CN112080331A - Organic nitrogen zirconium fullerene lubricant and preparation method thereof - Google Patents
Organic nitrogen zirconium fullerene lubricant and preparation method thereof Download PDFInfo
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- 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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- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M163/00—Lubricating compositions characterised by the additive being a mixture of a compound of unknown or incompletely defined constitution and a non-macromolecular compound, each of these compounds being essential
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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
- C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
- C10M2201/04—Elements
- C10M2201/041—Carbon; Graphite; Carbon black
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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
- 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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- C—CHEMISTRY; METALLURGY
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- 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
- C10M2201/14—Inorganic compounds or elements as ingredients in lubricant compositions inorganic compounds surface treated with organic compounds
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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
- C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
- C10M2207/10—Carboxylix acids; Neutral salts thereof
- C10M2207/12—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms
- C10M2207/125—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids
- C10M2207/126—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids monocarboxylic
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- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2215/00—Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
- C10M2215/02—Amines, e.g. polyalkylene polyamines; Quaternary amines
- C10M2215/04—Amines, e.g. polyalkylene polyamines; Quaternary amines having amino groups bound to acyclic or cycloaliphatic carbon atoms
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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
- C10M2227/06—Organic compounds derived from inorganic acids or metal salts
- C10M2227/066—Organic compounds derived from inorganic acids or metal salts derived from Mo or W
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Abstract
The invention discloses an organic nitrogen zirconium fullerene lubricant and a preparation method thereof, wherein the organic nitrogen zirconium fullerene lubricant is prepared by polar modified zirconia fullerene C60, tertiary carbon primary amine and nitrogen molybdenum complex; wherein the weight ratio of the polar modified zirconia fullerene C60 to the tertiary carbon primary amine to the nitrogen-molybdenum complex is as follows: 1: 2-3: 20 to 25. The polar modified zirconia fullerene C60 is prepared by reacting fullerene C60, lightly burned zirconia, concentrated sulfuric acid, hydrofluoric acid and lauric acid. The additive is a friction improver, an antiwear agent and an antioxidant of lubricating oil, in particular lubricating oil for internal combustion engines, has obvious antifriction and oil saving effects, and has the advantages of energy saving and environmental protection due to low sulfur and low phosphorus.
Description
Technical Field
The invention relates to a lubricant, in particular to an oil-soluble organic nitrogen zirconium fullerene lubricant and a preparation method thereof.
Background
The research on zirconia powder originated in the 20 th century, and was originally used for melting refractory materials for glass and steel smelting, and since then, it had not been much developed in four or fifty years, until 1968, the japanese panasonic electric appliances invented zirconia nonlinear resistance elements through the research on zirconia powder, and so far, zirconia powder was regarded by the scientific research and was on the stage of history.
By 1973, americans r. zechnall made electrolytic oxidation sensors from zirconia powder, which clearly showed the specific gravity of air and fuel inside automobile engines, and by 1980, zirconia powder was applied to the steel industry.
In 1982, energy-saving diesel engine cylinder liners were developed jointly by insulator japan and cummins engines usa, and have attracted attention all over the world. If zirconia is used in lubricating oil, engine wear can be greatly reduced, but zirconia cannot be dissolved in lubricating oil and is limited in use in lubricating oil.
Due to its unique structural characteristics, fullerene C60 has become a hot point for research in many subjects such as physics, chemistry, materials science, life science and related application fields in recent years. It is a quasi-spherical particle composed of concentric closed shells, the interlayer spacing of which is 0.349nm and is close to the interlayer spacing of 0.336nm of graphite, and the particles are all lubricants with excellent performance.
If the fullerene is applied to the lubricating oil, the anti-wear and anti-friction characteristics of the lubricating oil can be greatly improved, and the engine can be effectively protected.
The nitrogen-molybdenum complex is the highest antiwear friction reducer applied in lubricating oil. The anti-friction material has excellent anti-friction performance and excellent high-temperature oxidation resistance, and also has good oil solubility and dispersibility; the zirconium oxide and the fullerene are matched in the lubricating oil, so that the functions of wear resistance, friction reduction and oxidation resistance of the lubricating oil are greatly improved, the oil change period can be effectively prolonged, and an engine is effectively and durably protected.
Disclosure of Invention
The invention aims to solve the technical problem of providing an organic nitrogen-zirconium fullerene lubricant which has simple production method, low cost, good oil solubility and high yield and a preparation method thereof.
In order to solve the technical problems, the invention adopts the technical scheme that: a preparation method of an organic nitrogen zirconium fullerene lubricant comprises the following steps:
(1) synthesis of polar modified zirconia fullerene
Putting fullerene C60, zirconium dioxide, concentrated sulfuric acid and hydrofluoric acid into a container, reacting for 2-3 hours at 90-100 ℃ under vacuum, then washing with water and amine, adjusting the pH value to 7, adding lauric acid, continuing to react for 3-4 hours at 200-220 ℃, then filtering in vacuum to obtain a precipitate, washing with alcohol and water to neutrality to obtain brown paste which is polar modified zirconia fullerene; according to weight ratio, fullerene C60: zirconium dioxide: concentrated sulfuric acid: hydrofluoric acid: lauric acid 1: 0.3-0.5: 5-7: 5-7: 20-25;
(2) synthesis of organic nitrogen zirconium fullerene lubricant
Mixing the prepared polar modified zirconia fullerene with tertiary carbon primary amine, uniformly stirring, and reacting for 4-5 hours at the temperature of 100-120 ℃ and under the pressure of 0.1 MPa; cooling to 40-50 ℃, adding a nitrogen-molybdenum complex, increasing the temperature to 200-210 ℃, continuously reacting for 3-4 hours under the condition of unchanged pressure, then cooling to 100 ℃, and vacuumizing to 0.1 MPa; finally, filtering to obtain a yellow organic nitrogen zirconium fullerene lubricant; wherein, according to the weight ratio, the polarity modified zirconia fullerene: tertiary primary amine: nitrogen molybdenum complex ═ 1: 2-3: 20-25, and the nitrogen-molybdenum complex is prepared from CN 201610522146.1.
The concentrated sulfuric acid is 98% in mass percentage concentration, and the hydrofluoric acid is 40% in mass percentage concentration.
The vacuum condition in the polar modified zirconia fullerene synthesis step is 0.095-0.098 MPa.
The zirconium dioxide is lightly-fired zirconium dioxide.
Preferably, the ratio by weight of fullerene C60: zirconium dioxide: concentrated sulfuric acid: hydrofluoric acid: lauric acid 1: 0.4: 5: 5: 22; polar modified zirconia fullerene: tertiary primary amine: nitrogen molybdenum complex ═ 1: 2: 20.
the organic nitrogen zirconium fullerene lubricant prepared by the preparation method.
The invention has the beneficial effects that: the organic nitrogen zirconium fullerene lubricant is a friction improver, an antiwear agent and an antioxidant of lubricating oil, in particular lubricating oil for internal combustion engines, has obvious effects of reducing friction and saving oil, and has the advantages of energy conservation and environmental protection due to low sulfur and low phosphorus.
Detailed Description
The preparation method of the organic nitrogen zirconium fullerene lubricant comprises the following steps:
(1) synthesis of polar modified zirconia fullerene
Putting fullerene C60, zirconium dioxide, concentrated sulfuric acid and hydrofluoric acid into a container, reacting for 2-3 hours at 90-100 ℃ under vacuum, then washing with water and amine, adjusting the pH value to 7, adding lauric acid, continuing to react for 3-4 hours at 200-220 ℃, then filtering in vacuum to obtain a precipitate, washing with alcohol and water to neutrality to obtain brown paste which is polar modified zirconia fullerene; according to weight ratio, fullerene C60: zirconium dioxide: concentrated sulfuric acid: hydrofluoric acid: lauric acid 1: 0.3-0.5: 5-7: 5-7: 20-25;
(2) synthesis of organic nitrogen zirconium fullerene lubricant
Mixing the prepared polar modified zirconia fullerene with tertiary carbon primary amine, uniformly stirring, and reacting for 4-5 hours at the temperature of 100-120 ℃ and under the pressure of 0.1 MPa; cooling to 40-50 ℃, adding a nitrogen-molybdenum complex, increasing the temperature to 200-210 ℃, continuously reacting for 3-4 hours under the condition of unchanged pressure, then cooling to 100 ℃, and vacuumizing to 0.1 MPa; finally, filtering to obtain a yellow organic nitrogen zirconium fullerene lubricant; wherein, according to the weight ratio, the polarity modified zirconia fullerene: tertiary primary amine: nitrogen molybdenum complex ═ 1: 2-3: 20-25, and the nitrogen-molybdenum complex is prepared from CN 201610522146.1.
The concentrated sulfuric acid is 98% in mass percentage concentration, and the hydrofluoric acid is 40% in mass percentage concentration.
The vacuum condition in the polar modified zirconia fullerene synthesis step is 0.095-0.098 MPa.
The zirconium dioxide is lightly-fired zirconium dioxide.
Preferably, the ratio by weight of fullerene C60: zirconium dioxide: concentrated sulfuric acid: hydrofluoric acid: lauric acid 1: 0.4: 5: 5: 22; polar modified zirconia fullerene: tertiary primary amine: nitrogen molybdenum complex ═ 1: 2: 20.
the organic nitrogen zirconium fullerene lubricant prepared by the preparation method.
According to the invention, firstly, fullerene is used as a base to react with slightly-burned zirconium dioxide, concentrated sulfuric acid and hydrofluoric acid, then lauric acid is added, a method of adjusting the pH value is adopted to obtain the polar modified zirconium oxide fullerene which is beneficial to the next good reaction, then the polar modified zirconium oxide fullerene reacts with tertiary carbon primary amine and a nitrogen-molybdenum complex, and a two-step partial pressure reduction method is adopted, so that the organic nitrogen-zirconium fullerene lubricant with good lubricating property and excellent wear resistance is prepared.
The organic nitrogen-zirconium fullerene lubricant provided by the invention has the advantages of energy saving, low sulfur, low phosphorus, no chlorine, environmental protection and high efficiency.
The invention relates to a principle that slightly burned zirconium dioxide can be dissolved in inorganic acid:
ZrO2+4H+＝Zr4++2H2O
the polar zirconia fullerene modified by concentrated sulfuric acid is modified and then effectively matched with a nitrogen-molybdenum complex with high dispersibility and high oil solubility; the surface energy of the modified zirconia fullerene is greatly reduced, a monomolecular adsorption layer is formed, a hydrophilic group faces the surface of the fullerene, and a lipophilic oil group faces outwards, so that on one hand, fullerene particles have lipophilicity and are compatible and combined with an oil-soluble nitrogen-molybdenum complex, the zirconia fullerene is adsorbed on the surface of the nitrogen-molybdenum complex, and can be completely dissolved in lubricating oil to prevent the collision agglomeration and gravity precipitation of the zirconia-modified fullerene, and the dispersibility and stability of the zirconia-modified fullerene lubricant in the lubricating oil are improved.
The zirconia-modified fullerene lubricant is dissolved in various lubricating oil in a liquid state, and the minimum friction coefficient can be reduced to 0.0117; the film forming and bearing capacity of the lubricating oil can be obviously improved. The lubrication mechanism is effective to merge sliding friction and rolling friction. Under the normal working condition of the lubricating part, a physical and chemical adsorption film with the functions of friction reduction and wear resistance is formed on the friction surface, and the adsorption film is sliding friction; under the harsh working conditions of high speed, high temperature, high pressure and the like, the fullerene factor on the surface of the friction pair changes the sliding friction into rolling friction, and the engine is protected by a layer closer. The effective combination of sliding friction and rolling friction is a leading precedent in our country and even in other countries in the world.
The organic nitrogen zirconium fullerene lubricant organically synthesizes fullerene and a nitrogen molybdenum complex together, is an ionic liquid compound, has good oil solubility and can never precipitate. The lubricant is a rare environment-friendly lubricant with no sulfur, phosphorus and chlorine, small dosage and high performance.
At present, the fullerene lubricating oil additive at home and even abroad is in a solid nano type, and is dispersed in lubricating oil by a dispersant and can be precipitated after a long time. Experimental data show that when the 1% organic nitrogen-zirconium fullerene lubricant is added into engine oil, the friction coefficient can be reduced to be below 0.0187 (the friction coefficient of the conventional engine oil is above 0.08), and the diameter of the wear scar is only 0.28mm (the wear scar diameter of the conventional engine oil is about 0.50) in a four-ball machine 40 kilogram force 60-minute long friction experiment. Therefore, the following effects can be achieved by using the organonitrogen zirconium fullerene lubricant
1. Reduction of the coefficient of friction: can be reduced by more than 80 percent.
2. Fuel oil saving: the oil can be saved by more than 10%.
3. And (3) prolonging the oil change period: the lubricating oil can be replaced by extending to 8000 km or more.
In the following examples, the concentrated sulfuric acid is 98% by mass, and the hydrofluoric acid is 40% by mass. Zirconium dioxide may also be used as a lightly calcined zirconium dioxide. The nitrogen molybdenum complex is prepared from CN 201610522146.1.
Example 1
1. Synthesis of polar modified zirconia fullerene
Putting fullerene, zirconia, concentrated sulfuric acid and hydrofluoric acid into a container, reacting for 2 hours under the condition of vacuum (pressure of 0.095MPa) at 100 ℃, then washing with water and amine, adjusting the pH value to 7, adding lauric acid, continuing to react for 3 hours at the temperature of 200 ℃, then filtering in vacuum to obtain a pasty mixture, washing with alcohol and washing with ultrasonic water to neutrality to obtain brown pasty material which is polar modified zirconia fullerene;
fullerene C60: zirconium dioxide: concentrated sulfuric acid: hydrofluoric acid: lauric acid 1: 0.4: 5: 5: 22 (weight ratio).
2. Synthesis of organic nitrogen zirconium fullerene lubricant
5 g of the prepared polar modified zirconia fullerene is mixed with 10 g of tertiary carbon primary amine, and the mixture is uniformly stirred and reacts for 4 hours at the temperature of 100 ℃ and the pressure of 0.1 MPa; cooling to 40 ℃, adding 100 g of nitrogen-molybdenum complex, increasing the temperature to 200 ℃, continuing to react for 3 hours under the condition of constant pressure, then cooling to 100 ℃, and vacuumizing to 0.1 MPa; and finally, filtering to obtain the yellow organic nitrogen zirconium fullerene lubricant.
And (3) investigating the antifriction and wear resistance and the bearing capacity of the product: the four-ball machine is used for measuring, the extreme pressure and antifriction antiwear performance under the set load (the temperature is 20 ℃, the load is 392N, the speed is 1450R/min, and the time is 30min) 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 antiwear performance. By contrast, lubricating oil was directly used, and the diameter of the wear scar reached 0.8 mm. 1 percent (weight) of the product prepared in the embodiment is added into API SN5W/40 lubricating oil, the diameter of the abrasive wear scar reaches 0.28mm, and the friction coefficient is 0.0117.
Example 2
1. Synthesis of polar modified zirconia fullerene
Putting fullerene, zirconia, concentrated sulfuric acid and hydrofluoric acid into a container, reacting for 3 hours at 90 ℃ under vacuum (pressure of 0.098MPa), then washing with water and amine, adjusting pH to 7, adding lauric acid, continuing to react for 4 hours at 220 ℃, then filtering in vacuum to obtain a pasty mixture, washing with alcohol and water to neutrality, and obtaining brown paste which is polar modified zirconia fullerene;
fullerene C60: zirconium dioxide: concentrated sulfuric acid: hydrofluoric acid: lauric acid 1: 0.5: 7: 7: 25 (weight ratio).
2. Synthesis of organic nitrogen zirconium fullerene lubricant
Mixing 10 g of the prepared polar modified zirconia fullerene with 15 g of tertiary carbon primary amine, uniformly stirring, and reacting for 5 hours at the temperature of 120 ℃ and under the pressure of 0.1 MPa; cooling to 50 ℃, adding 250 g of nitrogen-molybdenum complex, increasing the temperature to 210 ℃, continuing to react for 4 hours under the condition of constant pressure, then cooling to 100 ℃, and vacuumizing to 0.1 MPa; and finally, filtering to obtain the yellow organic nitrogen zirconium fullerene lubricant.
And (3) investigating the antifriction and wear resistance and the bearing capacity of the product: the four-ball machine is used for measuring, the extreme pressure and antifriction antiwear performance under the set load (the temperature is 20 ℃, the load is 392N, the speed is 1450R/min, and the time is 30min) 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 antiwear performance. By contrast, lubricating oil was directly used, and the diameter of the wear scar reached 0.8 mm. 1 percent (weight) of the product prepared in the example is added into API SN5W/40 lubricating oil, the diameter of the wear scar reaches 0.29mm, and the friction coefficient is 0.0109.
Example 3
1. Synthesis of polar modified zirconia fullerene
Putting fullerene, zirconia, concentrated sulfuric acid and hydrofluoric acid into a container, reacting for 2.5 hours at 95 ℃ under vacuum (pressure of 0.095MPa), then washing with water and amine, adjusting pH to 7, adding lauric acid, continuing to react for 3.5 hours at 210 ℃, then filtering in vacuum to obtain a pasty mixture, washing with alcohol and water to neutrality, and obtaining brown paste which is polar modified zirconia fullerene;
fullerene C60: zirconium dioxide: concentrated sulfuric acid: hydrofluoric acid: lauric acid 1: 0.3: 6: 6: 21 (weight ratio).
2. Synthesis of organic nitrogen zirconium fullerene lubricant
8 g of the prepared polar modified zirconia fullerene is mixed with 20 g of tertiary carbon primary amine, and the mixture is uniformly stirred and reacts for 4.5 hours at the temperature of 110 ℃ and the pressure of 0.1 MPa; cooling to 40 ℃, adding 176 g of nitrogen-molybdenum complex, increasing the temperature to 208 ℃, continuing to react for 3.5 hours under the condition of constant pressure, then cooling to 100 ℃, and vacuumizing to 0.1 MPa; and finally, filtering to obtain the yellow organic nitrogen zirconium fullerene lubricant.
And (3) investigating the antifriction and wear resistance and the bearing capacity of the product: the four-ball machine is used for measuring, the extreme pressure and antifriction antiwear performance under the set load (the temperature is 20 ℃, the load is 392N, the speed is 1450R/min, and the time is 30min) 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 antiwear performance. By contrast, lubricating oil was directly used, and the diameter of the wear scar reached 0.8 mm. 1 percent (weight) of the product prepared in the example is added into API SN5W/40 lubricating oil, the diameter of the grinding spot reaches 0.27mm, and the friction coefficient is 0.0119.
Example 4
1. Synthesis of polar modified zirconia fullerene
Putting fullerene, zirconia, concentrated sulfuric acid and hydrofluoric acid into a container, reacting for 2.5 hours at 98 ℃ under vacuum (pressure of 0.097MPa), then washing with water and amine, adjusting pH to 7, adding lauric acid, continuing to react for 4 hours at 205 ℃, then filtering in vacuum to obtain a pasty mixture, washing with alcohol and water to neutrality, and obtaining brown paste which is polar modified zirconia fullerene;
fullerene C60: zirconium dioxide: concentrated sulfuric acid: hydrofluoric acid: lauric acid 1: 0.55: 5.5: 5.5: 24 (weight ratio).
2. Synthesis of organic nitrogen zirconium fullerene lubricant
Mixing 20 g of the prepared polar modified zirconia fullerene with 49 g of tertiary carbon primary amine, uniformly stirring, and reacting for 5 hours at the temperature of 120 ℃ and under the pressure of 0.1 MPa; cooling to 50 ℃, adding 450 g of nitrogen-molybdenum complex, increasing the temperature to 205 ℃, continuing to react for 3 hours under the condition of constant pressure, then cooling to 100 ℃, and vacuumizing to 0.1 MPa; and finally, filtering to obtain the yellow organic nitrogen zirconium fullerene lubricant.
And (3) investigating the antifriction and wear resistance and the bearing capacity of the product: the four-ball machine is used for measuring, the extreme pressure and antifriction antiwear performance under the set load (the temperature is 20 ℃, the load is 392N, the speed is 1450R/min, and the time is 30min) 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 antiwear performance. By contrast, lubricating oil was directly used, and the diameter of the wear scar reached 0.8 mm. 1 wt% of the product prepared in this example was added to API SN5W/40 lubricating oil, and the resulting lubricating oil had a wear scar diameter of 0.30mm and a coefficient of friction of 0.0143.
The above embodiments are merely illustrative of the technical ideas and features of the present invention, and the purpose thereof is to enable those skilled in the art to understand the contents of the present invention and implement the present invention, and not to limit the protection scope of the present invention. All equivalent changes and modifications made according to the spirit of the present invention should be covered within the protection scope of the present invention.
Claims (6)
1. The preparation method of the organic nitrogen zirconium fullerene lubricant is characterized by comprising the following steps:
(1) synthesis of polar modified zirconia fullerene
Putting fullerene C60, zirconium dioxide, concentrated sulfuric acid and hydrofluoric acid into a container, reacting for 2-3 hours at 90-100 ℃ under vacuum, then washing with water and amine, adjusting the pH value to 7, adding lauric acid, continuing to react for 3-4 hours at 200-220 ℃, then filtering in vacuum to obtain a precipitate, washing with alcohol and water to neutrality to obtain brown paste which is polar modified zirconia fullerene; according to weight ratio, fullerene C60: zirconium dioxide: concentrated sulfuric acid: hydrofluoric acid: lauric acid 1: 0.3-0.5: 5-7: 5-7: 20-25;
(2) synthesis of organic nitrogen zirconium fullerene lubricant
Mixing the prepared polar modified zirconia fullerene with tertiary carbon primary amine, uniformly stirring, and reacting for 4-5 hours at the temperature of 100-120 ℃ and under the pressure of 0.1 MPa; cooling to 40-50 ℃, adding a nitrogen-molybdenum complex, increasing the temperature to 200-210 ℃, continuously reacting for 3-4 hours under the condition of unchanged pressure, then cooling to 100 ℃, and vacuumizing to 0.1 MPa; finally, filtering to obtain a yellow organic nitrogen zirconium fullerene lubricant; wherein, according to the weight ratio, the polarity modified zirconia fullerene: tertiary primary amine: nitrogen molybdenum complex ═ 1: 2-3: 20-25, and the nitrogen-molybdenum complex is prepared from CN 201610522146.1.
2. The method of preparing an organonitrogen zirconium fullerene lubricant according to claim 1, wherein the concentrated sulfuric acid is 98% by mass, and the hydrofluoric acid is 40% by mass.
3. The method for producing an organonitrogen zirconium fullerene lubricant according to claim 1, wherein the vacuum condition in the polar modified zirconia fullerene synthesis step is 0.095 to 0.098 MPa.
4. The method of preparing an organonitrogen zirconium fullerene lubricant according to claim 1, wherein the zirconium dioxide is a lightly fired zirconium dioxide.
5. The method of preparing an organonitrogen zirconium fullerene lubricant according to claim 1, wherein the ratio by weight of fullerene C60: zirconium dioxide: concentrated sulfuric acid: hydrofluoric acid: lauric acid 1: 0.4: 5: 5: 22; polar modified zirconia fullerene: tertiary primary amine: nitrogen molybdenum complex ═ 1: 2: 20.
6. an organonitrogen zirconium fullerene lubricant prepared by the preparation method as set forth in any one of claims 1 to 5.
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| CN113755226A (en) * | 2021-10-21 | 2021-12-07 | 华亿金卫(杭州)能源有限公司 | Oil-soluble organic zirconium friction reducer and preparation method thereof |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20040077507A1 (en) * | 2001-01-23 | 2004-04-22 | Arno Lange | Alkoxylated alkyl phenols and the use thereof in fuels and lubricants |
| CN1752020A (en) * | 2005-06-22 | 2006-03-29 | 浙江大学 | Preparation method of inorganic fullerene molybdenum disulfide and its application |
| CN105018186A (en) * | 2015-08-11 | 2015-11-04 | 王严绪 | Organic nitrogen molybdenum fullerene lubricant and preparing method thereof |
| CN105062618A (en) * | 2015-08-11 | 2015-11-18 | 王严绪 | Fullerene, boron and nitrogen containing lubricant and preparation method thereof |
| CN105695062A (en) * | 2016-03-16 | 2016-06-22 | 李培青 | Zirconia-modified fullerene lubricant and preparation method thereof |
| CN105838478A (en) * | 2016-03-23 | 2016-08-10 | 青岛星沃能源科技有限公司 | Graphene/onion-like fullerene complex solid lubricant and preparation method thereof |
| CN106190434A (en) * | 2016-07-04 | 2016-12-07 | 王严绪 | Nitrogen molybdenum complex lube oil additive and preparation method thereof |
-
2020
- 2020-09-24 CN CN202011014980.2A patent/CN112080331A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20040077507A1 (en) * | 2001-01-23 | 2004-04-22 | Arno Lange | Alkoxylated alkyl phenols and the use thereof in fuels and lubricants |
| CN1752020A (en) * | 2005-06-22 | 2006-03-29 | 浙江大学 | Preparation method of inorganic fullerene molybdenum disulfide and its application |
| CN105018186A (en) * | 2015-08-11 | 2015-11-04 | 王严绪 | Organic nitrogen molybdenum fullerene lubricant and preparing method thereof |
| CN105062618A (en) * | 2015-08-11 | 2015-11-18 | 王严绪 | Fullerene, boron and nitrogen containing lubricant and preparation method thereof |
| CN105695062A (en) * | 2016-03-16 | 2016-06-22 | 李培青 | Zirconia-modified fullerene lubricant and preparation method thereof |
| CN105838478A (en) * | 2016-03-23 | 2016-08-10 | 青岛星沃能源科技有限公司 | Graphene/onion-like fullerene complex solid lubricant and preparation method thereof |
| CN106190434A (en) * | 2016-07-04 | 2016-12-07 | 王严绪 | Nitrogen molybdenum complex lube oil additive and preparation method thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113755226A (en) * | 2021-10-21 | 2021-12-07 | 华亿金卫(杭州)能源有限公司 | Oil-soluble organic zirconium friction reducer and preparation method thereof |
| CN113755226B (en) * | 2021-10-21 | 2022-04-29 | 华亿金卫(杭州)能源有限公司 | Oil-soluble organic zirconium friction reducer and preparation method thereof |
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