CN112920875A - Vehicle lubricating oil additive with semi-solid high-strength membrane, synthetic method of vehicle lubricating oil additive and lubricating oil - Google Patents

Vehicle lubricating oil additive with semi-solid high-strength membrane, synthetic method of vehicle lubricating oil additive and lubricating oil Download PDF

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CN112920875A
CN112920875A CN202110158326.7A CN202110158326A CN112920875A CN 112920875 A CN112920875 A CN 112920875A CN 202110158326 A CN202110158326 A CN 202110158326A CN 112920875 A CN112920875 A CN 112920875A
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lubricating oil
molybdenum
oil additive
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additive
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方道宝
池素玲
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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
    • C10M125/00Lubricating compositions characterised by the additive being an inorganic material
    • C10M125/04Metals; Alloys
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2201/00Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/04Elements
    • C10M2201/05Metals; Alloys
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2201/00Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/06Metal compounds
    • C10M2201/062Oxides; Hydroxides; Carbonates or bicarbonates
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2201/00Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/08Inorganic acids or salts thereof
    • 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
    • C10M2207/00Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/28Esters
    • C10M2207/281Esters of (cyclo)aliphatic monocarboxylic acids
    • 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
    • C10M2215/00Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
    • C10M2215/02Amines, e.g. polyalkylene polyamines; Quaternary amines
    • C10M2215/04Amines, e.g. polyalkylene polyamines; Quaternary amines having amino groups bound to acyclic or cycloaliphatic carbon atoms
    • 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
    • C10M2215/00Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
    • C10M2215/02Amines, e.g. polyalkylene polyamines; Quaternary amines
    • C10M2215/06Amines, e.g. polyalkylene polyamines; Quaternary amines having amino groups bound to carbon atoms of six-membered aromatic rings
    • C10M2215/064Di- and triaryl amines
    • 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
    • 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
    • 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
    • C10M2227/00Organic 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
    • C10M2227/06Organic compounds derived from inorganic acids or metal salts
    • C10M2227/066Organic compounds derived from inorganic acids or metal salts derived from Mo or W

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Metallurgy (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Organic Chemistry (AREA)
  • Lubricants (AREA)

Abstract

The invention relates to the technical field of lubricating oil additives, in particular to a semi-solid high-strength membrane vehicle lubricating oil additive, a synthetic method thereof and lubricating oil. The molybdenum oxide is used as a base to react with o-aminobenzenesulfonic acid and alkylated diphenylamine, potassium permanganate is added, a method for adjusting the pH value is adopted to obtain an organic molybdenum amine mixture which is favorable for the next good reaction, and then the organic molybdenum amine mixture reacts with calcium titanate, methyl methacrylate and didodecyl methyl tertiary amine, and a two-step pressure method is adopted, so that the molybdenum-titanium alloy lubricating oil additive with good lubricity and excellent wear resistance is prepared, is dissolved in various lubricating oils in a liquid ion form, is a friction modifier, an anti-wear agent and an antioxidant of lubricating oil for internal combustion engines, has an obvious oil saving effect, and can obviously improve the film forming and bearing capacity of the lubricating oil. Forming a chemical adsorption film with the functions of friction reduction and wear resistance on the friction surface; under the harsh working conditions of high speed, high temperature, high pressure and the like, the engine is further protected.

Description

Vehicle lubricating oil additive with semi-solid high-strength membrane, synthetic method of vehicle lubricating oil additive and lubricating oil
Technical Field
The invention relates to the technical field of lubricating oil additives, in particular to a semi-solid high-strength membrane vehicle lubricating oil additive, a synthetic method thereof and lubricating oil.
Background
The friction pair surface of modern engine is added with a layer of pre-lubricating material, the vehicle uses for a long time, the pre-lubricating material is consumed, and the general requirement of modern engine is to send out larger power on the premise of small volume and light weight, and the increasingly strict energy-saving and environmental protection requirements bring about the great increase of the engine power, and the piston connecting rod is shortened, and the load at the parts of piston ring and cylinder wall, valve tappet and cam, crankshaft and bearing bush, etc. which are the most strict in the working condition of the engine is greatly increased. In the case of an electronic fuel injection engine, especially a supercharged engine, high-temperature parts of the engine, such as pistons and cylinder walls, superchargers and the like, are considered to be more and more serious due to the problem of abrasion caused by a thin oil film. The conventional lubricating oil has the urgent requirements on corrosion resistance and abrasion resistance while the quality level is continuously improved so as to meet the requirements of overall lubrication and oil sludge dispersion of an engine.
The solid lubricant additive can avoid the friction effect generated by the forced fracture of substances between sliding surfaces, and the typical types of the solid lubricant additive are three types:
(one) inorganic layered structure substance: graphite, molybdenum disulfide, boron nitride, titanium metal, and the like. Compared with common lubricating oil, the titanium metal lubricating oil has three outstanding characteristics: (1) the titanium metal has strong corrosion resistance, and a layer of blunt oxide protective film can be generated when the engine is exposed to high-temperature air, so that when the engine is in a high-pressure and high-speed running state, the titanium lubricating oil can automatically track pressure points to generate a protective film, thereby reducing the abrasion of the engine and better protecting the engine; (2) the self-repairing titanium is used as liquid metal to enter the engine, so that the oxidation resistance of the engine can be improved, and the self-repairing titanium has a self-repairing function. The titanium-added engine oil forms a protective film at the most frequent friction place of the engine, which is like adding a wear-resistant shield to the wear point of the engine, and the engine can run for a longer time because the engine is protected at the molecular level; (3) the titanium lubricating oil for improving the heat dissipation of the automobile has very strong heat dissipation effect;
molybdenum disulfide is added after the renewal of four-generation products:
first generation molybdenum: molybdenum disulfide du (MoS2) is directly applied to bai, molybdenum disulfide is solid powder prepared by changing a molecular structure of molybdenum concentrate powder after chemical purification, the product is slightly silvery-gray in color black, has metallic luster and greasy feeling when being touched, is a good solid lubricant, is solid and cannot be dissolved in oil, and is only adopted in some lubricating grease at present.
Second generation molybdenum: sulfur-phosphorus-oxygen (S-P-O) organomolybdenum, starting to produce molybdenum dialkyl dithiosulfate (MODDP). The oil solubility of the product is improved, but the problem is not solved, sediment or gas generated by product decomposition can be generated when the process is unstable, and the phosphorus content is high, so that the poisoning of a tail gas catalyst is influenced, and the product is rarely applied at home and abroad at present.
Third-generation molybdenum: molybdenum alkyl dithiocarbamates (MoDTC), sulfur (S) -containing phosphorus (P) -free organomolybdenum, and in the eighth and ninety last century lubricating oil additive manufacturers developed to produce molybdenum dialkyl dithiocarbamates that, while phosphorus-free, are not oil soluble, friction reducing, and oxidation resistant, and that present a risk of corrosion and corrosion.
Fourth generation molybdenum: the product is the latest product which is pushed out in the century, is quite stable, solves the problem of oil solubility thoroughly, has low phosphorus content which is almost zero, has the greatest advantage of containing nitrogen and good high-temperature oxidation resistance, is widely used in high-grade SN lubricating oil with limit of S, P, and represents the development trend of organic molybdenum additives.
(II) Polymer Compound: the main representatives are polytetrafluoroethylene and nylon, polytetrafluoroethylene was originally used in grease and can now also be used in lubricating oil.
Cyanuric acid complex (MCA) is mainly used for light-duty grease and solder paste.
The solid lubricant additive has excellent performances of forming a film layer, reducing friction and the like through a direct action of a physical action mechanism at low temperature and high temperature, but when the solid lubricant is used in engine oil and gear oil, the solid lubricant needs to be stably dispersed in the oil, the particle size of solid particles is required to be in a range of 0.1-100 nanometers, and the solid lubricant cannot be coagulated, precipitated and block a filter and an oil pipe of a lubricating oil system under the condition of high and low temperature change to cause oil supply failure. At present, enough lubricating film layers can still be maintained at high temperature, lubricating oil flow failure cannot be caused at low temperature, or friction force is increased due to film layer thickness or film layer cracking, and the like, wherein the antiwear agents are mainly organic antiwear additives containing sulfur, phosphorus and nitrogen or containing boron, molybdenum, tungsten or rare earth elements, and additives synthesized based on graphene technology, nanotechnology and boron, molybdenum and tungsten technology. However, due to the pollution of the existing phosphorus-containing additive to the catalyst of the exhaust gas treatment device, more and more lubricating oil additives are concerned in the recent years that the phosphorus-free additive and the oil-soluble semi-solid high-strength film additive, such as the oil-soluble organic molybdenum additive, have excellent friction reduction and wear resistance. In view of this, research and development of a new lubricating oil additive have been carried out, which solves the defects of the existing additives, improves the protective effect of lubricating oil on engines, and becomes a problem to be solved urgently in the research and development process of lubricating oil additives.
Disclosure of Invention
In order to overcome the defects of the prior art, one of the purposes of the invention is to provide a semi-solid high-strength film vehicle lubricating oil additive, which contains molybdenum-titanium intelligent metal particles, can be automatically polymerized to a friction damaged part under the action of pressure and friction heat, and realizes intelligent dynamic repair. The worn engine can be quickly repaired, and the phenomena of engine oil burning, blue smoke emission and the like caused by wear are eliminated; the sealing performance of the cylinder and the power of the engine are recovered, the noise of the engine is reduced, the emission of harmful gas is reduced, the sealing performance of the cylinder and the power of the engine are recovered, the noise of the engine is reduced, and the emission of the harmful gas is reduced. The additive of the invention is safe and stable and can be compatible with various engine oils.
The invention also aims to provide a synthetic method of the semi-solid high-strength membrane vehicle lubricating oil additive.
The invention also aims to provide lubricating oil added with the lubricating oil additive.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a synthetic method of a semi-solid high-strength membrane vehicle lubricating oil additive comprises the following operation steps:
1) synthesis of organic molybdenum amine mixture:
putting molybdenum oxide, o-aminobenzenesulfonic acid and alkylated diphenylamine in a container, reacting for 2-3 hours at 140-150 ℃ under a sealed condition, then carrying out alkali washing and water washing, adjusting the pH value to be 6.5-7, adding potassium permanganate, continuing to react for 3-4 hours at 90-100 ℃, carrying out vacuum filtration to obtain a precipitate, and washing to be neutral to obtain an organic molybdenum amine mixture; wherein the weight ratio of molybdenum oxide, o-aminobenzenesulfonic acid, alkylated diphenylamine and potassium permanganate is 1: 3-5: 3-5: 7-10;
2) synthesizing the molybdenum-titanium alloy lubricating oil additive:
mixing the organic molybdenum amine mixture prepared in the step 1) with calcium titanate and methyl methacrylate, uniformly stirring, and reacting for 4-5 hours at 90-100 ℃ and under the pressure of 0.24-0.3 MPa; cooling to 50-60 ℃, adding didodecyl methyl tertiary amine, increasing the temperature to 180-190 ℃, continuously reacting for 3-4 hours under the condition of unchanged pressure, then cooling to 85-100 ℃, vacuumizing to 0.075-0.094 MPa, and filtering to obtain a yellow oil-soluble molybdenum-titanium alloy lubricating oil additive; wherein the weight ratio of the organic molybdenum amine mixture, the calcium titanate, the methyl methacrylate to the didodecyl methyl tertiary amine is 1: 5-8: 15-20: 15 to 20.
Preferably, in the step 1), the weight ratio of the molybdenum oxide, the o-aminobenzenesulfonic acid, the alkylated diphenylamine and the potassium permanganate is 1: 4: 4: 8.
preferably, the weight ratio of the organic molybdenum amine mixture, calcium titanate, methyl methacrylate and didodecyl methyl tertiary amine in the step 2) is 1: 6: 16: 16.
a semi-solid high-strength film additive for lubricating oil for car is prepared by said synthesizing process.
A lubricating oil, which contains the semi-solid high-strength film vehicle lubricating oil additive. Preferably, the mass percentage of the vehicle lubricating oil additive is 0.8-1%.
The lubricating oil additive for the vehicle is a molybdenum-titanium alloy lubricating oil additive synthesized based on a semi-solid high-strength membrane technology, and is different from dialkyl molybdenum dithiophosphate in that the molybdenum does not contain phosphorus elements in molecules, so that the pollution of the phosphorus elements to a catalyst of a tail gas processor is avoided. In the invention, firstly, molybdenum oxide is taken as a base to react with o-aminobenzenesulfonic acid and alkylated diphenylamine, potassium permanganate is added, a method of adjusting the pH value is adopted to obtain an organic molybdenum amine mixture which is favorable for the next good reaction, then the organic molybdenum amine mixture reacts with calcium titanate, methyl methacrylate and didodecyl methyl tertiary amine, a two-step pressure method is adopted, so that a molybdenum-titanium alloy lubricating oil additive with good lubricity and excellent wear resistance is prepared, the molybdenum-titanium alloy lubricating oil additive is dissolved in various lubricating oils in a liquid ion form, 1 percent of the vehicle lubricating oil additive with the semi-solid high-strength membrane synthesized by the invention is added into engine oil, the friction coefficient can be reduced to below 0.0298 and below 0.027 (the friction coefficient of the conventional engine oil is above 0.08), a four-ball machine 40 kg force long-rubbing test is carried out for 60 minutes, the diameter of a wear scar is reduced to below 0.35mm, and the minimum diameter is only 0.31mm (the diameter, the temperature reached 50 degrees and did not increase further. The lubricating oil is a friction modifier, an antiwear agent and an antioxidant of the lubricating oil for internal combustion engines, has obvious oil saving effect, and can obviously improve the film forming and bearing capacity of the lubricating oil. Under the normal working condition of the lubricating part, a chemical adsorption film with the functions of friction reduction and wear resistance is formed on the friction surface; under the harsh working conditions of high speed, high temperature, high pressure and the like, the engine is further protected.
The vehicle lubricating oil additive has the following advantages:
(1) the low-temperature fluidity of the fully synthetic engine oil is improved by 20 percent compared with the low-temperature fluidity of the traditional fully synthetic engine oil, and the best protection is formed at the starting moment; exhibits remarkably improved high-temperature oxidation resistance (thermal stability), and is capable of effectively improving the (high-temperature) oxidation stability of, for example, lubricating oil;
(2) the fuel oil is saved more strongly, the low-speed resistance is high, the abnormal sound of the engine is effectively eliminated, and the future development trend of low carbon, environmental protection and energy conservation in the automobile industry is met;
(3) the economy of the engine fuel is improved by 3.4%, the engine oil consumption is reduced by 25%, the antifriction capability is improved by 30%, and the performance is enhanced, so that the engine is protected, and the intermetallic friction affecting the power performance is reduced under different engine rotating speeds and driving environments;
(4) the cleanliness of the engine exceeds the standard value by 15 percent, and the fuel economy exceeds the standard 2.6 percent and the viscosity resistance is increased;
(5) the oil film has good adsorption performance and extremely high heat dissipation coefficient, the power of the engine is greatly improved by more than 10%, the oil consumption is saved by 2.5%, the noise is effectively reduced by more than 10%, the abrasion of the engine is effectively repaired, and the generation of oil sludge carbon deposition is inhibited;
(6) the automobile exhaust treatment system is effectively protected, the exhaust emission is reduced, and comprehensive protection is provided for novel engines such as turbocharging;
(7) the engine has high cleaning performance, and can keep various functions of the engine such as newly improving the working efficiency of the engine and keeping the continuous and stable power output of the engine.
Detailed Description
Preferred embodiments of the present invention will be described in detail with reference to the following examples. It is to be understood that the following examples are given for illustrative purposes only and are not intended to limit the scope of the present invention. Various modifications and substitutions may be made by those skilled in the art without departing from the spirit and scope of the invention, and all such modifications and substitutions are intended to be within the scope of the claims.
The experimental procedures used in the following examples are all conventional procedures unless otherwise specified. Materials, reagents and the like used in the following examples are commercially available unless otherwise specified.
Example 1
The embodiment provides a vehicle lubricating oil additive with a semi-solid high-strength membrane, and the synthesis method comprises the following steps:
1) synthesis of organic molybdenum amine mixture:
putting molybdenum oxide, o-aminobenzenesulfonic acid and alkylated diphenylamine in a container, reacting for 2 hours at 150 ℃ under a sealed condition, then carrying out alkali washing and water washing, adjusting the pH to 6.5, adding potassium permanganate, continuing to react for 3 hours at the temperature of 80-100 ℃, then carrying out vacuum filtration to obtain a precipitate, and washing to be neutral to obtain a brown substance which is an organic molybdenum amine mixture; molybdenum oxide o-aminobenzenesulfonic acid, alkylated diphenylamine: 1-potassium permanganate: 4: 4: 8 (weight ratio);
2) synthesizing the molybdenum-titanium alloy lubricating oil additive:
5 g of the prepared organic molybdenum amine mixture is mixed with 25 g of calcium titanate and 75 g of methyl methacrylate, and the mixture is reacted for 4 hours at the temperature of 90 ℃ and the pressure of 0.3MPa after being uniformly stirred; cooling to 50 ℃, adding 75 g of didodecyl methyl tertiary amine, increasing the temperature to 180 ℃, continuously reacting for 3 hours under the condition of constant pressure, then cooling to 100 ℃, and vacuumizing to 0.094 MPa; and finally, filtering to obtain the yellow molybdenum-titanium alloy lubricating oil additive, namely the semi-solid high-strength membrane vehicle lubricating additive provided by the embodiment.
Examination of antifriction and antiwear properties and load-bearing capacity of the product of this example: the four-ball machine is used for measuring, the extreme pressure and the antifriction and antiwear performance under the load (the temperature is 25 ℃, the load is 392N, the speed is 1200-1500R/min, and the time is 60min) are set, the steel ball used in the four-ball test is a GCR steel ball with the diameter of 12.2-12.7 mm, and the test shows that the product has good extreme pressure and antifriction and antiwear performance. By contrast, lubricating oil was directly used, and the diameter of the wear scar reached 0.7 mm. 1 wt% of the product prepared in this example was added to API SN0W/40 lubricating oil, and the resulting lubricating oil had a wear scar diameter of 0.35mm and a coefficient of friction of 0.0289.
Example 2
1) Synthesis of organic molybdenum amine mixture:
putting molybdenum oxide, o-aminobenzenesulfonic acid and alkylated diphenylamine in a container, reacting for 2.5 hours at 140 ℃ under a sealed condition, then carrying out alkali washing and water washing, adjusting the pH to 7, adding potassium permanganate, continuing to react for 3.5 hours at the temperature of 90 ℃, then carrying out vacuum filtration to obtain a precipitate, and washing to be neutral to obtain a brown substance which is an organic molybdenum amine mixture; molybdenum oxide o-aminobenzenesulfonic acid, alkylated diphenylamine: 1-potassium permanganate: 5: 5: 10 (weight ratio);
2) synthesizing the molybdenum-titanium alloy lubricating oil additive:
mixing 10 g of the prepared organic molybdenum amine mixture with 60 g of calcium titanate and 160 g of methyl methacrylate, uniformly stirring, and reacting for 5 hours at the temperature of 100 ℃ and the pressure of 0.24 MPa; cooling to 60 ℃, adding 160 g of didodecyl methyl tertiary amine, increasing the temperature to 190 ℃, continuously reacting for 4 hours under the condition of constant pressure, then cooling to 100 ℃, and vacuumizing to 0.094 MPa; and finally, filtering to obtain the yellow molybdenum-titanium alloy lubricating oil additive, namely the semi-solid high-strength membrane vehicle lubricating additive provided by the embodiment.
This example provides a review of the antifriction and antiwear properties and load bearing capabilities of the product: the four-ball machine is used for measuring, the extreme pressure and antifriction and antiwear performance under the load (the temperature is 25 ℃, the load is 392N, the speed is 1200-1500R/min, and the time is 60min) is set, the steel ball used in the four-ball test is a GCR steel ball with the diameter of 12.7mm, and the test shows that the product has good extreme pressure and antifriction and antiwear performance. By contrast, lubricating oil was directly used, and the diameter of the wear scar reached 0.7 mm. 1% by weight of the product prepared in this example was added to an API SN0W/40 lubricating oil to give a wear scar of 0.32mm in diameter and a coefficient of friction of 0.0271.
Example 3
1) Synthesis of organic molybdenum amine mixture:
putting molybdenum oxide, o-aminobenzenesulfonic acid and alkylated diphenylamine in a container, reacting for 3 hours at 145 ℃ under a sealed condition, then carrying out alkali washing and water washing, adjusting the pH to be 6.5, adding potassium permanganate, continuously reacting for 4 hours at 95 ℃, then carrying out vacuum filtration to obtain a precipitate, and washing to be neutral to obtain a brown substance, namely an organic molybdenum amine mixture; molybdenum oxide o-aminobenzenesulfonic acid, alkylated diphenylamine: 1-potassium permanganate: 3: 3: 9 (weight ratio);
2) synthesizing the molybdenum-titanium alloy lubricating oil additive:
mixing 40 g of the prepared organic molybdenum amine mixture with 320 g of calcium titanate and 800 g of methyl methacrylate, uniformly stirring, and reacting for 4.5 hours at the temperature of 95 ℃ and under the pressure of 0.28 MPa; cooling to 50 ℃, adding 800 g of didodecyl methyl tertiary amine, increasing the temperature to 185 ℃, continuously reacting for 3.5 hours under the condition of constant pressure, then cooling to 85 ℃, and vacuumizing to 0.075 MPa; and finally, filtering to obtain the yellow molybdenum-titanium alloy lubricating oil additive, namely the semi-solid high-strength membrane vehicle lubricating additive provided by the embodiment.
This example provides a review of the antifriction and antiwear properties and load bearing capabilities of the product: the four-ball machine is used for measuring, the extreme pressure and antifriction and antiwear performance under the load (the temperature is 25 ℃, the load is 392N, the speed is 1200-1500R/min, and the time is 60min) is set, the steel ball used in the four-ball test is a GCR steel ball with the diameter of 12.7mm, and the test shows that the product has good extreme pressure and antifriction and antiwear performance. By contrast, lubricating oil was directly used, and the diameter of the wear scar reached 0.7 mm. 0.8 wt% of the product prepared in the embodiment is added into API SN0W/40 lubricating oil, the diameter of the abrasive spot reaches 0.28-0.33 mm, and the friction coefficient is 0.0245-0.0285.
Example 4
1) Synthesis of organic molybdenum amine mixture:
putting molybdenum oxide, o-aminobenzenesulfonic acid and alkylated diphenylamine in a container, reacting for 3 hours at 150 ℃ under a sealed condition, then carrying out alkali washing and water washing, adjusting the pH to be 7, adding potassium permanganate, continuing to react for 3 hours at the temperature of 95-100 ℃, then carrying out vacuum filtration to obtain a precipitate, and washing to be neutral to obtain a brown substance which is an organic molybdenum amine mixture; molybdenum oxide o-aminobenzenesulfonic acid, alkylated diphenylamine: 1-potassium permanganate: 4.5: 4.5: 7 (weight ratio);
2) synthesizing the molybdenum-titanium alloy lubricating oil additive:
mixing 15 g of the prepared molybdenum-titanium synthetic semi-solid high-strength film technology with 105 g of calcium titanate and 285 g of methyl methacrylate, uniformly stirring, and reacting for 4 hours at the temperature of 95 ℃ and the pressure of 0.3 MPa; cooling to 60 ℃, adding 285 g of didodecyl methyl tertiary amine, increasing the temperature to 190 ℃, continuously reacting for 3 hours under the condition of constant pressure, then cooling to 90 ℃, and vacuumizing to 0.094 MPa; and finally, filtering to obtain the yellow molybdenum-titanium alloy lubricating oil additive, namely the semi-solid high-strength membrane vehicle lubricating additive provided by the embodiment.
This example provides a review of the antifriction and antiwear properties and load bearing capabilities of the product: the four-ball machine is used for measuring, the extreme pressure and antifriction and antiwear performance under the load (the temperature is 25 ℃, the load is 392N, the speed is 1200-1500R/min, and the time is 60min) is set, the steel ball used in the four-ball test is a GCR steel ball with the diameter of 12.7mm, and the test shows that the product has good extreme pressure and antifriction and antiwear performance. By contrast, lubricating oil was directly used, and the diameter of the wear scar reached 0.7 mm. 1 percent (weight) of the product prepared in the embodiment is added into API SN0W/40 lubricating oil, the diameter of the abrasive wear scar reaches 0.28-0.31 mm, and the friction coefficient is 0.0270-0.0298.
Example 5
1) Synthesis of organic molybdenum amine mixture:
putting molybdenum oxide, o-aminobenzenesulfonic acid and alkylated diphenylamine in a container, reacting for 2 hours at 150 ℃ under a sealed condition, then carrying out alkali washing and water washing, adjusting the pH to 6.5, adding potassium permanganate, continuing to react for 3 hours at the temperature of 100 ℃, then carrying out vacuum filtration to obtain a precipitate, and washing to be neutral to obtain a brown substance, namely an organic molybdenum amine mixture; molybdenum oxide o-aminobenzenesulfonic acid, alkylated diphenylamine: 1-potassium permanganate: 4: 4: 8 (weight ratio);
2) synthesizing the molybdenum-titanium alloy lubricating oil additive:
mixing 10 g of the prepared organic molybdenum amine mixture with 60 g of calcium titanate and 160 g of methyl methacrylate, uniformly stirring, and reacting for 5 hours at the temperature of 100 ℃ and the pressure of 0.3 MPa; cooling to 60 ℃, adding 160 g of didodecyl methyl tertiary amine, increasing the temperature to 190 ℃, continuously reacting for 4 hours under the condition of constant pressure, then cooling to 100 ℃, and vacuumizing to 0.094 MPa; and finally, filtering to obtain the yellow molybdenum-titanium alloy lubricating oil additive, namely the semi-solid high-strength membrane vehicle lubricating additive provided by the embodiment.
This example provides a review of the antifriction and antiwear properties and load bearing capabilities of the product: the four-ball machine is used for measuring, the extreme pressure and antifriction and antiwear performance under the load (the temperature is 25 ℃, the load is 392N, the speed is 1200-1500R/min, and the time is 60min) is set, the steel ball used in the four-ball test is a GCR steel ball with the diameter of 12.7mm, and the test shows that the product has good extreme pressure and antifriction and antiwear performance. By contrast, lubricating oil was directly used, and the diameter of the wear scar reached 0.7 mm. 1 percent (weight) of the product prepared by the embodiment is added into API SN0W/40 lubricating oil, the diameter of the wear scar reaches 0.26-0.28 mm, and the friction coefficient is 0.0212-0.0216.
Test examples
The comprehensive properties of the products provided in the above examples were measured, and the results are shown in tables 1 and 2 below:
TABLE 1
Figure BDA0002935294970000101
TABLE 2
Figure BDA0002935294970000102
Figure BDA0002935294970000111
The comprehensive performance test of the lubricating oil additive provided by the invention shows that the additive has the following advantages compared with the traditional additive:
(1) the semi-solid high-strength film vehicle lubricating oil additive synthesized by utilizing the organic molybdenum and the titanium does not contain phosphorus elements and metal elements, is not easy to generate ash, and is an environment-friendly antioxidant;
(2) compared with the compound in the prior art, the semi-solid high-strength film vehicle lubricating oil additive synthesized by organic molybdenum and titanium shows remarkably improved high-temperature oxidation resistance (thermal stability), and can effectively improve the (high-temperature) oxidation stability of lubricating oil;
(3) the semi-solid high-strength film vehicle lubricating oil additive synthesized by organic molybdenum and titanium shows excellent high-temperature oxidation resistance and also further shows excellent antirust performance;
(4) the semi-solid high-strength film vehicle lubricating oil additive synthesized by organic molybdenum and titanium shows excellent high-temperature oxidation resistance and simultaneously further shows excellent cleaning performance (namely deposit generation inhibition performance);
(5) the semi-solid high-strength film vehicle lubricating oil additive synthesized by organic molybdenum and titanium shows excellent high-temperature oxidation resistance, and further shows excellent performance of inhibiting viscosity increase and acid value increase;
in conclusion, the vehicle lubricating oil additive can be applied to gasoline and diesel engine lubricating oil, shows excellent oxidation resistance, clean dispersion performance, wear resistance and antirust performance, effectively repairs all parts of an engine to work in a severe environment, greatly improves the working efficiency of the engine, has the advantages of energy conservation, environmental protection and low carbon travel, and completely meets the requirements of national development tendency. Fully meets the requirements of gasoline and diesel engine oil products with specifications of SP/SN A3/B4/SL and diesel engine oil CK/CI/CH/CF/GL and above.
Although the invention has been described in detail above with reference to a general description and specific examples, it will be apparent to one skilled in the art that modifications or improvements may be made thereto based on the invention. Accordingly, such modifications and improvements are intended to be within the scope of the invention as claimed.

Claims (6)

1. The synthesis method of the semi-solid high-strength membrane vehicle lubricating oil additive is characterized by comprising the following operation steps of:
1) synthesis of organic molybdenum amine mixture:
putting molybdenum oxide, o-aminobenzenesulfonic acid and alkylated diphenylamine in a container, reacting for 2-3 hours at 140-150 ℃ under a sealed condition, then carrying out alkali washing and water washing, adjusting the pH value to be 6.5-7, adding potassium permanganate, continuing to react for 3-4 hours at 90-100 ℃, carrying out vacuum filtration to obtain a precipitate, and washing to be neutral to obtain an organic molybdenum amine mixture; wherein the weight ratio of molybdenum oxide, o-aminobenzenesulfonic acid, alkylated diphenylamine and potassium permanganate is 1: 3-5: 3-5: 7-10;
2) synthesizing the molybdenum-titanium alloy lubricating oil additive:
mixing the organic molybdenum amine mixture prepared in the step 1) with calcium titanate and methyl methacrylate, uniformly stirring, and reacting for 4-5 hours at 90-100 ℃ and under the pressure of 0.24-0.3 MPa; cooling to 50-60 ℃, adding didodecyl methyl tertiary amine, increasing the temperature to 180-190 ℃, continuously reacting for 3-4 hours under the condition of unchanged pressure, then cooling to 85-100 ℃, vacuumizing to 0.075-0.094 MPa, and filtering to obtain a yellow oil-soluble molybdenum-titanium alloy lubricating oil additive; wherein the weight ratio of the organic molybdenum amine mixture, the calcium titanate, the methyl methacrylate to the didodecyl methyl tertiary amine is 1: 5-8: 15-20: 15 to 20.
2. The method for synthesizing the semi-solid high-strength membrane vehicle lubricating oil additive according to claim 1, wherein the weight ratio of molybdenum oxide, o-aminobenzenesulfonic acid, alkylated diphenylamine and potassium permanganate in the step 1) is 1: 4: 4: 8.
3. the method for synthesizing the semi-solid high-strength membrane vehicle lubricating oil additive according to claim 2, wherein the weight ratio of the organic molybdenum amine mixture, the calcium titanate, the methyl methacrylate and the didodecyl methyl tertiary amine in the step 2) is 1: 6: 16: 16.
4. a semi-solid high-strength membrane vehicle lubricating oil additive is characterized by being prepared by the synthesis method of any one of claims 1 to 3.
5. A lubricating oil characterized by containing the semi-solid high-strength membrane of claim 4 as an additive for lubricating oils for vehicles.
6. The lubricating oil according to claim 5, wherein the mass percentage of the vehicle lubricating oil additive is 0.8-1%.
CN202110158326.7A 2021-02-05 2021-02-05 Vehicle lubricating oil additive with semi-solid high-strength membrane, synthetic method of vehicle lubricating oil additive and lubricating oil Pending CN112920875A (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20080139421A1 (en) * 2006-12-06 2008-06-12 Loper John T Lubricating Composition
CN102417848A (en) * 2010-09-27 2012-04-18 中国石油天然气股份有限公司 Energy-efficient vehicle gear lubricating oil composition
CN107142135A (en) * 2017-07-07 2017-09-08 郑州市久润润滑油有限责任公司 A kind of titanium maxter alloy lube oil additive and preparation method thereof
CN108791142A (en) * 2018-06-11 2018-11-13 徐州光森电器工具有限公司 Electric vehicle lubricates control assembly

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20080139421A1 (en) * 2006-12-06 2008-06-12 Loper John T Lubricating Composition
CN102417848A (en) * 2010-09-27 2012-04-18 中国石油天然气股份有限公司 Energy-efficient vehicle gear lubricating oil composition
CN107142135A (en) * 2017-07-07 2017-09-08 郑州市久润润滑油有限责任公司 A kind of titanium maxter alloy lube oil additive and preparation method thereof
CN108791142A (en) * 2018-06-11 2018-11-13 徐州光森电器工具有限公司 Electric vehicle lubricates control assembly

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