CN112646635A - Lubricating oil composition and preparation method thereof - Google Patents
Lubricating oil composition and preparation method thereof Download PDFInfo
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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
- C10M157/00—Lubricating compositions characterised by the additive being a mixture of two or more macromolecular compounds covered by more than one of the main groups C10M143/00 - C10M155/00, each of these compounds being essential
- C10M157/10—Lubricating compositions characterised by the additive being a mixture of two or more macromolecular compounds covered by more than one of the main groups C10M143/00 - C10M155/00, each of these compounds being essential at least one of them being a compound containing atoms of elements not provided for in groups C10M157/02 - C10M157/08
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G65/00—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
- C08G65/02—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring
- C08G65/32—Polymers modified by chemical after-treatment
- C08G65/329—Polymers modified by chemical after-treatment with organic compounds
- C08G65/336—Polymers modified by chemical after-treatment with organic compounds containing silicon
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G65/00—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
- C08G65/02—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring
- C08G65/32—Polymers modified by chemical after-treatment
- C08G65/329—Polymers modified by chemical after-treatment with organic compounds
- C08G65/337—Polymers modified by chemical after-treatment with organic compounds containing other elements
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G69/00—Macromolecular compounds obtained by reactions forming a carboxylic amide link in the main chain of the macromolecule
- C08G69/42—Polyamides containing atoms other than carbon, hydrogen, oxygen, and nitrogen
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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
- C10M159/00—Lubricating compositions characterised by the additive being of unknown or incompletely defined constitution
- C10M159/12—Reaction products
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M169/00—Lubricating compositions characterised by containing as components a mixture of at least two types of ingredient selected from base-materials, thickeners or additives, covered by the preceding groups, each of these compounds being essential
- C10M169/04—Mixtures of base-materials and additives
- C10M169/048—Mixtures of base-materials and additives the additives being a mixture of compounds of unknown or incompletely defined constitution, non-macromolecular and macromolecular compounds
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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
- C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
- C10M2201/06—Metal compounds
- C10M2201/062—Oxides; Hydroxides; Carbonates or bicarbonates
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- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2205/00—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions
- C10M2205/02—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions containing acyclic monomers
- C10M2205/0206—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions containing acyclic monomers used as base material
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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
- C10M2209/00—Organic macromolecular compounds containing oxygen as ingredients in lubricant compositions
- C10M2209/10—Macromolecular compoundss obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- C10M2209/103—Polyethers, i.e. containing di- or higher polyoxyalkylene groups
- C10M2209/104—Polyethers, i.e. containing di- or higher polyoxyalkylene groups of alkylene oxides containing two carbon atoms only
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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
- 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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- 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
- C10M2227/00—Organic non-macromolecular compounds containing atoms of elements not provided for in groups C10M2203/00, C10M2207/00, C10M2211/00, C10M2215/00, C10M2219/00 or C10M2223/00 as ingredients in lubricant compositions
- C10M2227/04—Organic non-macromolecular compounds containing atoms of elements not provided for in groups C10M2203/00, C10M2207/00, C10M2211/00, C10M2215/00, C10M2219/00 or C10M2223/00 as ingredients in lubricant compositions having a silicon-to-carbon bond, e.g. organo-silanes
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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
- C10M2229/00—Organic macromolecular compounds containing atoms of elements not provided for in groups C10M2205/00, C10M2209/00, C10M2213/00, C10M2217/00, C10M2221/00 or C10M2225/00 as ingredients in lubricant compositions
- C10M2229/04—Siloxanes with specific structure
- C10M2229/05—Siloxanes with specific structure containing atoms other than silicon, hydrogen, oxygen or carbon
- C10M2229/054—Siloxanes with specific structure containing atoms other than silicon, hydrogen, oxygen or carbon containing phosphorus
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Abstract
The invention discloses a lubricating oil composition which is characterized by being prepared from the following components in parts by weight: 5-8 parts of ethoxy silicon-based ionized modified single-terminal amino polyethylene glycol carboxyl-containing metal organic framework salt, 3-6 parts of rare earth oxide nanoparticles, 15-25 parts of amino-terminated silicone oil/bis (4-carboxyphenyl) phenyl phosphine oxide polycondensate, 1-2 parts of 1, 3-dimethyl imidazolium dimethyl phosphate and 45-55 parts of poly alpha-olefin synthetic base oil. The invention also discloses a preparation method of the lubricating oil composition. The lubricating oil composition disclosed by the invention has the advantages of obvious lubricating effect and excellent extreme pressure performance and wear resistance.
Description
Technical Field
The invention relates to the technical field of lubricating oil, in particular to a lubricating oil composition and a preparation method thereof.
Background
In recent years, with the progress of global industrialization and the continuous development of industrial machinery, the application range of lubricating oil is wider and higher, and the performance requirements of the lubricating oil are higher and higher, so that the lubricating oil not only can reduce friction, protect machinery and workpieces, play roles of lubrication, auxiliary cooling, rust prevention, cleaning, sealing, buffering and the like, but also has higher requirements on the service life and the bearing performance.
Lubricating oils are generally composed of two parts, a base oil and additives. The base oil is the main component of the lubricating oil, determines the basic properties of the lubricating oil, and the additive can make up and improve the deficiency in the performance of the base oil, can endow the lubricating oil with new performance, and is an important component of the lubricating oil. However, the conventional lubricating oil often has poor compatibility between the base oil and the additive, so that the overall performance needs to be further improved. In addition, the lubricating oil on the market has the advantages of unobvious effects on the aspects of reducing mechanical vibration noise, reducing oil temperature, resisting abrasion and oxidation, high price, single effect, non-ideal use effect, easy severe damage to mechanical parts after long-term use and possible accidents in severe cases.
The Chinese patent with the application number of 201510900610.1 discloses a lubricating oil composition, which comprises the following components in percentage by mass: 85-95% of perfluoropolyether and 5-15% of boron nitride. The lubricating oil composition has the advantages of good lubricating performance and high stability in an oxygen-enriched environment, and is particularly suitable for lubricating the internal surface and structure of equipment exposed in the oxygen-enriched environment. However, the compatibility between the perfluoropolyether and boron nitride is poor, the perfluoropolyether is easy to cause extravasation in the long-term storage and transportation process, the performance stability is influenced, the base oil is the perfluoropolyether, the base oil is poor in wettability, the corrosion resistance is not ideal, the solubility to the additive is poor, the intersolubility with other oil products is poor, and the perfluoropolyether is decomposed at high temperature to form toxic gas. In addition, perfluoropolyethers are expensive, limiting their use.
Therefore, the lubricating oil composition with obvious lubricating effect and excellent extreme pressure performance and wear resistance is developed, meets the market demand, has wide market value and application prospect, and has very important significance for promoting the development of the field of lubricating oil.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention provides a lubricating oil composition which is characterized by being prepared from the following components in parts by weight: 5-8 parts of ethoxy silicon-based ionized modified single-terminal amino polyethylene glycol carboxyl-containing metal organic framework salt, 3-6 parts of rare earth oxide nanoparticles, 15-25 parts of amino-terminated silicone oil/bis (4-carboxyphenyl) phenyl phosphine oxide polycondensate, 1-2 parts of 1, 3-dimethyl imidazolium dimethyl phosphate and 45-55 parts of poly alpha-olefin synthetic base oil.
Preferably, the polyalphaolefin synthetic base oil is produced by INEOS
170 poly-alpha-olefin synthetic base oil.
Preferably, the method for preparing the amino-terminated silicone oil/bis (4-carboxyphenyl) phenylphosphine oxide polycondensate comprises the following steps: adding amino-terminated silicone oil and bis (4-carboxyphenyl) phenylphosphine oxide into a high-boiling-point solvent, reacting for 1-3 hours at the temperature of 150 ℃ and 170 ℃ under normal pressure, adding 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride and 4-dimethylaminopyridine into the solvent, heating to the temperature of 210 ℃ and 225 ℃, carrying out primary polycondensation for 4-6 hours, transferring the reaction liquid into a reaction kettle, vacuumizing to 500Pa, heating to the temperature of 240 ℃ and 260 ℃, carrying out polycondensation for 8-10 hours, precipitating in water, carrying out suction filtration, washing for 3-5 times by using dichloromethane, and carrying out rotary evaporation to remove the dichloromethane to obtain the amino-terminated silicone oil/bis (4-carboxyphenyl) phenylphosphine oxide polycondensate.
Preferably, the mol ratio of the amino-terminated silicone oil, the bis (4-carboxyphenyl) phenylphosphine oxide, the high-boiling-point solvent, the 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride and the 4-dimethylaminopyridine is 1:1 (6-10) to 0.6-0.9: 0.4.
Preferably, the amino-terminated silicone oil is prepared by the following method: chinese invention patent example 1 with application number 201710145310.6; the high boiling point solvent is at least one of dimethyl sulfoxide, N-dimethylformamide, N-dimethylacetamide and N-methylpyrrolidone.
Preferably, the preparation method of the rare earth oxide nanoparticles is described in Chinese patent application No. 201610381018.X, example 1.
Preferably, the preparation method of the carboxyl-containing metal organic framework salt of the ethoxy silicon-based ionized modified single-ended amino polyethylene glycol comprises the following steps:
step D1, adding amino polyethylene glycol and 3-chloropropyl trimethoxyl silane into ethanol, stirring and reacting for 4-6 hours at 50-70 ℃, and then performing rotary evaporation to remove ethanol to obtain an intermediate product;
and D2, adding the intermediate product prepared in the step D1 and the metal organic framework with carboxyl into N, N-dimethylformamide, stirring and reacting for 3-5 hours at 80-90 ℃, and then removing the N, N-dimethylformamide by rotary evaporation to obtain the ethyoxyl silicon-based ionized modified single-terminal amino polyethylene glycol metal organic framework salt with carboxyl.
Preferably, the molar ratio of the single-end amino polyethylene glycol, the 3-chloropropyl trimethoxy silane and the ethanol in the step D1 is 1:3 (12-20).
Preferably, the number average molecular weight of the single-terminal amino polyethylene glycol is 2000.
Preferably, the mass ratio of the intermediate product, the metal-organic framework with carboxyl and the N, N-dimethylformamide in the step D2 is 1 (0.1-0.3) to (5-10).
Preferably, the preparation method of the metal-organic framework with carboxyl is described in chinese patent application No. 201810731784.3, example 1.
Another object of the present invention is to provide a method for preparing the lubricating oil composition, which is characterized by comprising the steps of: the components are uniformly stirred according to the parts by weight and then are placed in a KH-700 type ultrasonic oscillator to be oscillated for 10-15 minutes under the power of 600-700W, so as to obtain the lubricating oil composition.
Adopt the produced beneficial effect of above-mentioned technical scheme to lie in:
(1) the preparation method of the lubricating oil composition provided by the invention is simple and easy to implement, convenient to operate and control, high in production efficiency and finished product qualification rate, suitable for continuous large-scale production, and high in economic value and social value.
(2) The lubricating oil composition provided by the invention overcomes the defect that the conventional lubricating oil is poor in matching between base oil and an additive, so that the comprehensive performance needs to be further improved; the lubricating oil on the market has the defects of no outstanding effect on reducing mechanical vibration noise, reducing oil temperature, resisting wear and oxidation, high price, single effect, unsatisfactory use effect, easy serious damage to mechanical parts after long-term use and possible accident occurrence in serious conditions, and the prepared lubricating oil composition has obvious lubricating effect, excellent extreme pressure performance and excellent wear resistance through the synergistic effect of all components.
(3) According to the lubricating oil composition provided by the invention, the added ethyoxyl silicon-based ionized modified single-ended amino polyethylene glycol carboxyl-containing metal organic framework salt effectively improves the lubricating property, the wear resistance and the thermal stability, the substance is connected with the carboxyl on the carboxyl-containing metal organic framework through the ionic bond through the quaternary ammonium salt on the ethyoxyl silicon-based ionized modified single-ended amino polyethylene glycol, and the advantages of polyethylene glycol, an organic metal framework and an ionic salt are combined, and the synergistic effect is realized, so that the comprehensive performance of the prepared lubricating oil composition is better, the ethyoxyl silicon-based structure introduced on the substance can be connected with inorganic components through the bridging effect, the compatibility among the components in the lubricating oil is further improved, the performance stability of the lubricating oil is further improved, the lubricating oil is not easy to separate out in the long-; the special structure in the organic metal framework can form a smooth surface, so that the lubricating effect is improved; and the special cavity structure can adsorb and fix the lake moistening oil, thereby improving the bearing performance of the lake moistening oil.
(4) According to the lubricating oil composition provided by the invention, the addition of the rare earth oxide nanoparticles can effectively improve the wear resistance, improve the lubricating property, stability and thermal stability, and have better wear resistance and friction reduction properties; the addition of the amino-terminated silicone oil/bis (4-carboxyphenyl) phenyl phosphine oxide polycondensate combines the advantages of the silicone oil, the amide and the phenyl phosphine oxide structure, so that the prepared polycondensate has good comprehensive performance, good wear resistance and excellent lubricating performance; the addition of 1, 3-dimethylimidazolium dimethylphosphate can further improve the above properties and effectively reduce coking.
Detailed Description
To make it possible toThe present invention will be described in detail with reference to the accompanying drawings, which are included to provide a further understanding of the invention. The examples are intended to illustrate the invention only and are not intended to limit the scope of the invention; the polyalphaolefin synthetic base oils referred to in the examples of the invention are produced for INEOS
170 poly-alpha-olefin synthetic base oil; the preparation method of the amino-terminated silicone oil is as follows: chinese invention patent example 1 with application number 201710145310.6; the preparation method of the rare earth oxide nanoparticles is disclosed in Chinese patent application example 1 with the application number of 201610381018. X; the preparation method of the metal organic framework with carboxyl is disclosed in the patent example 1 of Chinese invention with the application number of 201810731784.3; the number average molecular weight of the single-end amino polyethylene glycol is 2000; other raw materials were all purchased commercially.
Example 1
The lubricating oil composition is characterized by being prepared from the following components in parts by weight: 5 parts of ethoxy silicon-based ionized modified single-terminal amino polyethylene glycol carboxyl-containing metal organic framework salt, 3 parts of rare earth oxide nanoparticles, 15 parts of amino-terminal silicone oil/bis (4-carboxyphenyl) phenyl phosphine oxide polycondensate, 1 part of 1, 3-dimethyl imidazolium dimethyl phosphate and 45 parts of poly alpha-olefin synthetic base oil.
The preparation method of the amino-terminated silicone oil/bis (4-carboxyphenyl) phenylphosphine oxide polycondensate comprises the following steps: adding amino-terminated silicone oil and bis (4-carboxyphenyl) phenyl phosphine oxide into a high boiling point solvent, reacting for 1 hour at 150 ℃ under normal pressure, adding 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride and 4-dimethylaminopyridine into the solvent, heating to 210 ℃, carrying out primary polycondensation for 4 hours, transferring the reaction solution into a reaction kettle, vacuumizing to 500Pa, heating to 240 ℃, carrying out polycondensation for 8 hours, precipitating in water, carrying out suction filtration, washing for 3 times by using dichloromethane, and carrying out rotary evaporation to remove the dichloromethane to obtain the amino-terminated silicone oil/bis (4-carboxyphenyl) phenyl phosphine oxide polycondensate.
The mol ratio of the amino-terminated silicone oil, the bis (4-carboxyphenyl) phenylphosphine oxide, the high-boiling-point solvent, the 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride and the 4-dimethylaminopyridine is 1:1:6:0.6: 0.4; the high boiling point solvent is dimethyl sulfoxide.
The preparation method of the ethyoxyl silicon-based ionized modified single-terminal amino polyethylene glycol metal-organic framework salt with carboxyl comprises the following steps:
d1, adding amino polyethylene glycol and 3-chloropropyl trimethoxyl silane into ethanol, stirring and reacting for 4 hours at 50 ℃, and then performing rotary evaporation to remove ethanol to obtain an intermediate product;
and D2, adding the intermediate product prepared in the step D1 and the metal organic framework with carboxyl into N, N-dimethylformamide, stirring and reacting for 3 hours at 80 ℃, and then removing the N, N-dimethylformamide by rotary evaporation to obtain the ethyoxyl silicon-based ionized modified single-terminal amino polyethylene glycol metal organic framework salt with carboxyl.
In the step D1, the molar ratio of the single-end amino polyethylene glycol to the 3-chloropropyl trimethoxy silane to the ethanol is 1:3: 12.
The mass ratio of the intermediate product, the metal-organic framework with carboxyl and the N, N-dimethylformamide in the step D2 is 1:0.1: 5.
A method for preparing the lubricating oil composition is characterized by comprising the following steps: the components are evenly stirred according to the weight portion, and then are placed in a KH-700 type ultrasonic oscillator to be oscillated for 10 minutes under the power of 600W, so as to obtain the lubricating oil composition.
Example 2
The lubricating oil composition is characterized by being prepared from the following components in parts by weight: 6 parts of ethyoxyl silicon-based ionized modified single-terminal amino polyethylene glycol carboxyl-containing metal organic framework salt, 4 parts of rare earth oxide nanoparticles, 17 parts of amino-terminal silicone oil/bis (4-carboxyphenyl) phenyl phosphine oxide polycondensate, 1.2 parts of 1, 3-dimethyl imidazolium dimethyl phosphate and 47 parts of poly alpha-olefin synthetic base oil.
The preparation method of the amino-terminated silicone oil/bis (4-carboxyphenyl) phenylphosphine oxide polycondensate comprises the following steps: adding amino-terminated silicone oil and bis (4-carboxyphenyl) phenyl phosphine oxide into a high boiling point solvent, reacting for 1.5 hours at 155 ℃ under normal pressure, adding 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride and 4-dimethylaminopyridine into the solvent, heating to 215 ℃, carrying out primary polycondensation for 4.5 hours, transferring the reaction liquid into a reaction kettle, vacuumizing to 500Pa, heating to 245 ℃, carrying out polycondensation for 8.5 hours, precipitating in water, carrying out suction filtration, washing for 3-5 times by using dichloromethane, and carrying out rotary evaporation to remove the dichloromethane to obtain the amino-terminated silicone oil/bis (4-carboxyphenyl) phenyl phosphine oxide polycondensate.
The mol ratio of the amino-terminated silicone oil, the bis (4-carboxyphenyl) phenylphosphine oxide, the high-boiling-point solvent, the 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride and the 4-dimethylaminopyridine is 1:1:7:0.7: 0.4; the high boiling point solvent is dimethyl sulfoxide.
The preparation method of the ethyoxyl silicon-based ionized modified single-terminal amino polyethylene glycol metal-organic framework salt with carboxyl comprises the following steps:
step D1, adding amino polyethylene glycol and 3-chloropropyl trimethoxyl silane into ethanol, stirring and reacting for 4.5 hours at 55 ℃, and then performing rotary evaporation to remove ethanol to obtain an intermediate product;
and D2, adding the intermediate product prepared in the step D1 and the metal organic framework with carboxyl into N, N-dimethylformamide, stirring and reacting for 3.5 hours at 82 ℃, and then removing the N, N-dimethylformamide by rotary evaporation to obtain the ethyoxyl silicon-based ionized modified single-terminal amino polyethylene glycol metal organic framework salt with carboxyl.
In the step D1, the molar ratio of the single-end amino polyethylene glycol to the 3-chloropropyl trimethoxy silane to the ethanol is 1:3: 14.
The mass ratio of the intermediate product, the metal-organic framework with carboxyl and the N, N-dimethylformamide in the step D2 is 1:0.15: 6.
A method for preparing the lubricating oil composition is characterized by comprising the following steps: the components are evenly stirred according to the weight portion, and then are placed in a KH-700 type ultrasonic oscillator to be oscillated for 11 minutes under the power of 6200W, so as to obtain the lubricating oil composition.
Example 3
The lubricating oil composition is characterized by being prepared from the following components in parts by weight: 6.5 parts of ethyoxyl silicon-based ionized modified single-terminal amino polyethylene glycol carboxyl-containing metal organic framework salt, 4.5 parts of rare earth oxide nanoparticles, 20 parts of amino-terminated silicone oil/bis (4-carboxyphenyl) phenyl phosphine oxide polycondensate, 1.5 parts of 1, 3-dimethyl imidazolium dimethyl phosphate and 50 parts of poly alpha-olefin synthetic base oil.
The preparation method of the amino-terminated silicone oil/bis (4-carboxyphenyl) phenylphosphine oxide polycondensate comprises the following steps: adding amino-terminated silicone oil and bis (4-carboxyphenyl) phenyl phosphine oxide into a high boiling point solvent, reacting for 2 hours at 160 ℃ under normal pressure, adding 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride and 4-dimethylaminopyridine into the solvent, heating to 218 ℃, carrying out primary polycondensation for 5 hours, transferring the reaction solution into a reaction kettle, vacuumizing to 500Pa, heating to 250 ℃, carrying out polycondensation for 9 hours, precipitating in water, carrying out suction filtration, washing for 3-5 times by using dichloromethane, and carrying out rotary evaporation to remove the dichloromethane to obtain the amino-terminated silicone oil/bis (4-carboxyphenyl) phenyl phosphine oxide polycondensate.
The mol ratio of the amino-terminated silicone oil, the bis (4-carboxyphenyl) phenylphosphine oxide, the high-boiling-point solvent, the 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride and the 4-dimethylaminopyridine is 1:1:8:0.75: 0.4; the high boiling point solvent is N, N-dimethylformamide.
The preparation method of the ethyoxyl silicon-based ionized modified single-terminal amino polyethylene glycol metal-organic framework salt with carboxyl comprises the following steps:
step D1, adding amino polyethylene glycol and 3-chloropropyl trimethoxyl silane into ethanol, stirring and reacting for 5 hours at 60 ℃, and then performing rotary evaporation to remove ethanol to obtain an intermediate product;
and D2, adding the intermediate product prepared in the step D1 and the metal organic framework with carboxyl into N, N-dimethylformamide, stirring and reacting for 4 hours at 85 ℃, and then removing the N, N-dimethylformamide by rotary evaporation to obtain the ethyoxyl silicon-based ionized modified single-terminal amino polyethylene glycol metal organic framework salt with carboxyl.
In the step D1, the molar ratio of the single-end amino polyethylene glycol to the 3-chloropropyl trimethoxy silane to the ethanol is 1:3: 16.
The mass ratio of the intermediate product, the metal-organic framework with carboxyl and the N, N-dimethylformamide in the step D2 is 1:0.2: 7.5.
A method for preparing the lubricating oil composition is characterized by comprising the following steps: the components are uniformly stirred according to the parts by weight, and then are placed in a KH-700 type ultrasonic oscillator to be oscillated for 13 minutes under the power of 650W, so as to obtain the lubricating oil composition.
Example 4
The lubricating oil composition is characterized by being prepared from the following components in parts by weight: 7.5 parts of ethoxy silicon-based ionized modified single-terminal amino polyethylene glycol carboxyl-containing metal organic framework salt, 5.5 parts of rare earth oxide nanoparticles, 23 parts of amino-terminal silicone oil/bis (4-carboxyphenyl) phenyl phosphine oxide polycondensate, 1.8 parts of 1, 3-dimethyl imidazolium dimethyl phosphate and 53 parts of poly alpha-olefin synthetic base oil.
The preparation method of the amino-terminated silicone oil/bis (4-carboxyphenyl) phenylphosphine oxide polycondensate comprises the following steps: adding amino-terminated silicone oil and bis (4-carboxyphenyl) phenyl phosphine oxide into a high boiling point solvent, reacting for 2.5 hours at 165 ℃ under normal pressure, adding 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride and 4-dimethylaminopyridine into the solvent, heating to 223 ℃, carrying out primary polycondensation for 5.5 hours, transferring the reaction liquid into a reaction kettle, vacuumizing to 500Pa, heating to 255 ℃, carrying out polycondensation for 9.5 hours, precipitating in water, carrying out suction filtration, washing for 5 times by using dichloromethane, and carrying out rotary evaporation to remove the dichloromethane to obtain the amino-terminated silicone oil/bis (4-carboxyphenyl) phenyl phosphine oxide polycondensate.
The mol ratio of the amino-terminated silicone oil, the bis (4-carboxyphenyl) phenylphosphine oxide, the high-boiling-point solvent, the 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride and the 4-dimethylaminopyridine is 1:1:9.5:0.85: 0.4; the high boiling point solvent is N, N-dimethylacetamide.
The preparation method of the ethyoxyl silicon-based ionized modified single-terminal amino polyethylene glycol metal-organic framework salt with carboxyl comprises the following steps:
step D1, adding amino polyethylene glycol and 3-chloropropyl trimethoxyl silane into ethanol, stirring and reacting for 5.8 hours at 68 ℃, and then removing the ethanol by rotary evaporation to obtain an intermediate product;
and D2, adding the intermediate product prepared in the step D1 and the metal organic framework with carboxyl into N, N-dimethylformamide, stirring and reacting for 4.5 hours at 88 ℃, and then removing the N, N-dimethylformamide by rotary evaporation to obtain the ethyoxyl silicon-based ionized modified single-terminal amino polyethylene glycol metal organic framework salt with carboxyl.
In the step D1, the molar ratio of the single-end amino polyethylene glycol to the 3-chloropropyl trimethoxy silane to the ethanol is 1:3: 18.
The mass ratio of the intermediate product, the metal-organic framework with carboxyl and the N, N-dimethylformamide in the step D2 is 1:0.28: 9.
A method for preparing the lubricating oil composition is characterized by comprising the following steps: the components are stirred uniformly according to the weight portion, and then are put into a KH-700 type ultrasonic oscillator to be oscillated for 14 minutes under the power of 690W, so as to obtain the lubricating oil composition.
Example 5
The lubricating oil composition is characterized by being prepared from the following components in parts by weight: 8 parts of ethoxy silicon-based ionized modified single-terminal amino polyethylene glycol carboxyl-containing metal organic framework salt, 6 parts of rare earth oxide nanoparticles, 25 parts of amino-terminal silicone oil/bis (4-carboxyphenyl) phenyl phosphine oxide polycondensate, 2 parts of 1, 3-dimethyl imidazolium dimethyl phosphate and 55 parts of poly alpha-olefin synthetic base oil.
The preparation method of the amino-terminated silicone oil/bis (4-carboxyphenyl) phenylphosphine oxide polycondensate comprises the following steps: adding amino-terminated silicone oil and bis (4-carboxyphenyl) phenyl phosphine oxide into a high boiling point solvent, reacting for 3 hours at 170 ℃ under normal pressure, adding 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride and 4-dimethylaminopyridine into the solvent, heating to 225 ℃, carrying out primary polycondensation for 6 hours, transferring the reaction solution into a reaction kettle, vacuumizing to 500Pa, heating to 260 ℃, carrying out polycondensation for 10 hours, precipitating in water, carrying out suction filtration, washing for 5 times by using dichloromethane, and carrying out rotary evaporation to remove the dichloromethane to obtain the amino-terminated silicone oil/bis (4-carboxyphenyl) phenyl phosphine oxide polycondensate.
The mol ratio of the amino-terminated silicone oil, the bis (4-carboxyphenyl) phenylphosphine oxide, the high-boiling-point solvent, the 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride and the 4-dimethylaminopyridine is 1:1:10:0.9: 0.4; the high boiling point solvent is formed by mixing dimethyl sulfoxide, N-dimethylformamide, N-dimethylacetamide and N-methylpyrrolidone according to a mass ratio of 1:2:3: 2.
The preparation method of the ethyoxyl silicon-based ionized modified single-terminal amino polyethylene glycol metal-organic framework salt with carboxyl comprises the following steps:
step D1, adding amino polyethylene glycol and 3-chloropropyl trimethoxyl silane into ethanol, stirring and reacting for 6 hours at 70 ℃, and then performing rotary evaporation to remove ethanol to obtain an intermediate product;
and D2, adding the intermediate product prepared in the step D1 and the metal organic framework with carboxyl into N, N-dimethylformamide, stirring and reacting for 5 hours at 90 ℃, and then removing the N, N-dimethylformamide by rotary evaporation to obtain the ethyoxyl silicon-based ionized modified single-terminal amino polyethylene glycol metal organic framework salt with carboxyl.
In the step D1, the molar ratio of the single-end amino polyethylene glycol to the 3-chloropropyl trimethoxy silane to the ethanol is 1:3: 20.
The mass ratio of the intermediate product, the metal-organic framework with carboxyl and the N, N-dimethylformamide in the step D2 is 1:0.3: 10.
A method for preparing the lubricating oil composition is characterized by comprising the following steps: the components are evenly stirred according to the weight portion, and then are placed in a KH-700 type ultrasonic oscillator to be oscillated for 15 minutes under the power of 700W, so as to obtain the lubricating oil composition.
Comparative example 1
This example provides a lubricating oil composition having substantially the same formulation and preparation as example 1, except that no rare earth oxide nanoparticles were added.
Comparative example 2
This example provides a lubricating oil composition having substantially the same formulation and preparation as in example 1, except that 1, 3-dimethylimidazolium dimethylphosphate was not added.
Comparative example 3
This example provides a lubricating oil composition having substantially the same formulation and method of manufacture as in example 1, except that no amino-terminated silicone oil/bis (4-carboxyphenyl) phenylphosphine oxide polycondensate was added.
Comparative example 4
This example provides a lubricating oil composition having substantially the same formulation and preparation as in example 1, except that no carboxyl-containing metal organic framework salt of an ethoxylated silicon-based ionically-modified single-terminal amino polyethylene glycol is added.
Comparative example 5
This example provides a lubricating oil composition having substantially the same formulation and preparation as in example 1, except that a carboxyl-containing metal organic framework is used in place of the carboxyl-containing metal organic framework salt of the ethoxylated silicon-based ionically-modified single-terminal amino polyethylene glycol.
The lubricating oil compositions obtained in examples 1 to 5 and comparative examples 1 to 5 were subjected to respective performance tests, and the results are shown in Table 1. The test method is as follows:
four-ball experiment: 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.
As can be seen from Table 1, the lubricating oil compositions disclosed in the examples of the present invention have better extreme pressure and lubricating properties as a result of the synergistic effect of the components.
TABLE 1 Properties of samples of examples and comparative examples
| Item | Maximum No-seize negative (PB)/N (kg) | Sintering load (PD)/N (kg) | Abrasive grain diameter d/mm |
| Example 1 | 96 | 168 | 0.20 |
| Example 2 | 98 | 170 | 0.17 |
| Example 3 | 101 | 173 | 0.15 |
| Example 4 | 103 | 176 | 0.12 |
| Example 5 | 106 | 178 | 0.10 |
| Comparative example 1 | 72 | 137 | 0.35 |
| Comparative example 2 | 74 | 141 | 0.31 |
| Comparative example 3 | 75 | 144 | 0.37 |
| Comparative example 4 | 69 | 131 | 0.33 |
| Comparative example 5 | 72 | 135 | 0.31 |
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 lubricating oil composition is characterized by being prepared from the following components in parts by weight: 5-8 parts of ethoxy silicon-based ionized modified single-terminal amino polyethylene glycol carboxyl-containing metal organic framework salt, 3-6 parts of rare earth oxide nanoparticles, 15-25 parts of amino-terminated silicone oil/bis (4-carboxyphenyl) phenyl phosphine oxide polycondensate, 1-2 parts of 1, 3-dimethyl imidazolium dimethyl phosphate and 45-55 parts of poly alpha-olefin synthetic base oil.
2. The lubricating oil composition of claim 1, wherein the polyalphaolefin synthetic base oil is INEOS-produced
170 poly-alpha-olefin synthetic base oil.
3. Lubricating oil composition according to claim 1, characterized in that the method for preparing the amino-terminated silicone oil/bis (4-carboxyphenyl) phenylphosphine oxide polycondensate comprises the steps of: adding amino-terminated silicone oil and bis (4-carboxyphenyl) phenylphosphine oxide into a high-boiling-point solvent, reacting for 1-3 hours at the temperature of 150 ℃ and 170 ℃ under normal pressure, adding 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride and 4-dimethylaminopyridine into the solvent, heating to the temperature of 210 ℃ and 225 ℃, carrying out primary polycondensation for 4-6 hours, transferring the reaction liquid into a reaction kettle, vacuumizing to 500Pa, heating to the temperature of 240 ℃ and 260 ℃, carrying out polycondensation for 8-10 hours, precipitating in water, carrying out suction filtration, washing for 3-5 times by using dichloromethane, and carrying out rotary evaporation to remove the dichloromethane to obtain the amino-terminated silicone oil/bis (4-carboxyphenyl) phenylphosphine oxide polycondensate.
4. The lubricating oil composition of claim 3, wherein the molar ratio of amino-terminated silicone oil, bis (4-carboxyphenyl) phenylphosphine oxide, high boiling point solvent, 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride, 4-dimethylaminopyridine is 1:1 (6-10) to (0.6-0.9) to 0.4.
5. The lubricating oil composition according to claim 3, wherein the high boiling point solvent is at least one of dimethylsulfoxide, N-dimethylformamide, N-dimethylacetamide, and N-methylpyrrolidone.
6. The lubricating oil composition as claimed in claim 1, wherein the preparation method of the carboxyl-bearing metal organic framework salt of the ethoxylated silicon-based ionized modified single-ended amino polyethylene glycol comprises the following steps:
step D1, adding amino polyethylene glycol and 3-chloropropyl trimethoxyl silane into ethanol, stirring and reacting for 4-6 hours at 50-70 ℃, and then performing rotary evaporation to remove ethanol to obtain an intermediate product;
and D2, adding the intermediate product prepared in the step D1 and the metal organic framework with carboxyl into N, N-dimethylformamide, stirring and reacting for 3-5 hours at 80-90 ℃, and then removing the N, N-dimethylformamide by rotary evaporation to obtain the ethyoxyl silicon-based ionized modified single-terminal amino polyethylene glycol metal organic framework salt with carboxyl.
7. The lubricating oil composition of claim 6, wherein the molar ratio of the single-ended amino polyethylene glycol, the 3-chloropropyltrimethoxysilane and the ethanol in step D1 is 1:3 (12-20).
8. The lubricating oil composition of claim 6, wherein the number average molecular weight of the single-terminal amino polyethylene glycol is 2000.
9. The lubricating oil composition according to claim 6, wherein the mass ratio of the intermediate product, the metal-organic framework having carboxyl groups, and N, N-dimethylformamide in the step D2 is 1 (0.1-0.3) to 5-10.
10. A method for preparing a lubricating oil composition according to any one of claims 1 to 9, comprising the steps of: the components are uniformly stirred according to the parts by weight and then are placed in a KH-700 type ultrasonic oscillator to be oscillated for 10-15 minutes under the power of 600-700W, so as to obtain the lubricating oil composition.
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