embodiment of the Chinese patent with the application number of 200910310305.1; the preparation method of the silicon nitride nanowire is disclosed in the first embodiment of the Chinese patent with the application number of 200810063928.9.
Preferably, the preparation method of the fluorine-containing N, N' -sulfuryl diimidazole salt/polyethylene glycol dicarboxylic acid polycondensate comprises the following steps:
step D1, adding N, N' -sulfuryl diimidazole and 2-chloro-1- (4-fluorophenyl) ethanol into N, N-dimethylformamide, stirring and reacting for 4-6 hours at 40-60 ℃, and then removing the solvent by rotary evaporation to obtain an intermediate product;
and D2, adding the intermediate product prepared in the step D1, polyethylene glycol dicarboxylic acid, dicyclohexylcarbodiimide and 4-dimethylaminopyridine into a high-boiling-point solvent, stirring and reacting for 4-6 hours at the temperature of 100-140 ℃, then removing the solvent by rotary evaporation, adding the crude product into a sodium monofluorophosphate solution with the mass percentage concentration of 5-10%, stirring and reacting for 4-6 hours, then placing the obtained mixed solution into a dialysis bag, dialyzing for 10-20 hours in deionized water, and then removing the water in the dialysis bag by rotary evaporation to obtain the fluorine-containing N, N' -thiodiimidazole salt/polyethylene glycol dicarboxylic acid polycondensate.
Preferably, the molar ratio of the N, N' -sulfuryl diimidazole, the 2-chloro-1- (4-fluorophenyl) ethanol and the N, N-dimethylformamide in the step D1 is 1:1 (6-10).
Preferably, the molar ratio of the intermediate product, the polyethylene glycol dicarboxylic acid, the dicyclohexylcarbodiimide, the 4-dimethylaminopyridine and the high-boiling-point solvent in the step D2 is 1:1 (0.6-1) to 0.5 (10-15).
Preferably, the high boiling point solvent is at least one of dimethyl sulfoxide, N-dimethylformamide and N-methylpyrrolidone; the polyethylene glycol dicarboxylic acid has a number average molecular weight of 600, a name of Schenss, a cargo number: SJ010AE163184, purchased from mote laboratory products.
Preferably, the mass ratio of the crude product to the sodium monofluorophosphate solution is 1 (4-8).
Another object of the present invention is to provide a method for preparing the highly wear-resistant lubricating oil, which is characterized by comprising the following steps: adding base oil into a reaction kettle according to the weight parts, controlling the temperature to be between 60 and 80 ℃, then adding benzotriazole-1-oxyl tris (dimethylamino) phosphonium hexafluorophosphate, a modified boron nitride nanotube silicon nitride nanowire compound and a fluorine-containing N, N' -sulfuryl diimidazole salt/polyethylene glycol dicarboxylic acid polycondensate, uniformly stirring, cooling to 50 to 60 ℃, adding a viscous agent, a dispersing agent and an antioxidant, and uniformly stirring to obtain the high-wear-resistance lubricating oil finished product.
Adopt the produced beneficial effect of above-mentioned technical scheme to lie in:
(1) the preparation method of the high-wear-resistance lubricating oil provided by the invention is simple and easy to implement, convenient to operate and control, low in equipment dependence, high in production efficiency and finished product qualification rate, low in pollution in the preparation process, suitable for continuous large-scale production, and high in economic value and social value.
(2) The high wear-resistant lubricating oil provided by the invention overcomes the defects that the high wear-resistant lubricating oil in the prior art is poor in comprehensive performance, large in corrosion to equipment and free from further improvement in performance stability and wear resistance, and the prepared high wear-resistant lubricating oil is remarkable in lubricating effect, good in wear resistance, strong in extreme pressure resistance and bearing capacity, good in oxidation stability and long in service life through the synergistic effect of the components.
(3) The benzotriazole-1-oxyl tris (dimethylamino) phosphonium hexafluorophosphate serving as the ionic salt of the high-wear-resistance lubricating oil provided by the invention has the advantages of low volatility, low friction coefficient and wear loss, high wear resistance and good stability, so that the wear resistance of the lubricating oil prepared after the benzotriazole-1-oxyl tris (dimethylamino) phosphonium hexafluorophosphate is effectively improved, the economic performance of the lubricating oil is further improved, the lubricating oil also has the corrosion resistance, the compatibility among components can be enhanced, the stability of the lubricating oil is improved, and the problem of component phase separation and precipitation of the lubricating oil when the lubricating oil is placed for a long time is solved. The substance is used as a pesticide intermediate in the prior art, and the substance is applied to lubricating oil for the first time, has good compatibility with other components in the lubricating oil, has good use effect, and has obvious effect of improving the comprehensive performance of the lubricating oil.
(4) The high-wear-resistance lubricating oil provided by the invention is added with the modified boron nitride nanotube silicon nitride nanowire compound, so that not only are a plurality of advantages of the traditional nano materials retained, but also the nano tubes and the nanowire have smooth surfaces and a self-lubricating effect, so that the wear resistance and the comprehensive performance of the lubricating oil are effectively improved; in addition, the composite has good stability and excellent temperature resistance, so that the application range of the lubricating oil is wider.
(5) The high-wear-resistance lubricating oil provided by the invention contains the fluorine-containing N, N' -sulfuryl diimidazole salt/polyethylene glycol dicarboxylic acid polycondensate, and can improve the lubricating property and the wear resistance of the lubricating oil; because the molecular chain contains an ionic salt structure, the volatility is low, and the stability is improved; the main molecular chain contains polyether and ionic salt structures, so that the compatibility among all components can be improved, the storage and transportation stability of the lubricating oil is good, and the structures also have cleaning performance and lubricating performance; the sulfuryl imidazole and fluorine-containing result introduced into the molecular chain can improve the oxidation resistance and the lubricating property, and can also improve the extreme pressure resistance and the high bearing capacity, so that the wear resistance is good, the performance stability is good, and the service life is long.
(6) According to the high-wear-resistance lubricating oil provided by the invention, introduced ionic salt anions and chloride ions are removed through ion exchange, and meanwhile, a monofluorophosphate radical structure is introduced to have a synergistic effect with other components, so that the corrosion resistance is effectively improved, and the environmental pollution is reduced.
Detailed Description
In order to make the technical solutions of the present invention better understood and make the above features, objects, and advantages of the present invention more comprehensible, the present invention is further described with reference to the following examples. The examples are intended to illustrate the invention only and are not intended to limit the scope of the invention; the polyethylene glycol dicarboxylic acid involved in the examples of the present invention has a number average molecular weight of 600, and is available under the brand name of Schen, cat #: SJ010AE163184, purchased from mote laboratory goods mall; the preparation method of the boron nitride nanotube refers to the first specific embodiment of the Chinese patent with the application number of 200910310305.1; the preparation method of the silicon nitride nanowire is disclosed in the first embodiment of the Chinese patent with the application number of 200810063928.9; other raw materials were all purchased commercially.
Example 1
The high-wear-resistance lubricating oil is characterized by being prepared from the following components in parts by weight: 3 parts of benzotriazole-1-oxyl tris (dimethylamino) phosphonium hexafluorophosphate, 4 parts of modified boron nitride nanotube silicon nitride nanowire compound, 8 parts of fluorine-containing N, N' -sulfuryl diimidazole salt/polyethylene glycol dicarboxylic acid polycondensate, 70 parts of base oil, 0.8 part of a viscosity agent, 0.5 part of a dispersant and 1 part of an antioxidant.
The viscous agent is hydrogenated styrene diene copolymer; the dispersant is triethylhexylphosphoric acid; the antioxidant is 2, 6-tertiary butyl-4-methylphenol; the base oil is base oil HVI 500.
The preparation method of the modified boron nitride nanotube silicon nitride nanowire compound comprises the following steps: uniformly mixing the boron nitride nanotube and the silicon nitride nanowire, dispersing the mixture in an organic solvent, adding N, N '-bis (2-hydroxyethyl) -N, N' -bis (trimethoxysilylpropyl) ethylenediamine, stirring the mixture at the temperature of 60 ℃ for reacting for 4 hours, and then performing rotary evaporation to remove the solvent to obtain the modified boron nitride nanotube-silicon nitride nanowire compound.
The mass ratio of the boron nitride nanotube to the silicon nitride nanowire to the organic solvent to the N, N '-bis (2-hydroxyethyl) -N, N' -bis (trimethoxysilylpropyl) ethylenediamine is 1:1:10: 0.1; the organic solvent is ethanol.
The preparation method of the fluorine-containing N, N' -sulfuryl diimidazole salt/polyethylene glycol dicarboxylic acid polycondensate comprises the following steps:
step D1, adding N, N' -sulfuryl diimidazole and 2-chloro-1- (4-fluorophenyl) ethanol into N, N-dimethylformamide, stirring and reacting for 4 hours at 40 ℃, and then removing the solvent by rotary evaporation to obtain an intermediate product;
and D2, adding the intermediate product prepared in the step D1, polyethylene glycol dicarboxylic acid, dicyclohexylcarbodiimide and 4-dimethylaminopyridine into a high-boiling-point solvent, stirring and reacting for 4 hours at 100 ℃, removing the solvent by rotary evaporation, adding the crude product into a sodium monofluorophosphate solution with the mass percentage concentration of 5%, stirring and reacting for 4 hours, putting the obtained mixed solution into a dialysis bag, dialyzing for 10 hours in deionized water, and removing water in the dialysis bag by rotary evaporation to obtain the fluorine-containing N, N' -thiodiimidazole salt/polyethylene glycol dicarboxylic acid polycondensate.
In the step D1, the molar ratio of the N, N' -sulfuryl diimidazole to the 2-chloro-1- (4-fluorophenyl) ethanol to the N, N-dimethylformamide is 1:1: 6.
The molar ratio of the intermediate product, polyethylene glycol dicarboxylic acid, dicyclohexylcarbodiimide, 4-dimethylaminopyridine and high-boiling-point solvent in the step D2 is 1:1:0.6:0.5: 10; the high boiling point solvent is dimethyl sulfoxide.
The mass ratio of the crude product to the sodium monofluorophosphate solution is 1: 4.
The preparation method of the high-abrasion-resistance lubricating oil is characterized by comprising the following steps of: adding base oil into a reaction kettle according to the parts by weight, controlling the temperature at 60 ℃, then adding benzotriazole-1-oxyl tris (dimethylamino) phosphonium hexafluorophosphate, a modified boron nitride nanotube silicon nitride nanowire compound and a fluorine-containing N, N' -sulfuryl diimidazole salt/polyethylene glycol dicarboxylic acid polycondensate, uniformly stirring, cooling to 50 ℃, adding a viscous agent, a dispersing agent and an antioxidant, and uniformly stirring to obtain the high-wear-resistance lubricating oil finished product.
Example 2
The high-wear-resistance lubricating oil is characterized by being prepared from the following components in parts by weight: 3.5 parts of benzotriazole-1-oxyl tris (dimethylamino) phosphonium hexafluorophosphate, 5 parts of modified boron nitride nanotube silicon nitride nanowire compound, 9 parts of fluorine-containing N, N' -sulfuryl diimidazole salt/polyethylene glycol dicarboxylic acid polycondensate, 72 parts of base oil, 0.9 part of viscosity agent, 0.6 part of dispersant and 1.2 parts of antioxidant.
The viscous agent is polymethacrylate; the dispersant is vinyl bis stearamide; the antioxidant is bis (3, 5-tertiary butyl-4-hydroxyphenyl) sulfide; the base oil is base oil HVI 500.
The preparation method of the modified boron nitride nanotube silicon nitride nanowire compound comprises the following steps: uniformly mixing the boron nitride nanotube and the silicon nitride nanowire, dispersing the mixture in an organic solvent, adding N, N '-bis (2-hydroxyethyl) -N, N' -bis (trimethoxysilylpropyl) ethylenediamine into the organic solvent, stirring the mixture at 65 ℃ for reacting for 4.5 hours, and then performing rotary evaporation to remove the solvent to obtain a modified boron nitride nanotube-silicon nitride nanowire compound; the mass ratio of the boron nitride nanotube to the silicon nitride nanowire to the organic solvent to the N, N '-bis (2-hydroxyethyl) -N, N' -bis (trimethoxysilylpropyl) ethylenediamine is 1:1.2:12: 0.15; the organic solvent is dichloromethane.
The preparation method of the fluorine-containing N, N' -sulfuryl diimidazole salt/polyethylene glycol dicarboxylic acid polycondensate comprises the following steps:
step D1, adding N, N' -sulfuryl diimidazole and 2-chloro-1- (4-fluorophenyl) ethanol into N, N-dimethylformamide, stirring and reacting for 4.5 hours at the temperature of 45 ℃, and then removing the solvent by rotary evaporation to obtain an intermediate product;
and D2, adding the intermediate product prepared in the step D1, polyethylene glycol dicarboxylic acid, dicyclohexylcarbodiimide and 4-dimethylaminopyridine into a high-boiling-point solvent, stirring and reacting for 4.5 hours at 110 ℃, then performing rotary evaporation to remove the solvent, adding the crude product into a sodium monofluorophosphate solution with the mass percentage concentration of 6%, stirring and reacting for 4.5 hours, then placing the obtained mixed solution into a dialysis bag, dialyzing for 12 hours in deionized water, and then performing rotary evaporation to remove water in the dialysis bag to obtain the fluorine-containing N, N' -thiodiimidazole salt/polyethylene glycol dicarboxylic acid polycondensate.
In the step D1, the molar ratio of the N, N' -sulfuryl diimidazole to the 2-chloro-1- (4-fluorophenyl) ethanol to the N, N-dimethylformamide is 1:1: 7.
The molar ratio of the intermediate product, polyethylene glycol dicarboxylic acid, dicyclohexylcarbodiimide, 4-dimethylaminopyridine and high-boiling-point solvent in the step D2 is 1:1:0.7:0.5: 11; the high boiling point solvent is N, N-dimethylformamide.
The mass ratio of the crude product to the sodium monofluorophosphate solution is 1: 5.
The preparation method of the high-abrasion-resistance lubricating oil is characterized by comprising the following steps of: adding base oil into a reaction kettle according to the parts by weight, controlling the temperature at 65 ℃, then adding benzotriazole-1-oxyl tris (dimethylamino) phosphonium hexafluorophosphate, a modified boron nitride nanotube silicon nitride nanowire compound and a fluorine-containing N, N' -sulfuryl diimidazole salt/polyethylene glycol dicarboxylic acid polycondensate, uniformly stirring, cooling to 53 ℃, adding a viscous agent, a dispersing agent and an antioxidant, and uniformly stirring to obtain the high-wear-resistance lubricating oil finished product.
Example 3
The high-wear-resistance lubricating oil is characterized by being prepared from the following components in parts by weight: 4 parts of benzotriazole-1-oxyl tris (dimethylamino) phosphonium hexafluorophosphate, 6 parts of modified boron nitride nanotube silicon nitride nanowire compound, 10 parts of fluorine-containing N, N' -sulfuryl diimidazole salt/polyethylene glycol dicarboxylic acid polycondensate, 75 parts of base oil, 1 part of a viscosity agent, 0.7 part of a dispersing agent and 1.5 parts of an antioxidant.
The viscosity agent is an ethylene propylene copolymer; the dispersant is stearic acid monoglyceride; the antioxidant is tetra [ beta- (3, 5-tertiary butyl-4-hydroxyphenyl) propionic acid ] pentaerythritol ester; the base oil is base oil HVI 500.
The preparation method of the modified boron nitride nanotube silicon nitride nanowire compound comprises the following steps: uniformly mixing the boron nitride nanotube and the silicon nitride nanowire, dispersing the mixture in an organic solvent, adding N, N '-bis (2-hydroxyethyl) -N, N' -bis (trimethoxysilylpropyl) ethylenediamine into the organic solvent, stirring the mixture at 70 ℃ for reacting for 5 hours, and performing rotary evaporation to remove the solvent to obtain a modified boron nitride nanotube-silicon nitride nanowire compound; the mass ratio of the boron nitride nanotube to the silicon nitride nanowire to the organic solvent to the N, N '-bis (2-hydroxyethyl) -N, N' -bis (trimethoxysilylpropyl) ethylenediamine is 1:1.5:13: 0.2; the organic solvent is acetone.
The preparation method of the fluorine-containing N, N' -sulfuryl diimidazole salt/polyethylene glycol dicarboxylic acid polycondensate comprises the following steps:
step D1, adding N, N' -sulfuryl diimidazole and 2-chloro-1- (4-fluorophenyl) ethanol into N, N-dimethylformamide, stirring and reacting for 5 hours at 50 ℃, and then removing the solvent by rotary evaporation to obtain an intermediate product;
and D2, adding the intermediate product prepared in the step D1, polyethylene glycol dicarboxylic acid, dicyclohexylcarbodiimide and 4-dimethylaminopyridine into a high-boiling-point solvent, stirring and reacting for 5 hours at 120 ℃, removing the solvent by rotary evaporation, adding the crude product into a sodium monofluorophosphate solution with the mass percentage concentration of 5-10%, stirring and reacting for 5 hours, putting the obtained mixed solution into a dialysis bag, dialyzing for 15 hours in deionized water, and removing water in the dialysis bag by rotary evaporation to obtain the fluorine-containing N, N' -thiodiimidazole salt/polyethylene glycol dicarboxylic acid polycondensate.
In the step D1, the molar ratio of the N, N' -sulfuryl diimidazole to the 2-chloro-1- (4-fluorophenyl) ethanol to the N, N-dimethylformamide is 1:1: 8.
The molar ratio of the intermediate product, polyethylene glycol dicarboxylic acid, dicyclohexylcarbodiimide, 4-dimethylaminopyridine and high-boiling-point solvent in the step D2 is 1:1:0.8:0.5: 13; the high boiling point solvent is N-methyl pyrrolidone.
The mass ratio of the crude product to the sodium monofluorophosphate solution is 1: 6.
The preparation method of the high-abrasion-resistance lubricating oil is characterized by comprising the following steps of: adding base oil into a reaction kettle according to the parts by weight, controlling the temperature to be 70 ℃, then adding benzotriazole-1-oxyl tris (dimethylamino) phosphonium hexafluorophosphate, a modified boron nitride nanotube silicon nitride nanowire compound and a fluorine-containing N, N' -sulfuryl diimidazole salt/polyethylene glycol dicarboxylic acid polycondensate, uniformly stirring, cooling to 55 ℃, adding a viscous agent, a dispersing agent and an antioxidant, and uniformly stirring to obtain the finished product of the high-wear-resistant lubricating oil.
Example 4
The high-wear-resistance lubricating oil is characterized by being prepared from the following components in parts by weight: 3-5 parts of benzotriazole-1-oxyl tris (dimethylamino) phosphonium hexafluorophosphate, 7 parts of modified boron nitride nanotube silicon nitride nanowire compound, 11 parts of fluorine-containing N, N' -sulfuryl diimidazole salt/polyethylene glycol dicarboxylic acid polycondensate, 78 parts of base oil, 1.1 parts of a viscosity agent, 0.9 part of a dispersant and 1.8 parts of an antioxidant.
The viscous agent is formed by mixing hydrogenated styrene diene copolymer, polymethacrylate and ethylene propylene copolymer according to the mass ratio of 1:3: 2; the dispersing agent is formed by mixing triethyl hexyl phosphoric acid, vinyl distearamide, stearic acid monoglyceride, polyethylene glycol and mono-alkenyl succinimide according to the mass ratio of 1:3:2:1: 2; the antioxidant is prepared by mixing 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 and docosanol ester according to the mass ratio of 1:2:2: 3; the base oil is base oil HVI 500.
The preparation method of the modified boron nitride nanotube silicon nitride nanowire compound comprises the following steps: the boron nitride nanotube and the silicon nitride nanowire are uniformly mixed and dispersed in an organic solvent, then N, N '-bis (2-hydroxyethyl) -N, N' -bis (trimethoxysilylpropyl) ethylenediamine is added into the mixture, the mixture is stirred and reacts for 5.8 hours at the temperature of 75 ℃, and then the solvent is removed by rotary evaporation, so that the modified boron nitride nanotube silicon nitride nanowire compound is obtained.
The mass ratio of the boron nitride nanotube to the silicon nitride nanowire to the organic solvent to the N, N '-bis (2-hydroxyethyl) -N, N' -bis (trimethoxysilylpropyl) ethylenediamine is 1:1.8:15: 0.28; the organic solvent is ethanol.
The preparation method of the fluorine-containing N, N' -sulfuryl diimidazole salt/polyethylene glycol dicarboxylic acid polycondensate comprises the following steps:
step D1, adding N, N' -sulfuryl diimidazole and 2-chloro-1- (4-fluorophenyl) ethanol into N, N-dimethylformamide, stirring and reacting for 5.8 hours at 55 ℃, and then removing the solvent by rotary evaporation to obtain an intermediate product;
and D2, adding the intermediate product prepared in the step D1, polyethylene glycol dicarboxylic acid, dicyclohexylcarbodiimide and 4-dimethylaminopyridine into a high-boiling-point solvent, stirring and reacting for 5.5 hours at 135 ℃, removing the solvent by rotary evaporation, adding the crude product into a 9 mass percent sodium monofluorophosphate solution, stirring and reacting for 5.8 hours, putting the obtained mixed solution into a dialysis bag, dialyzing for 18 hours in deionized water, and removing water in the dialysis bag by rotary evaporation to obtain the fluorine-containing N, N' -thiodiimidazole salt/polyethylene glycol dicarboxylic acid polycondensate.
In the step D1, the molar ratio of the N, N' -sulfuryl diimidazole to the 2-chloro-1- (4-fluorophenyl) ethanol to the N, N-dimethylformamide is 1:1: 9.5.
The molar ratio of the intermediate product, polyethylene glycol dicarboxylic acid, dicyclohexylcarbodiimide, 4-dimethylaminopyridine and high-boiling-point solvent in the step D2 is 1:1:0.9:0.5: 14; the high boiling point solvent is formed by mixing dimethyl sulfoxide, N-dimethylformamide and N-methylpyrrolidone according to the mass ratio of 1:3: 5.
The mass ratio of the crude product to the sodium monofluorophosphate solution is 1: 7.5.
The preparation method of the high-abrasion-resistance lubricating oil is characterized by comprising the following steps of: adding base oil into a reaction kettle according to the parts by weight, controlling the temperature to be 78 ℃, then adding benzotriazole-1-oxyl tris (dimethylamino) phosphonium hexafluorophosphate, a modified boron nitride nanotube silicon nitride nanowire compound and a fluorine-containing N, N' -sulfuryl diimidazole salt/polyethylene glycol dicarboxylic acid polycondensate, uniformly stirring, cooling to 58 ℃, adding a viscous agent, a dispersing agent and an antioxidant, and uniformly stirring to obtain the finished product of the high-wear-resistant lubricating oil.
Example 5
The high-wear-resistance lubricating oil is characterized by being prepared from the following components in parts by weight: 5 parts of benzotriazole-1-oxyl tris (dimethylamino) phosphonium hexafluorophosphate, 8 parts of modified boron nitride nanotube silicon nitride nanowire compound, 12 parts of fluorine-containing N, N' -sulfuryl diimidazole salt/polyethylene glycol dicarboxylic acid polycondensate, 80 parts of base oil, 1.2 parts of a viscosity agent, 1 part of a dispersing agent and 2 parts of an antioxidant.
The viscous agent is hydrogenated styrene diene copolymer; the dispersant is a monoalkenyl succinimide; the antioxidant is a didodecanol ester; the base oil is base oil HVI 500.
The preparation method of the modified boron nitride nanotube silicon nitride nanowire compound comprises the following steps: uniformly mixing the boron nitride nanotube and the silicon nitride nanowire, dispersing the mixture in an organic solvent, adding N, N '-bis (2-hydroxyethyl) -N, N' -bis (trimethoxysilylpropyl) ethylenediamine into the organic solvent, stirring the mixture at the temperature of 80 ℃ to react for 6 hours, and then performing rotary evaporation to remove the solvent to obtain a modified boron nitride nanotube silicon nitride nanowire compound; the mass ratio of the boron nitride nanotube to the silicon nitride nanowire to the organic solvent to the N, N '-bis (2-hydroxyethyl) -N, N' -bis (trimethoxysilylpropyl) ethylenediamine is 1:2:16: 0.3; the organic solvent is dichloromethane.
The preparation method of the fluorine-containing N, N' -sulfuryl diimidazole salt/polyethylene glycol dicarboxylic acid polycondensate comprises the following steps:
step D1, adding N, N' -sulfuryl diimidazole and 2-chloro-1- (4-fluorophenyl) ethanol into N, N-dimethylformamide, stirring and reacting for 6 hours at the temperature of 60 ℃, and then removing the solvent by rotary evaporation to obtain an intermediate product;
and D2, adding the intermediate product prepared in the step D1, polyethylene glycol dicarboxylic acid, dicyclohexylcarbodiimide and 4-dimethylaminopyridine into a high-boiling-point solvent, stirring and reacting for 6 hours at 140 ℃, removing the solvent by rotary evaporation, adding the crude product into a 10 mass percent sodium monofluorophosphate solution, stirring and reacting for 6 hours, putting the obtained mixed solution into a dialysis bag, dialyzing for 20 hours in deionized water, and removing water in the dialysis bag by rotary evaporation to obtain the fluorine-containing N, N' -thiodiimidazole salt/polyethylene glycol dicarboxylic acid polycondensate.
In the step D1, the molar ratio of the N, N' -sulfuryl diimidazole to the 2-chloro-1- (4-fluorophenyl) ethanol to the N, N-dimethylformamide is 1:1: 10.
The molar ratio of the intermediate product, polyethylene glycol dicarboxylic acid, dicyclohexylcarbodiimide, 4-dimethylaminopyridine and high-boiling-point solvent in the step D2 is 1:1:1:0.5: 15; the high boiling point solvent is dimethyl sulfoxide.
The mass ratio of the crude product to the sodium monofluorophosphate solution is 1: 8.
The preparation method of the high-abrasion-resistance lubricating oil is characterized by comprising the following steps of: adding base oil into a reaction kettle according to the parts by weight, controlling the temperature to be between 80 ℃, then adding benzotriazole-1-oxyl tris (dimethylamino) phosphonium hexafluorophosphate, a modified boron nitride nanotube silicon nitride nanowire compound and a fluorine-containing N, N' -sulfuryl diimidazole salt/polyethylene glycol dicarboxylic acid polycondensate, uniformly stirring, cooling to 60 ℃, adding a viscous agent, a dispersing agent and an antioxidant, and uniformly stirring to obtain the finished product of the high-wear-resistance lubricating oil.
Comparative example 1
This example provides a highly wear resistant lubricant having substantially the same formulation and preparation as in example 1, except that benzotriazol-1-yloxytris (dimethylamino) phosphonium hexafluorophosphate is not added.
Comparative example 2
The present example provides a highly wear resistant lubricant, the formulation and preparation method of which are substantially the same as those of example 1, except that no modified boron nitride nanotube silicon nitride nanowire composite is added.
Comparative example 3
This example provides a highly antiwear lubricating oil having substantially the same formulation and preparation as in example 1, except that no fluorine-containing N, N' -thiobisimidazolium salt/polyethylene glycol dicarboxylic acid polycondensate was added.
Comparative example 4
The present example provides a highly wear resistant lubricant, the formulation and preparation method of which are substantially the same as those of example 1, except that no boron nitride nanotube is added in the preparation process of the modified boron nitride nanotube silicon nitride nanowire composite.
Comparative example 5
The present example provides a highly wear resistant lubricant, the formulation and preparation method of which are substantially the same as those of example 1, except that no silicon nitride nanowire is added in the preparation process of the modified boron nitride nanotube silicon nitride nanowire composite.
The samples obtained in the above examples 1 to 5 and comparative examples 1 to 5 were subjected to the relevant performance tests, the test results are shown in table 1, the test methods are as follows, four-ball test: testing was performed 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.
TABLE 1 Properties of samples of examples and comparative examples
| Item | Maximum No-seize load (PB)/N (kg) | Sintering load (PD)/N (kg) | Abrasive grain diameter d/mm |
| Example 1 | 94 | 168 | 0.22 |
| Example 2 | 96 | 171 | 0.19 |
| Example 3 | 99 | 175 | 0.17 |
| Example 4 | 102 | 178 | 0.14 |
| Example 5 | 105 | 182 | 0.11 |
| Comparative example 1 | 82 | 140 | 0.35 |
| Comparative example 2 | 75 | 135 | 0.43 |
| Comparative example 3 | 80 | 137 | 0.37 |
| Comparative example 4 | 78 | 139 | 0.41 |
| Comparative example 5 | 77 | 138 | 0.39 |
As can be seen from Table 1, the highly antiwear lubricating oils disclosed in the examples of the present invention have better extreme pressure properties and lubricating properties than the comparative examples, which are the result of the synergistic effect of the components.
The foregoing shows and describes the general principles and broad features of the present invention and advantages thereof. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present 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 (10)
1. The high-wear-resistance lubricating oil is characterized by being prepared from the following components in parts by weight: 3-5 parts of benzotriazole-1-oxyl tris (dimethylamino) phosphonium hexafluorophosphate, 4-8 parts of modified boron nitride nanotube silicon nitride nanowire compound, 8-12 parts of fluorine-containing N, N' -thiodiglycolamidate/polyethylene glycol dicarboxylic acid polycondensate, 70-80 parts of base oil, 0.8-1.2 parts of a viscosity agent, 0.5-1 part of a dispersing agent and 1-2 parts of an antioxidant.
2. The highly wear resistant lubricant according to claim 1, wherein said viscosity agent is at least one of hydrogenated styrene diene copolymer, polymethacrylate, ethylene propylene copolymer.
3. The highly antiwear lubricating oil according to claim 1, wherein the dispersant is one or two or more of triethylhexylphosphoric acid, vinylbisstearamide, stearic acid monoglyceride, polyethylene glycol, and monoalkenylbutyldiimide in any ratio.
4. The highly antiwear lubricating oil according to claim 1, wherein the antioxidant is at least one 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 ], and didodecyl alcohol ester.
5. The highly antiwear lubricating oil according to claim 1, wherein the base oil is at least one of base oil HVI500, base oil HVI200, base oil 150 BS.
6. The high-wear-resistance lubricating oil according to claim 1, wherein the preparation method of the modified boron nitride nanotube silicon nitride nanowire compound comprises the following steps: uniformly mixing the boron nitride nanotube and the silicon nitride nanowire, dispersing the mixture in an organic solvent, adding N, N '-bis (2-hydroxyethyl) -N, N' -bis (trimethoxysilylpropyl) ethylenediamine, stirring and reacting for 4-6 hours at the temperature of 60-80 ℃, and then removing the solvent by rotary evaporation to obtain the modified boron nitride nanotube-silicon nitride nanowire compound.
7. The high-wear-resistance lubricating oil of claim 6, wherein the mass ratio of the boron nitride nanotubes, the silicon nitride nanowires, the organic solvent and the N, N '-bis (2-hydroxyethyl) -N, N' -bis (trimethoxysilylpropyl) ethylenediamine is 1 (1-2) to (10-16) to (0.1-0.3); the organic solvent is any one of ethanol, dichloromethane and acetone.
8. The highly antiwear lubricating oil according to claim 1, wherein the process for producing the fluorine-containing N, N' -thiodiimidazole salt/polyethylene glycol dicarboxylic acid polycondensate comprises the steps of:
step D1, adding N, N' -sulfuryl diimidazole and 2-chloro-1- (4-fluorophenyl) ethanol into N, N-dimethylformamide, stirring and reacting for 4-6 hours at 40-60 ℃, and then removing the solvent by rotary evaporation to obtain an intermediate product;
and D2, adding the intermediate product prepared in the step D1, polyethylene glycol dicarboxylic acid, dicyclohexylcarbodiimide and 4-dimethylaminopyridine into a high-boiling-point solvent, stirring and reacting for 4-6 hours at the temperature of 100-140 ℃, then removing the solvent by rotary evaporation, adding the crude product into a sodium monofluorophosphate solution with the mass percentage concentration of 5-10%, stirring and reacting for 4-6 hours, then placing the obtained mixed solution into a dialysis bag, dialyzing for 10-20 hours in deionized water, and then removing the water in the dialysis bag by rotary evaporation to obtain the fluorine-containing N, N' -thiodiimidazole salt/polyethylene glycol dicarboxylic acid polycondensate.
9. The high antiwear lubricating oil according to claim 1, wherein the molar ratio of N, N' -sulfuryl diimidazole, 2-chloro-1- (4-fluorophenyl) ethanol, N-dimethylformamide in step D1 is 1:1 (6-10); the molar ratio of the intermediate product, the polyethylene glycol dicarboxylic acid, the dicyclohexylcarbodiimide, the 4-dimethylaminopyridine and the high-boiling-point solvent in the step D2 is 1:1 (0.6-1) to 0.5 (10-15); the high boiling point solvent is at least one of dimethyl sulfoxide, N-dimethylformamide and N-methylpyrrolidone; the mass ratio of the crude product to the sodium monofluorophosphate solution is 1 (4-8).
10. A method for preparing a highly wear resistant lubricating oil according to any one of claims 1 to 9, characterized by comprising the steps of: adding base oil into a reaction kettle according to the weight parts, controlling the temperature to be between 60 and 80 ℃, then adding benzotriazole-1-oxyl tris (dimethylamino) phosphonium hexafluorophosphate, a modified boron nitride nanotube silicon nitride nanowire compound and a fluorine-containing N, N' -sulfuryl diimidazole salt/polyethylene glycol dicarboxylic acid polycondensate, uniformly stirring, cooling to 50 to 60 ℃, adding a viscous agent, a dispersing agent and an antioxidant, and uniformly stirring to obtain the high-wear-resistance lubricating oil finished product.
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