CN109609243A - A kind of preparation method of multilayered structure type fullerene nano lubricating oil - Google Patents

A kind of preparation method of multilayered structure type fullerene nano lubricating oil Download PDF

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CN109609243A
CN109609243A CN201811494194.XA CN201811494194A CN109609243A CN 109609243 A CN109609243 A CN 109609243A CN 201811494194 A CN201811494194 A CN 201811494194A CN 109609243 A CN109609243 A CN 109609243A
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parts
lubricating oil
multilayered structure
structure type
fullerene
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张振芳
张文雯
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Beijing Fulexi Technology Co Ltd
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Beijing Fulexi Technology Co Ltd
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    • 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
    • C10M133/00Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing nitrogen
    • C10M133/02Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing nitrogen having a carbon chain of less than 30 atoms
    • C10M133/38Heterocyclic nitrogen compounds
    • C10M133/44Five-membered ring containing nitrogen and carbon only
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    • C10M155/00Lubricating compositions characterised by the additive being a macromolecular compound containing atoms of elements not provided for in groups C10M143/00 - C10M153/00
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    • C10M2201/00Inorganic compounds or elements as ingredients in lubricant compositions
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    • C10M2205/00Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions
    • C10M2205/02Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions containing acyclic monomers
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    • C10M2207/00Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/02Hydroxy compounds
    • C10M2207/023Hydroxy compounds having hydroxy groups bound to carbon atoms of six-membered aromatic rings
    • C10M2207/024Hydroxy compounds having hydroxy groups bound to carbon atoms of six-membered aromatic rings having at least two phenol groups but no condensed ring
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    • C10M2207/00Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/10Carboxylix acids; Neutral salts thereof
    • C10M2207/12Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms
    • C10M2207/121Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of seven or less carbon atoms
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    • C10M2207/10Carboxylix acids; Neutral salts thereof
    • C10M2207/12Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms
    • C10M2207/125Carboxylix 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
    • C10M2207/127Carboxylix 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 polycarboxylic
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    • C10M2207/00Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
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    • C10M2209/00Organic macromolecular compounds containing oxygen as ingredients in lubricant compositions
    • C10M2209/10Macromolecular compoundss obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • C10M2209/102Polyesters
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    • C10M2215/00Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
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    • C10M2215/102Ureas; Semicarbazides; Allophanates
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    • C10M2215/00Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
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    • C10M2219/00Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions
    • C10M2219/02Sulfur-containing compounds obtained by sulfurisation with sulfur or sulfur-containing compounds
    • C10M2219/024Sulfur-containing compounds obtained by sulfurisation with sulfur or sulfur-containing compounds of esters, e.g. fats
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    • C10M2219/00Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions
    • C10M2219/04Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions containing sulfur-to-oxygen bonds, i.e. sulfones, sulfoxides
    • C10M2219/044Sulfonic acids, Derivatives thereof, e.g. neutral salts
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    • C10M2223/00Organic non-macromolecular compounds containing phosphorus as ingredients in lubricant compositions
    • C10M2223/02Organic non-macromolecular compounds containing phosphorus as ingredients in lubricant compositions having no phosphorus-to-carbon bonds
    • C10M2223/04Phosphate esters
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    • C10M2223/00Organic non-macromolecular compounds containing phosphorus as ingredients in lubricant compositions
    • C10M2223/02Organic non-macromolecular compounds containing phosphorus as ingredients in lubricant compositions having no phosphorus-to-carbon bonds
    • C10M2223/049Phosphite
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    • C10N2030/00Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
    • C10N2030/06Oiliness; Film-strength; Anti-wear; Resistance to extreme pressure

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

Abstract

The invention belongs to technical field of lubricating oil, and in particular to a kind of preparation method of multilayered structure type fullerene nano lubricating oil;A kind of composition of multilayered structure type fullerene nano lubricating oil includes following substance: the lubricating oil of 100-120 part according to the mass fraction, 1-3 parts of multilayered structure type fullerene, 1-2 parts of auxiliary additive, 2-5 parts of foam reducing composition, 3-5 parts of matal deactivator, 3-6 parts of anticorrosive, 1-3 parts of antioxidant.Multilayered structure type fullerene nano lubricating oil prepared by the present invention is using the fullerene of the multiple structural type of addition as additive, because it is layer structure, molecule can slide in the case where stress, its lubricant effect for effectively raising lubricant, higher than simple nano material raising oil lubrication performance, the ability for promoting lubricating oil to carry is bigger;In addition, further improving the bearing capacity of lubricating oil by the way that other substances are added, improving its application range.

Description

A kind of preparation method of multilayered structure type fullerene nano lubricating oil
Technical field
The invention belongs to technical field of lubricating oil, and in particular to a kind of preparation of multilayered structure type fullerene nano lubricating oil Method.
Background technique
It with the development of nanometer material science technology, has further pushed nanometer in the application of lubrication technology, and has received Meter level material is studied as lube oil additive to the research topic for becoming a more heated door.Nowadays, it has been found that Nano metal particles, nano-oxide, nanometer sulfide, carbon nanotube, fullerene, diamond and nano magnetic particle etc. The greasy property of lubricating oil can be effectively promoted significantly to improve.
However, normal fullerene is a kind of hollow molecules being made of completely carbon atom, shape is in ball-type, ellipsoid The shapes such as type, column type or tubulose.And the fullerene of multilayered structure type is the derivative of fullerene, because being layer structure, point Son can slide in the case where stress, effectively raise the lubricant effect of lubricant, mention than simple nano material High oil lubrication performance is higher, and the ability for promoting lubricating oil to carry is bigger.
Summary of the invention
In order to achieve the purpose that in background technique, a kind of multilayered structure type fullerene nano lubricating oil proposed by the present invention Preparation method;
What the present invention realized by the following technical solutions:
A kind of a kind of preparation method of multilayered structure type fullerene nano lubricating oil, it is characterised in that: multilayer knot The composition of configuration fullerene nano lubricating oil includes following substance: the lubricating oil of 100-120 part according to the mass fraction, 1-3 parts Multilayered structure type fullerene, 1-2 parts of auxiliary additive, 2-5 parts of foam reducing composition, 3-5 parts of matal deactivator, 3-6 parts Anticorrosive, 1-3 parts of antioxidant.
Further, the multilayered structure type fullerene is, by temperature of reaction kettle control at 65 DEG C, revolving speed 200- 300rpm, be added into reaction kettle the water of 100-120 part of mass fraction meter, 20-30 parts of fullerene, 2-4 parts of sodium sulfonate, After 0.2-0.5 parts of ammonium persulfate is stirred 30 minutes, then by 4-6 parts of butyl acrylate, 3-5 parts of methyl methacrylate Ester, 1-2 parts 1,3- butadiene be added reaction kettle in, carry out reaction 6-8 hours after, temperature of reaction kettle is increased to 70 DEG C, so After carry out reaction 2-3 hour, then stop heating, after cooled to room temperature, obtained substance be spray-dried, is obtained Solid powder, the substance are exactly multilayered structure type fullerene.
Further, the lubricating oil is, by 75SN, 20-30 of 60SN, 30-50 part of 40-60 part of mass fraction meter The 150SN of 100SN, 10-15 part of part is added to the mixer the substance obtained after mixing, which is exactly to lubricate Oil.
Further, the foam reducing composition is, by the polyvinyl acetate of 6-8 part of mass fraction meter, 5-10 parts poly- Ester polyol, 3-5 parts of glycerol, 1-3 parts of octanol, 2-3 parts of polymerization silicone oil ester, 3-4 parts of poly- butyl ester are added thereto reaction In kettle, after carrying out reaction 1-2 hours, obtained substance is exactly foam reducing composition.
Further, the auxiliary additive is, by the PE wax of 3-5 part of mass fraction meter, 1-3 parts of two fourth of phosphorous acid Ester, 2-4 parts of diphenyl phosphate, 4-6 parts of wool grease, 10-12 parts of vulcanized vegetable oils add, 4-8 parts of nano zinc powder enters reaction In kettle, the product obtained after being stirred to react 30-50 minutes, which is exactly auxiliary additive.
Further, the matal deactivator is the N for being 6-10 parts by mass fraction, N- diakylaminomethylene benzene Bis- salicylidene butanediamine of triazole, 2-5 parts of N, N-, 3-5 parts of N, the addition of N- dimethyl benzene azoles, 4-6 parts of N, N- dimethyl Siloxanes is added to the mixer the substance obtained after mixing, should be exactly matal deactivator.
Further, the anticorrosive is, by the barium mahogany sulfonate, 4-6 parts of octene of 10-20 part of mass fraction meter The substance that base glutaric acid, 3-6 parts of dodecyl sodium sulfate, 4-8 parts of urea are obtained after mixing, the substance are exactly Anticorrosive.
Further, the antioxidant is, by the hydroquinone of 5-9 part of mass fraction meter, 4-6 parts to methylbenzene Phenol, 2-3 parts of sodium citrate, 4-8 parts of 2- butyl formate base -3- fourth agent phenol are added to the mixer progress and obtain after mixing The substance arrived, the substance are exactly antioxidant.
Further, the multilayered structure type fullerene nano lubricating oil the preparation method is as follows: by temperature of reaction kettle control 100-120 parts of lubricating oil, 1-3 parts of multilayered structure type fullerene, 1-2 is added under the conditions of 50-60 DEG C in system in a kettle Auxiliary additive, 2-5 parts of the foam reducing composition, 3-5 parts of matal deactivator, 3-6 parts of anticorrosive, 1-3 parts of antioxygen of part Agent is added in reaction kettle, and agitator speed is adjusted to 600-800rpm, is stirred to react after forty minutes, material is placed into It carries out ultrasonic disperse 1-2 hours in ultrasonic instrument, after dispersion completely, solution is taken out, which is exactly multilayered structure type fowler Alkene nano lubricating oil.
Beneficial to benefit
(1) multilayered structure type fullerene nano lubricating oil prepared by the present invention is made using the fullerene for adding multiple structural type For additive, because it is layer structure, molecule can slide in the case where stress, effectively raise lubricant Lubricant effect, higher than simple nano material raising oil lubrication performance, the ability for promoting lubricating oil to carry is bigger.
(2) present invention is by being added the objects such as auxiliary additive, foam reducing composition, matal deactivator, anticorrosive, antioxidant Matter further improves the bearing capacity of lubricating oil, improves its application range.
Specific embodiment
In order to keep the purpose of the present invention, technical scheme and beneficial effects clearer, below in conjunction with experimental data, to this The preferred embodiment of invention is described in detail, to facilitate the technical staff to understand.
Embodiment 1
A kind of a kind of preparation method of multilayered structure type fullerene nano lubricating oil, it is characterised in that: multilayer knot The composition of configuration fullerene nano lubricating oil includes following substance: 110 parts of lubricating oil according to the mass fraction, 3 parts of multilayer Structural type fullerene, 1 part of auxiliary additive, 2 parts of foam reducing composition, 4 parts of matal deactivator, 3 parts of anticorrosive, 2 parts Antioxidant.
Further, the multilayered structure type fullerene is to control temperature of reaction kettle at 65 DEG C, revolving speed 200rpm, 120 parts of water, 25 parts of fullerene, 4 parts of the sodium sulfonate, 0.2 part of ammonium persulfate of mass fraction meter are added into reaction kettle After being stirred 30 minutes, then by 4 parts of butyl acrylate, 4 parts of methyl methacrylate, the 1 of 1 part, 3- butadiene be added In reaction kettle, after carrying out reaction 6 hours, temperature of reaction kettle is increased to 70 DEG C, then carries out reaction 3 hours, then stops adding Heat after cooled to room temperature, obtained substance is spray-dried, solid powder is obtained, which is exactly multilayered structure Type fullerene.
Further, the lubricating oil is, by 40 parts of 60SN of mass fraction meter, 40 parts of 75SN, 20 parts 100SN, 12 parts of 150SN are added to the mixer the substance obtained after mixing, which is exactly lubricating oil.
Further, the foam reducing composition is, 7 parts of polyvinyl acetate of mass fraction meter, 10 parts of polyester is more First alcohol, 4 parts of glycerol, 3 parts of octanol, 2 parts of polymerization silicone oil ester, 4 parts of poly- butyl ester are added thereto in reaction kettle, are reacted After 1 hour, obtained substance is exactly foam reducing composition.
Further, the auxiliary additive is, by 4 parts of PE wax of mass fraction meter, 3 parts of dibutyl phosphite, 3 Part diphenyl phosphate, 4 parts of wool grease, 11 parts of vulcanized vegetable oils add, 8 parts of nano zinc powder enters in reaction kettle, be stirred The product obtained after forty minutes is reacted, which is exactly auxiliary additive.
Further, the matal deactivator is the N for being 10 parts by mass fraction, N- diakylaminomethylene benzene three Azoles, 3 parts of N, bis- salicylidene butanediamine of N-, 5 parts of N, the addition of N- dimethyl benzene azoles, 5 parts of N, N- dimethyl siloxane add Enter the substance obtained after mixing in mixing machine, should be exactly matal deactivator.
Further, the anticorrosive is, by 20 parts of barium mahogany sulfonate of mass fraction meter, 5 parts of octenyl penta The substance that diacid, 3 parts of dodecyl sodium sulfate, 6 parts of urea are obtained after mixing, the substance are exactly anticorrosion Agent.
Further, the antioxidant is, by 9 parts of hydroquinone of mass fraction meter, 5 parts of p-methyl phenol, 2 The sodium citrate, 6 parts of 2- butyl formate base -3- fourth agent phenol of part are added to the mixer the object obtained after mixing Matter, the substance are exactly antioxidant.
Further, the multilayered structure type fullerene nano lubricating oil the preparation method is as follows: by temperature of reaction kettle control 110 parts of lubricating oil, 3 parts of multilayered structure type fullerene, 1 part of auxiliary are added in a kettle and adds under the conditions of 60 DEG C for system Add agent, 2 parts of foam reducing composition, 4 parts of matal deactivator, 3 parts of anticorrosive, 2 parts of antioxidant to be added in reaction kettle, stirs Device rotational speed regulation is mixed to 800rpm, is stirred to react after forty minutes, material is placed into progress ultrasonic disperse 2 in ultrasonic instrument Hour, after dispersion completely, solution is taken out, which is exactly multilayered structure type fullerene nano lubricating oil.
Embodiment 2
A kind of a kind of preparation method of multilayered structure type fullerene nano lubricating oil, it is characterised in that: multilayer knot The composition of configuration fullerene nano lubricating oil includes following substance: 120 parts of lubricating oil according to the mass fraction, 2 parts of multilayer Structural type fullerene, 1 part of auxiliary additive, 4 parts of foam reducing composition, 5 parts of matal deactivator, 5 parts of anticorrosive, 3 parts It is anti-oxidant.
Further, the multilayered structure type fullerene is to control temperature of reaction kettle at 65 DEG C, revolving speed 300rpm, 110 parts of water, 30 parts of fullerene, 3 parts of the sodium sulfonate, 0.3 part of ammonium persulfate of mass fraction meter are added into reaction kettle After being stirred 30 minutes, then by 5 parts of butyl acrylate, 5 parts of methyl methacrylate, the 1 of 1 part, 3- butadiene be added In reaction kettle, after carrying out reaction 8 hours, temperature of reaction kettle is increased to 70 DEG C, then carries out reaction 2 hours, then stops adding Heat after cooled to room temperature, obtained substance is spray-dried, solid powder is obtained, which is exactly multilayered structure Type fullerene.
Further, the lubricating oil is, by 50 parts of 60SN of mass fraction meter, 30 parts of 75SN, 25 parts 100SN, 15 parts of 150SN are added to the mixer the substance obtained after mixing, which is exactly lubricating oil.
Further, the foam reducing composition is, 7 parts of polyvinyl acetate of mass fraction meter, 10 parts of polyester is more First alcohol, 4 parts of glycerol, 1 part of octanol, 2 parts of polymerization silicone oil ester, 4 parts of poly- butyl ester are added thereto in reaction kettle, are reacted After 2 hours, obtained substance is exactly foam reducing composition.
Further, the auxiliary additive is, by 4 parts of PE wax of mass fraction meter, 3 parts of dibutyl phosphite, 3 Part diphenyl phosphate, 6 parts of wool grease, 11 parts of vulcanized vegetable oils add, 8 parts of nano zinc powder enters in reaction kettle, be stirred The product obtained after forty minutes is reacted, which is exactly auxiliary additive.
Further, the matal deactivator is the N for being 8 parts by mass fraction, N- diakylaminomethylene benzene three Azoles, 5 parts of N, bis- salicylidene butanediamine of N-, 4 parts of N, the addition of N- dimethyl benzene azoles, 6 parts of N, N- dimethyl siloxane add Enter the substance obtained after mixing in mixing machine, should be exactly matal deactivator.
Further, the anticorrosive is, by 15 parts of barium mahogany sulfonate of mass fraction meter, 6 parts of octenyl penta The substance that diacid, 5 parts of dodecyl sodium sulfate, 4 parts of urea are obtained after mixing, the substance are exactly anticorrosion Agent.
Further, the antioxidant is, by 7 parts of hydroquinone of mass fraction meter, 6 parts of p-methyl phenol, 2 The sodium citrate, 4 parts of 2- butyl formate base -3- fourth agent phenol of part are added to the mixer the object obtained after mixing Matter, the substance are exactly antioxidant.
Further, the multilayered structure type fullerene nano lubricating oil the preparation method is as follows: by temperature of reaction kettle control 120 parts of lubricating oil, 2 parts of multilayered structure type fullerene, 1 part of auxiliary are added in a kettle and adds under the conditions of 55 DEG C for system Add agent, 4 parts of foam reducing composition, 5 parts of matal deactivator, 5 parts of anticorrosive, 3 parts of antioxidant to be added in reaction kettle, stirs Device rotational speed regulation is mixed to 600-800rpm, is stirred to react after forty minutes, material is placed into ultrasonic instrument and carries out ultrasound Dispersion 1-2 hours takes out solution, which is exactly multilayered structure type fullerene nano lubricating oil after dispersion completely.
Embodiment 3
A kind of a kind of preparation method of multilayered structure type fullerene nano lubricating oil, it is characterised in that: multilayer knot The composition of configuration fullerene nano lubricating oil includes following substance: 120 parts of lubricating oil according to the mass fraction, 3 parts of multilayer Structural type fullerene, 2 parts of auxiliary additive, 5 parts of foam reducing composition, 5 parts of matal deactivator, 6 parts of anticorrosive, 3 parts Antioxidant.
Further, the multilayered structure type fullerene is to control temperature of reaction kettle at 65 DEG C, revolving speed 300rpm, 120 parts of water, 30 parts of fullerene, 4 parts of the sodium sulfonate, 0.5 part of ammonium persulfate of mass fraction meter are added into reaction kettle After being stirred 30 minutes, then by 6 parts of butyl acrylate, 5 parts of methyl methacrylate, the 1 of 2 parts, 3- butadiene be added In reaction kettle, after carrying out reaction 8 hours, temperature of reaction kettle is increased to 70 DEG C, then carries out reaction 3 hours, then stops adding Heat after cooled to room temperature, obtained substance is spray-dried, solid powder is obtained, which is exactly multilayered structure Type fullerene.
Further, the lubricating oil is, by 60 parts of 60SN of mass fraction meter, 50 parts of 75SN, 30 parts 100SN, 15 parts of 150SN are added to the mixer the substance obtained after mixing, which is exactly lubricating oil.
Further, the foam reducing composition is, 8 parts of polyvinyl acetate of mass fraction meter, 10 parts of polyester is more First alcohol, 5 parts of glycerol, 3 parts of octanol, 3 parts of polymerization silicone oil ester, 4 parts of poly- butyl ester are added thereto in reaction kettle, are reacted After 2 hours, obtained substance is exactly foam reducing composition.
Further, the auxiliary additive is, by 5 parts of PE wax of mass fraction meter, 3 parts of dibutyl phosphite, 4 Part diphenyl phosphate, 6 parts of wool grease, 12 parts of vulcanized vegetable oils add, 8 parts of nano zinc powder enters in reaction kettle, be stirred The product that reaction obtains after 50 minutes, which is exactly auxiliary additive.
Further, the matal deactivator is the N for being 10 parts by mass fraction, N- diakylaminomethylene benzene three Azoles, 5 parts of N, bis- salicylidene butanediamine of N-, 5 parts of N, the addition of N- dimethyl benzene azoles, 6 parts of N, N- dimethyl siloxane add Enter the substance obtained after mixing in mixing machine, should be exactly matal deactivator.
Further, the anticorrosive is, by 20 parts of barium mahogany sulfonate of mass fraction meter, 6 parts of octenyl penta The substance that diacid, 6 parts of dodecyl sodium sulfate, 8 parts of urea are obtained after mixing, the substance are exactly anticorrosion Agent.
Further, the antioxidant is, by 9 parts of hydroquinone of mass fraction meter, 6 parts of p-methyl phenol, 3 The sodium citrate, 8 parts of 2- butyl formate base -3- fourth agent phenol of part are added to the mixer the object obtained after mixing Matter, the substance are exactly antioxidant.
Further, the multilayered structure type fullerene nano lubricating oil the preparation method is as follows: by temperature of reaction kettle control 120 parts of lubricating oil, 3 parts of multilayered structure type fullerene, 2 parts of auxiliary are added in a kettle and adds under the conditions of 60 DEG C for system Add agent, 5 parts of foam reducing composition, 5 parts of matal deactivator, 6 parts of anticorrosive, 3 parts of antioxidant to be added in reaction kettle, stirs Device rotational speed regulation is mixed to 800rpm, is stirred to react after forty minutes, material is placed into progress ultrasonic disperse 2 in ultrasonic instrument Hour, after dispersion completely, solution is taken out, which is exactly multilayered structure type fullerene nano lubricating oil.
Embodiment 4
A kind of a kind of preparation method of multilayered structure type fullerene nano lubricating oil, it is characterised in that: multilayer knot The composition of configuration fullerene nano lubricating oil includes following substance: 100 parts of lubricating oil according to the mass fraction, 1 part of multilayer Structural type fullerene, 1 part of auxiliary additive, 2 parts of foam reducing composition, 3 parts of matal deactivator, 3 parts of anticorrosive, 1 part Antioxidant.
Further, the multilayered structure type fullerene is to control temperature of reaction kettle at 65 DEG C, revolving speed 200rpm, 100 parts of water, 20 parts of fullerene, 2 parts of the sodium sulfonate, 0.2 part of ammonium persulfate of mass fraction meter are added into reaction kettle After being stirred 30 minutes, then by 4 parts of butyl acrylate, 3 parts of methyl methacrylate, the 1 of 1 part, 3- butadiene be added In reaction kettle, after carrying out reaction 8 hours, temperature of reaction kettle is increased to 70 DEG C, then carries out reaction 2 hours, then stops adding Heat after cooled to room temperature, obtained substance is spray-dried, solid powder is obtained, which is exactly multilayered structure Type fullerene.
Further, the lubricating oil is, by 40 parts of 60SN of mass fraction meter, 30 parts 75SN, 20-30 part 100SN, 10 parts of 150SN are added to the mixer the substance obtained after mixing, which is exactly lubricating oil.
Further, the foam reducing composition is, by 6 parts of polyvinyl acetate of mass fraction meter, 5 parts of polyester polyols Alcohol, 3 parts of glycerol, 1 part of octanol, 2 parts of polymerization silicone oil ester, 3 parts of poly- butyl ester are added thereto in reaction kettle, carry out reaction 1 After hour, obtained substance is exactly foam reducing composition.
Further, the auxiliary additive is, by the PE wax of 3-5 part of mass fraction meter, 1 part of two fourth of phosphorous acid Ester, 2 parts of diphenyl phosphate, 4 parts of wool grease, 10 parts of vulcanized vegetable oils add, 4 parts of nano zinc powder enters in reaction kettle, carry out The product obtained after being stirred to react 30 minutes, the substance are exactly auxiliary additive.
Further, the matal deactivator is the N for being 6 parts by mass fraction, N- diakylaminomethylene benzene three Azoles, 2 parts of N, bis- salicylidene butanediamine of N-, 3 parts of N, the addition of N- dimethyl benzene azoles, 4 parts of N, N- dimethyl siloxane add Enter the substance obtained after mixing in mixing machine, should be exactly matal deactivator.
Further, the anticorrosive is, by 10 parts of barium mahogany sulfonate of mass fraction meter, 4 parts of octenyl penta The substance that diacid, 3 parts of dodecyl sodium sulfate, 4 parts of urea are obtained after mixing, the substance are exactly anticorrosion Agent.
Further, the antioxidant is, by 5 parts of hydroquinone of mass fraction meter, 4 parts of p-methyl phenol, 2 The sodium citrate, 4 parts of 2- butyl formate base -3- fourth agent phenol of part are added to the mixer the object obtained after mixing Matter, the substance are exactly antioxidant.
Further, the multilayered structure type fullerene nano lubricating oil the preparation method is as follows: by temperature of reaction kettle control 100 parts of lubricating oil, 1 part of multilayered structure type fullerene, 1 part of auxiliary are added in a kettle and adds under the conditions of 50 DEG C for system Add agent, 2 parts of foam reducing composition, 3 parts of matal deactivator, 3 parts of anticorrosive, 1 part of antioxidant to be added in reaction kettle, stirs Device rotational speed regulation is mixed to 600rpm, is stirred to react after forty minutes, material is placed into progress ultrasonic disperse 1 in ultrasonic instrument Hour, after dispersion completely, solution is taken out, which is exactly multilayered structure type fullerene nano lubricating oil.
Embodiment 5
A kind of a kind of preparation method of multilayered structure type fullerene nano lubricating oil, it is characterised in that: multilayer knot The composition of configuration fullerene nano lubricating oil includes following substance: 100 parts of lubricating oil according to the mass fraction, 1 part of multilayer Structural type fullerene, 1 part of auxiliary additive, 2 parts of foam reducing composition, 3 parts of matal deactivator, 3 parts of anticorrosive, 1 part Antioxidant.
Further, the structural formula of the multilayered structure type fullerene are as follows:
Middle R1For phenyl, R2For hydrogen preparation process are as follows:
Fullerene, amine oxime compound, 4-dimethylaminopyridine are dissolved in o-dibromobenzene by the molar ratio of 1:1:5, in 180 It DEG C is stirred to react 5 hours, is cooled and separated after purification, obtains target product.
Further, the lubricating oil is, by 40 parts of 60SN of mass fraction meter, 30 parts 75SN, 20-30 part 100SN, 10 parts of 150SN are added to the mixer the substance obtained after mixing, which is exactly lubricating oil.
Further, the foam reducing composition is, by 6 parts of polyvinyl acetate of mass fraction meter, 5 parts of polyester polyols Alcohol, 3 parts of glycerol, 1 part of octanol, 2 parts of polymerization silicone oil ester, 3 parts of poly- butyl ester are added thereto in reaction kettle, carry out reaction 1 After hour, obtained substance is exactly foam reducing composition.
Further, the auxiliary additive is, by the PE wax of 3-5 part of mass fraction meter, 1 part of two fourth of phosphorous acid Ester, 2 parts of diphenyl phosphate, 4 parts of wool grease, 10 parts of vulcanized vegetable oils add, 4 parts of nano zinc powder enters in reaction kettle, carry out The product obtained after being stirred to react 30 minutes, the substance are exactly auxiliary additive.
Further, the matal deactivator is the N for being 6 parts by mass fraction, N- diakylaminomethylene benzene three Azoles, 2 parts of N, bis- salicylidene butanediamine of N-, 3 parts of N, the addition of N- dimethyl benzene azoles, 4 parts of N, N- dimethyl siloxane add Enter the substance obtained after mixing in mixing machine, should be exactly matal deactivator.
Further, the anticorrosive is, by 10 parts of barium mahogany sulfonate of mass fraction meter, 4 parts of octenyl penta The substance that diacid, 3 parts of dodecyl sodium sulfate, 4 parts of urea are obtained after mixing, the substance are exactly anticorrosion Agent.
Further, the antioxidant is, by 5 parts of hydroquinone of mass fraction meter, 4 parts of p-methyl phenol, 2 The sodium citrate, 4 parts of 2- butyl formate base -3- fourth agent phenol of part are added to the mixer the object obtained after mixing Matter, the substance are exactly antioxidant.
Further, the multilayered structure type fullerene nano lubricating oil the preparation method is as follows: by temperature of reaction kettle control 100 parts of lubricating oil, 1 part of multilayered structure type fullerene, 1 part of auxiliary are added in a kettle and adds under the conditions of 50 DEG C for system Add agent, 2 parts of foam reducing composition, 3 parts of matal deactivator, 3 parts of anticorrosive, 1 part of antioxidant to be added in reaction kettle, stirs Device rotational speed regulation is mixed to 600rpm, is stirred to react after forty minutes, material is placed into progress ultrasonic disperse 1 in ultrasonic instrument Hour, after dispersion completely, solution is taken out, which is exactly multilayered structure type fullerene nano lubricating oil.
Embodiment 6
A kind of a kind of preparation method of multilayered structure type fullerene nano lubricating oil, it is characterised in that: multilayer knot The composition of configuration fullerene nano lubricating oil includes following substance: 100 parts of lubricating oil according to the mass fraction, 1 part of multilayer Structural type fullerene, 1 part of auxiliary additive, 2 parts of foam reducing composition, 3 parts of matal deactivator, 3 parts of anticorrosive, 1 part Antioxidant.
Further, the multilayered structure type fullerene is,
(1) fullerene is dissolved in ethyl alcohol, vortex, ultrasonic mixing are uniform, and the concentration for obtaining fowler enolate solution is 5mg/ mL;(2) chitosan oligosaccharide is dissolved in acidic organic solvent, vortex, ultrasonic mixing are uniform, and the concentration for obtaining chitosan acid solution is 5mg/mL;The acidic organic solvent includes acetic acid, propionic acid or butyric acid;3) fowler enolate solution and chitosan oligosaccharide acid solution are pressed into body After mixing than 0.5:2, glutaraldehyde solution is added in product, and the final mass percent concentration of glutaraldehyde in the solution is 1.5%, It is reacted 4 hours in 120 DEG C, after being cooled to room temperature, successively uses organic solvent and water washing, obtain fullerene/chitosan oligosaccharide suspension; (4) phenyl boric acid is dissolved in organic solvent, is vortexed, is uniformly mixed, the fullerene/chitosan oligosaccharide suspension is added, at room temperature instead Answer 12 hours, successively the fullerene chitosan-modified to get hydrophilic phenyl boric acid functionalization with organic solvent and water washing;Institute Stating the concentration of phenyl boric acid in the solution is 100mg/mL;The organic solvent is methanol or ethyl alcohol.
Further, the lubricating oil is, by 40 parts of 60SN of mass fraction meter, 30 parts 75SN, 20-30 part 100SN, 10 parts of 150SN are added to the mixer the substance obtained after mixing, which is exactly lubricating oil.
Further, the foam reducing composition is, by 6 parts of polyvinyl acetate of mass fraction meter, 5 parts of polyester polyols Alcohol, 3 parts of glycerol, 1 part of octanol, 2 parts of polymerization silicone oil ester, 3 parts of poly- butyl ester are added thereto in reaction kettle, carry out reaction 1 After hour, obtained substance is exactly foam reducing composition.
Further, the matal deactivator is the N for being 6 parts by mass fraction, N- diakylaminomethylene benzene three Azoles, 2 parts of N, bis- salicylidene butanediamine of N-, 3 parts of N, the addition of N- dimethyl benzene azoles, 4 parts of N, N- dimethyl siloxane add Enter the substance obtained after mixing in mixing machine, should be exactly matal deactivator.
Further, the anticorrosive is made of fatty amine and fatty phenol, in terms of anticorrosive total volume percent, institute Stating fatty amine and fatty phenol content is 25%, and the fatty amine is N, and the sub- bigcatkin willow propane diamine of N '-two, fatty phenol is the tertiary fourth of 2,6- bis- Base paracresol, the two mix to obtain anti-corrosion of metal component with volume ratio 1:2 ratio;Cheating components: fatty amine salt 35% are passivated, it is described Fatty amine salt be to prepare to obtain with volume ratio 1:1 ratio by benzotriazole, benzotriazole fatty amine salt;Antioxygen inhibition component: Yeast fat acid 25-40%, the yeast fat acid are petroleum yeast fat acid C16-C18;The auxiliary additive, with body Product percentages, surface active composition, 70% dispersion peat component including 40%, the surface active composition is C4-C5 Quinoline and/or N-methylmorpholine;The surface active composition C4-C5 morpholine, N-methylmorpholine it is one such or two kinds with body Mixture of the product than equal proportion, the dispersion peat component: 10% yeast fat acid, 20% fatty amine calcium salt, the fat Amine calcium salt is the T154+T109 mother liquor that polyisobutylene-bis-succinimide, alkyl calcium salicylate are prepared with volume ratio 1:1 ratio.
Further, the antioxidant is, by 5 parts of hydroquinone of mass fraction meter, 4 parts of p-methyl phenol, 2 The sodium citrate, 4 parts of 2- butyl formate base -3- fourth agent phenol of part are added to the mixer the object obtained after mixing Matter, the substance are exactly antioxidant.
Further, the multilayered structure type fullerene nano lubricating oil the preparation method is as follows: by temperature of reaction kettle control 100 parts of lubricating oil, 1 part of multilayered structure type fullerene, 1 part of auxiliary are added in a kettle and adds under the conditions of 50 DEG C for system Add agent, 2 parts of foam reducing composition, 3 parts of matal deactivator, 3 parts of anticorrosive, 1 part of antioxidant to be added in reaction kettle, stirs Device rotational speed regulation is mixed to 600rpm, is stirred to react after forty minutes, material is placed into progress ultrasonic disperse 1 in ultrasonic instrument Hour, after dispersion completely, solution is taken out, which is exactly multilayered structure type fullerene nano lubricating oil.
Experimental analysis:
1, lubricating oil bearing capacity is tested
The same class lubricating oil that the embodiment 1-4 lubricating oil prepared and market are sold is carried out to test its bearing capacity, is surveyed Test result is as follows:
It can be seen that lubricating oil prepared by the present invention by above-mentioned test result, bearing capacity is higher, is common market 1.5 times or more of the same class lubricating oil sold, application range is more extensive.And the present embodiment 5-6, the multilayered structure of use Type fullerene, can more enhance bearing capacity, and bearing capacity is highest.
Finally, it is stated that preferred embodiment above is only used to illustrate the technical scheme of the present invention rather than limits, although logical It crosses above preferred embodiment the present invention is described in detail, however, those skilled in the art should understand that, can be Various changes are made to it in form and in details, without departing from defined by claims of the present invention.

Claims (10)

1. a kind of preparation method of multilayered structure type fullerene nano lubricating oil, it is characterised in that: a kind of multilayered structure The composition of type fullerene nano lubricating oil includes following substance: the lubricating oil of 100-120 part according to the mass fraction, 1-3 parts Multilayered structure type fullerene, 1-2 parts of auxiliary additive, 2-5 parts of foam reducing composition, 3-5 parts of matal deactivator, 3-6 parts Anticorrosive, 1-3 parts of antioxidant.
2. a kind of preparation method of multilayered structure type fullerene nano lubricating oil according to claim 1, it is characterised in that: The multilayered structure type fullerene is to control temperature of reaction kettle at 65 DEG C, revolving speed 200-300rpm, add into reaction kettle Enter the water, 20-30 parts of fullerene, 2-4 parts of sodium sulfonate, 0.2-0.5 parts of ammonium persulfate of 100-120 part of mass fraction meter After being stirred 30 minutes, then by 4-6 parts of butyl acrylate, 3-5 parts of methyl methacrylate, the 1 of 1-2 parts, 3- fourth two Alkene is added in reaction kettle, and after carrying out reaction 6-8 hours, temperature of reaction kettle is increased to 70 DEG C, then carries out reaction 2-3 hours, Then stop heating, after cooled to room temperature, obtained substance is spray-dried, solid powder is obtained, the substance is just It is multilayered structure type fullerene.
3. a kind of preparation method of multilayered structure type fullerene nano lubricating oil according to claim 1, it is characterised in that: The structural formula of the multilayered structure type fullerene are as follows:
Middle R1For phenyl, substituted-phenyl, naphthalene, furyl or C1-4 linear chain or branched chain Alkyl, the substituent group on the substituted-phenyl phenyl ring are fluorine, chlorine, bromine or methoxyl group, R2For hydrogen or C1-4 linear or branched alkyl group;System Standby technique are as follows:
By fullerene, amine oxime compound, 4-dimethylaminopyridine by 1:(0.5~1): the molar ratio of (3~5) is dissolved in adjacent dibromo Benzene is stirred to react 4~5 hours in 180 DEG C, is cooled and separated after purification, obtains target product.
4. a kind of preparation method of multilayered structure type fullerene nano lubricating oil according to claim 1, it is characterised in that: The multilayered structure type fullerene is,
(1) fullerene is dissolved in ethyl alcohol, vortex, ultrasonic mixing are uniform, and the concentration for obtaining fowler enolate solution is 5-50mg/ mL;(2) chitosan oligosaccharide is dissolved in acidic organic solvent, vortex, ultrasonic mixing are uniform, and the concentration for obtaining chitosan acid solution is 5- 100mg/mL;The acidic organic solvent includes acetic acid, propionic acid or butyric acid;3) fowler enolate solution and chitosan oligosaccharide acid solution are pressed After mixing, glutaraldehyde solution is added in volume ratio 0.5:1~2:2.5, and the final mass percentage of glutaraldehyde in the solution is dense Degree is 1.5%~3%, in 120-160 DEG C reaction 1-4 hours, after being cooled to room temperature, successively with organic solvent and water washing, obtain Fullerene/chitosan oligosaccharide suspension;(4) phenyl boric acid is dissolved in organic solvent, is vortexed, is uniformly mixed, the fullerene/shell is added Oligosaccharides suspension reacts 12-32 hours, at room temperature successively with organic solvent and water washing to get hydrophilic phenyl boric acid function Change chitosan-modified fullerene;The concentration of the phenyl boric acid in the solution is 1~100mg/mL;The organic solvent is methanol Or ethyl alcohol.
5. a kind of preparation method of multilayered structure type fullerene nano lubricating oil according to claim 1, it is characterised in that: The lubricating oil is, by 100SN, 10-15 of 75SN, 20-30 part of 60SN, 30-50 part of 40-60 part of mass fraction meter The 150SN of part is added to the mixer the substance obtained after mixing, which is exactly lubricating oil.
6. a kind of preparation method of multilayered structure type fullerene nano lubricating oil according to claim 1, it is characterised in that: The foam reducing composition is, by the polyvinyl acetate of 6-8 part of mass fraction meter, 5-10 parts of polyester polyol, 3-5 parts Glycerol, 1-3 parts of octanol, 2-3 parts of polymerization silicone oil ester, 3-4 parts of poly- butyl ester are added thereto in reaction kettle, carry out reaction 1-2 After hour, obtained substance is exactly foam reducing composition.
7. a kind of preparation method of multilayered structure type fullerene nano lubricating oil according to claim 1, it is characterised in that: The matal deactivator is the N for being 6-10 parts by mass fraction, N- diakylaminomethylene benzotriazole, 2-5 parts of N, N- Mixing machine is added in two salicylidene butanediamine, 3-5 parts of N, the addition of N- dimethyl benzene azoles, 4-6 parts of N, N- dimethyl siloxane The middle substance obtained after mixing should be exactly matal deactivator.
8. a kind of preparation method of multilayered structure type fullerene nano lubricating oil according to claim 1, it is characterised in that: The anticorrosive is made of fatty amine and fatty phenol, in terms of anticorrosive total volume percent, the fatty amine and fat Phenol content is 20~25%, and the fatty amine is N, and the sub- bigcatkin willow propane diamine of N '-two, fatty phenol is 2,6-di-tert-butyl p-cresol, The two mixes to obtain anti-corrosion of metal component with volume ratio 1:2 ratio;It is passivated cheating components: fatty amine salt 30-35%, the fat Amine salt is to prepare to obtain with volume ratio 1:1 ratio by benzotriazole, benzotriazole fatty amine salt;Antioxygen inhibition component: cerolin Fat acid 25-40%, the yeast fat acid are petroleum yeast fat acid C16-C18;The auxiliary additive, with volume basis Than meter, surface active composition, 60-70% including 30-40% disperse peat component, and the surface active composition is C4-C5 Quinoline and/or N-methylmorpholine;The surface active composition C4-C5 morpholine, N-methylmorpholine it is one such or two kinds with body Mixture of the product than equal proportion, the dispersion peat component: 10-20% yeast fat acid, 15-20% fatty amine calcium salt, it is described Fatty amine calcium salt be T154+T109 that polyisobutylene-bis-succinimide, alkyl calcium salicylate are prepared with volume ratio 1:1 ratio Mother liquor.
9. a kind of preparation method of multilayered structure type fullerene nano lubricating oil according to claim 1, it is characterised in that: The antioxidant is, by the hydroquinone of 5-9 part of mass fraction meter, 4-6 parts of p-methyl phenol, 2-3 parts of lemon Sour sodium, 4-8 parts of 2- butyl formate base -3- fourth agent phenol is added to the mixer the substance obtained after mixing, the object Matter is exactly antioxidant.
10. a kind of preparation method of multilayered structure type fullerene nano lubricating oil according to claim 1, feature exist In: the multilayered structure type fullerene nano lubricating oil the preparation method is as follows: controlling temperature of reaction kettle in 50-60 DEG C of item Under part, 100-120 parts of lubricating oil, 1-3 parts of multilayered structure type fullerene, the addition of 1-2 parts of auxiliary are added in a kettle Reaction is added in agent, 2-5 parts of foam reducing composition, 3-5 parts of matal deactivator, 3-6 parts of anticorrosive, 1-3 parts of antioxidant In kettle, agitator speed adjust to 600-800rpm, be stirred to react after forty minutes, by material be placed into ultrasonic instrument into Row ultrasonic disperse 1-2 hours, after dispersion completely, solution is taken out, which is exactly multilayered structure type fullerene nano lubricating oil.
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