CN110041985A - A kind of Composite Nanoparticles as Additive in Lubricating Oil and preparation method thereof with self-repair function - Google Patents
A kind of Composite Nanoparticles as Additive in Lubricating Oil and preparation method thereof with self-repair function Download PDFInfo
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- CN110041985A CN110041985A CN201910421013.9A CN201910421013A CN110041985A CN 110041985 A CN110041985 A CN 110041985A CN 201910421013 A CN201910421013 A CN 201910421013A CN 110041985 A CN110041985 A CN 110041985A
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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
- 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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- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M177/00—Special methods of preparation of lubricating compositions; Chemical modification by after-treatment of components or of the whole of a lubricating composition, not covered by other classes
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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
- C10M2201/04—Elements
- C10M2201/041—Carbon; Graphite; Carbon black
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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
- C10M2201/06—Metal compounds
- C10M2201/061—Carbides; Hydrides; Nitrides
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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
- C10M2201/06—Metal compounds
- C10M2201/062—Oxides; Hydroxides; Carbonates or bicarbonates
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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
- C10M2201/087—Boron oxides, acids or salts
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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
- C10M2201/10—Compounds containing silicon
- C10M2201/102—Silicates
- C10M2201/103—Clays; Mica; Zeolites
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
- C10M2201/10—Compounds containing silicon
- C10M2201/105—Silica
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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
- C10M2201/14—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
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- C10M2203/00—Organic non-macromolecular hydrocarbon compounds and hydrocarbon fractions as ingredients in lubricant compositions
- C10M2203/10—Petroleum or coal fractions, e.g. tars, solvents, bitumen
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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
- C10M2219/00—Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions
- C10M2219/02—Sulfur-containing compounds obtained by sulfurisation with sulfur or sulfur-containing compounds
- C10M2219/022—Sulfur-containing compounds obtained by sulfurisation with sulfur or sulfur-containing compounds of hydrocarbons, e.g. olefines
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- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2219/00—Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions
- C10M2219/04—Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions containing sulfur-to-oxygen bonds, i.e. sulfones, sulfoxides
- C10M2219/044—Sulfonic acids, Derivatives thereof, e.g. neutral salts
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- C10M2219/00—Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions
- C10M2219/06—Thio-acids; Thiocyanates; Derivatives thereof
- C10M2219/062—Thio-acids; Thiocyanates; Derivatives thereof having carbon-to-sulfur double bonds
- C10M2219/066—Thiocarbamic type compounds
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- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
- C10N2030/06—Oiliness; Film-strength; Anti-wear; Resistance to extreme pressure
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- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
- C10N2030/56—Boundary lubrication or thin film lubrication
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Abstract
The present invention discloses a kind of Composite Nanoparticles as Additive in Lubricating Oil and preparation method thereof with self-repair function, belongs to technical field of lubricating oil.Lube oil additive constituent of the present invention is as follows in parts by mass: composite nanoparticle 20-30 parts modified, 10-20 parts of fine mineral micro mist, 5-10 parts of sodium alkyl benzene sulfonate, 3-6 parts of antiwear additive and 3-5 parts of preservative.The present invention is easy to reunite nano particle additive in the prior art, bad dispersibility aiming at the problem that, select copper particle, nano-titanium dioxide and the additive of graphite and boron nitride as nanoparticle with laminated structure, it is modified by the way of Coated with Oleic Acid, ultrasonic disperse and high speed ball milling, it is aided with fine mineral micro mist, surface scratch can quickly and effectively be filled, to repair mechanical damage, the two mutual cooperation effect, to increase the lubricant effect of lubricating oil, extend Working Life of Lubricating Oil, anti-attrition anti-wear effect is significant.
Description
Technical field
The invention belongs to technical field of lubricating oil, and in particular to a kind of composite Nano lubricating oil with self-repair function adds
Add agent and preparation method thereof.
Background technique
Fretting wear is material and one of damage of facilities and the main form of failure, how effectively to control friction, subtracts
Less wear, improvement greasy property have become energy saving and material, shorten the important measures of maintenance time.Lubricant rubs in reduction
Wiping, reducing abrasion aspect is current most effective measure, and the use of additive is that raising oil property is most important and effective
Mode.But common antiwear additive contains S, Cl etc. and not only has corrosion to machine but also have the element of pollution to environment.Cause
This develops energy saving, pollution-free, efficient additive to replace original additive be always that scientific research personnel constantly explores
Direction.In recent years, nanoparticle as lube oil additive due to its good antifriction, wear-resistant, extruding and self-repair function
Attention by domestic and international scientific research personnel.
Nanoscale science and technology is considered as new science and technology geared to the 21st century, and good characteristic causes the wide of researcher
General attention.In recent years, nano material shows important application value and wide application prospect in fields such as light, electricity, magnetic,
Simultaneously because the good characteristic that there are nanoparticle many traditional conventional materials not have, to show special, excellent
Physicochemical properties enter everybody visual field.For nanoparticle as lube oil additive, advantage is mainly reflected in following three
A aspect: first is that the diffusivity of nanoparticle and self-diffusion ability are stronger, it is good that abrasion resistance is easily formed on the metal surface
Permeable formation or diffusion layer reach antifriction antiwear effect；Second is that nanoparticle has the characteristics that partial size is small, it is approximately ball in shape
Shape can roll between friction pair, function similarly to the effect of " ball bearing ", friction type is become rolling from sliding friction
Dynamic friction reduces coefficient of friction；Third is that nanoparticle can be polished and be strengthened to friction surface, and external load is supported,
Improve bearing capacity.However nanoparticle exists and has a single function as lube oil additive at present, nanoparticle is reunited,
Disperse unevenly, to cause its antiwear and reducing friction ineffective, good lubricant effect cannot be played in base oil.
Summary of the invention
To solve, nano particle additive dispersion effect existing in the prior art is bad, easy to reunite, asking of having a single function
Topic, the present invention provide a kind of favorable dispersibility, and the Composite Nanoparticles as Additive in Lubricating Oil with self-repair function, and disclose its tool
Preparation.
The technical scheme adopted by the invention is that:
A kind of Composite Nanoparticles as Additive in Lubricating Oil with self-repair function, constituent are as follows in parts by mass: modified
20-30 parts of composite nanoparticle, 10-20 parts of fine mineral micro mist, 5-10 parts of sodium alkyl benzene sulfonate, 3-6 parts of antiwear additive and anti-
Rotten agent 3-5 parts.
The modified composite nanoparticle is prepared by following methods:
(1) copper chloride and sodium hydroxide are weighed respectively, and are configured to the water that mass concentration is respectively 3mol/l and 3mol/l
Solution is gradually dropped sodium hydroxide solution according to volume ratio 1:5 while stirring copper chloride solution, obtains uniform hydrogen-oxygen
Change copper suspension；
(2) using deionized water washing step (1) gained Kocide SD suspension 3-5 times, then according to solid-to-liquid ratio 1g:
Composite nanoparticle is added in 3ml, and stirring obtains mixed liquor A afterwards for 24 hours, and mixed liquor A two volumes are then added in whipping process
, volumetric concentration be 30% formic acid solution, persistently stir 12h, obtain mixture B；
(3) oleic acid, petroleum ether and mixture B are mixed evenly according to volume ratio 1:1:1, add and with 80 DEG C at
Ultrasonic reaction 5h, and with ball milling 12h in planetary ball mill, separating obtained product is then centrifuged for, with 50 DEG C in vacuum desiccator
Lower drying for 24 hours, obtains modified composite nanoparticle.
Preferably, in step (2) composite nanoparticle be by nano-titanium dioxide, nano graphite powder and nm-class boron nitride by
It is obtained by mixing according to mass ratio 1:3:1.
Preferably, the revolving speed of planetary ball mill is 250 revs/min in step (3).
Preferably, the fine mineral micro mist is warp after being mixed by palygorskite powder, silicon dioxide powder according to mass ratio 1:1
It is obtained after crossing ball milling, for 24 hours, 300 revs/min of drum's speed of rotation, the average grain diameter for obtaining mixture is 70-100nm to ball milling.
Preferably, the preservative is zinc dialkyl dithiocarbamate or molybdenum dialkyldithiocarbamacompositions.
Preferably, the antiwear additive is sulfide isobutene or kodalk.
A kind of preparation method of the Composite Nanoparticles as Additive in Lubricating Oil with self-repair function, comprising the following steps:
(1) it prepares modified composite nanoparticle: weighing copper chloride and sodium hydroxide respectively, and be configured to mass concentration difference
Sodium hydroxide is gradually dropped according to volume ratio 1:5 while stirring copper chloride solution for the aqueous solution of 3mol/l and 3mol/l
Solution obtains uniform Kocide SD suspension；
(2) using deionized water washing step (1) gained Kocide SD suspension 3-5 times, then according to solid-to-liquid ratio 1g:
Composite nanoparticle is added in 3ml, and stirring obtains mixed liquor A afterwards for 24 hours, and mixed liquor A two volumes are then added in whipping process
, volumetric concentration be 30% formic acid solution, persistently stir 12h, obtain mixture B；
(3) oleic acid, petroleum ether and mixture B are mixed evenly according to volume ratio 1:1:1, add and with 80 DEG C at
Ultrasonic reaction 5h, and with ball milling 12h in planetary ball mill, separating obtained product is then centrifuged for, with 50 DEG C in vacuum desiccator
Lower drying for 24 hours, obtains modified composite nanoparticle；
(4) it after mixing palygorskite powder, silicon dioxide powder according to mass ratio 1:1, is obtained after ball milling, drum's speed of rotation
300 revs/min, for 24 hours, the average grain diameter for obtaining mixture is 70-100nm to ball milling, obtains fine mineral micro mist；
(5) will modified composite nanoparticle, fine mineral micro mist, sodium alkyl benzene sulfonate, antiwear additive and preservative according to
Parts by weight are uniformly mixed, and obtain additive of the present invention after planetary ball mill ball milling, and 80 revs/min of drum's speed of rotation, ball
Grind 1h.
Lube oil additive usage amount of the present invention is 98 parts of 2 parts of lube oil additive of the present invention of lubricating oil addition.
Each raw material used herein is commercially available gained.
The utility model has the advantages that
The present invention is easy to reunite nano particle additive in the prior art, bad dispersibility aiming at the problem that, select copper particle, receive
Rice titanium dioxide and the additive of graphite and boron nitride as nanoparticle with laminated structure, using Coated with Oleic Acid, ultrasound
Disperse and the mode of ball milling is told to be modified it, the carboxyl long-chain and Cu of oleic acid2+In conjunction with formation fatty acid salt, and with ion
The form of key is adsorbed on the surface of nanoparticle, so that interparticle distance becomes larger, interaction force reduces, and is aided with ultrasonic disperse and ball
Mill utmostly alleviates the agglomeration of nanoparticle, in addition with the graphite and boron nitride of lamellar structure, so that Cu particle exists
Mechanical friction process can be aided with fine mineral micro mist with fast filming, can quickly and effectively fill surface scratch, to repair mechanical damage
Wound, the two mutual cooperation effect extend Working Life of Lubricating Oil to increase the lubricant effect of lubricating oil, and anti-attrition anti-wear effect is aobvious
It writes.
Detailed description of the invention
Fig. 1 sample ultra-violet absorption spectrum with time of repose variation.
Fig. 2 specimen surface shape appearance figure, before 1 is repairs, after 2 is repair.
Specific embodiment
Technical scheme is described further combined with specific embodiments below, but not limited to this.
Embodiment 1
A kind of Composite Nanoparticles as Additive in Lubricating Oil with self-repair function, constituent are as follows in parts by mass: modified
20 parts of composite nanoparticle, 10 parts of fine mineral micro mist, 5 parts of sodium alkyl benzene sulfonate, 3 parts of antiwear additive and 3 parts of preservative.
The modified composite nanoparticle is prepared by following methods:
(1) copper chloride and sodium hydroxide are weighed respectively, and are configured to the water that mass concentration is respectively 3mol/l and 3mol/l
Solution is gradually dropped sodium hydroxide solution according to volume ratio 1:5 while stirring copper chloride solution, obtains uniform hydrogen-oxygen
Change copper suspension；
(2) using deionized water washing step (1) gained Kocide SD suspension 3-5 times, then according to solid-to-liquid ratio 1g:
Composite nanoparticle is added in 3ml, and stirring obtains mixed liquor A afterwards for 24 hours, and mixed liquor A two volumes are then added in whipping process
, volumetric concentration be 30% formic acid solution, persistently stir 12h, obtain mixture B；
(3) oleic acid, petroleum ether and mixture B are mixed evenly according to volume ratio 1:1:1, add and with 80 DEG C at
Ultrasonic reaction 5h, and with ball milling 12h in planetary ball mill, separating obtained product is then centrifuged for, with 50 DEG C in vacuum desiccator
Lower drying for 24 hours, obtains modified composite nanoparticle.
Composite nanoparticle is by nano-titanium dioxide, nano graphite powder and nm-class boron nitride according to quality in step (2)
It is obtained by mixing than 1:3:1.
The revolving speed of planetary ball mill is 250 revs/min in step (3).
The fine mineral micro mist is after being mixed by palygorskite powder, silicon dioxide powder according to mass ratio 1:1, after ball milling
It obtains, for 24 hours, 300 revs/min of drum's speed of rotation, the average grain diameter for obtaining mixture is 70-100nm to ball milling.
The preservative is zinc dialkyl dithiocarbamate.
The antiwear additive is sulfide isobutene.
A kind of preparation method of the Composite Nanoparticles as Additive in Lubricating Oil with self-repair function, comprising the following steps:
(1) it prepares modified composite nanoparticle: weighing copper chloride and sodium hydroxide respectively, and be configured to mass concentration difference
Sodium hydroxide is gradually dropped according to volume ratio 1:5 while stirring copper chloride solution for the aqueous solution of 3mol/l and 3mol/l
Solution obtains uniform Kocide SD suspension；
(2) using deionized water washing step (1) gained Kocide SD suspension 3 times, then according to solid-to-liquid ratio 1g:3ml
Be added composite nanoparticle, stirring obtain mixed liquor A afterwards for 24 hours, then in whipping process be added mixed liquor A two volumes,
The formic acid solution that volumetric concentration is 30%, persistently stirs 12h, obtains mixture B；
(3) oleic acid, petroleum ether and mixture B are mixed evenly according to volume ratio 1:1:1, add and with 80 DEG C at
Ultrasonic reaction 5h, and with ball milling 12h in planetary ball mill, separating obtained product is then centrifuged for, with 50 DEG C in vacuum desiccator
Lower drying for 24 hours, obtains modified composite nanoparticle；
(4) it after mixing palygorskite powder, silicon dioxide powder according to mass ratio 1:1, is obtained after ball milling, drum's speed of rotation
300 revs/min, for 24 hours, the average grain diameter for obtaining mixture is 70-100nm to ball milling, obtains fine mineral micro mist；
(5) will modified composite nanoparticle, fine mineral micro mist, sodium alkyl benzene sulfonate, antiwear additive and preservative according to
Parts by weight are uniformly mixed, and obtain additive of the present invention after planetary ball mill ball milling, and 80 revs/min of drum's speed of rotation, ball
Grind 1h.
Lube oil additive usage amount of the present invention is 98 parts of 2 parts of lube oil additive of the present invention of lubricating oil addition.
Embodiment 2
A kind of Composite Nanoparticles as Additive in Lubricating Oil with self-repair function, constituent are as follows in parts by mass: modified
25 parts of composite nanoparticle, 15 parts of fine mineral micro mist, 8 parts of sodium alkyl benzene sulfonate, 5 parts of antiwear additive and 4 parts of preservative.
The modified composite nanoparticle is prepared by following methods:
(1) copper chloride and sodium hydroxide are weighed respectively, and are configured to the water that mass concentration is respectively 3mol/l and 3mol/l
Solution is gradually dropped sodium hydroxide solution according to volume ratio 1:5 while stirring copper chloride solution, obtains uniform hydrogen-oxygen
Change copper suspension；
(2) using deionized water washing step (1) gained Kocide SD suspension 3-5 times, then according to solid-to-liquid ratio 1g:
Composite nanoparticle is added in 3ml, and stirring obtains mixed liquor A afterwards for 24 hours, and mixed liquor A two volumes are then added in whipping process
, volumetric concentration be 30% formic acid solution, persistently stir 12h, obtain mixture B；
(3) oleic acid, petroleum ether and mixture B are mixed evenly according to volume ratio 1:1:1, add and with 80 DEG C at
Ultrasonic reaction 5h, and with ball milling 12h in planetary ball mill, separating obtained product is then centrifuged for, with 50 DEG C in vacuum desiccator
Lower drying for 24 hours, obtains modified composite nanoparticle.
Composite nanoparticle is by nano-titanium dioxide, nano graphite powder and nm-class boron nitride according to quality in step (2)
It is obtained by mixing than 1:3:1.
The revolving speed of planetary ball mill is 250 revs/min in step (3).
The fine mineral micro mist is after being mixed by palygorskite powder, silicon dioxide powder according to mass ratio 1:1, after ball milling
It obtains, for 24 hours, 300 revs/min of drum's speed of rotation, the average grain diameter for obtaining mixture is 70-100nm to ball milling.
The preservative is molybdenum dialkyldithiocarbamacompositions.
The antiwear additive is kodalk.
A kind of preparation method of the Composite Nanoparticles as Additive in Lubricating Oil with self-repair function, comprising the following steps:
(1) it prepares modified composite nanoparticle: weighing copper chloride and sodium hydroxide respectively, and be configured to mass concentration difference
Sodium hydroxide is gradually dropped according to volume ratio 1:5 while stirring copper chloride solution for the aqueous solution of 3mol/l and 3mol/l
Solution obtains uniform Kocide SD suspension；
(2) using deionized water washing step (1) gained Kocide SD suspension 4 times, then according to solid-to-liquid ratio 1g:3ml
Be added composite nanoparticle, stirring obtain mixed liquor A afterwards for 24 hours, then in whipping process be added mixed liquor A two volumes,
The formic acid solution that volumetric concentration is 30%, persistently stirs 12h, obtains mixture B；
(3) oleic acid, petroleum ether and mixture B are mixed evenly according to volume ratio 1:1:1, add and with 80 DEG C at
Ultrasonic reaction 5h, and with ball milling 12h in planetary ball mill, separating obtained product is then centrifuged for, with 50 DEG C in vacuum desiccator
Lower drying for 24 hours, obtains modified composite nanoparticle；
(4) it after mixing palygorskite powder, silicon dioxide powder according to mass ratio 1:1, is obtained after ball milling, drum's speed of rotation
300 revs/min, for 24 hours, the average grain diameter for obtaining mixture is 70-100nm to ball milling, obtains fine mineral micro mist；
(5) will modified composite nanoparticle, fine mineral micro mist, sodium alkyl benzene sulfonate, antiwear additive and preservative according to
Parts by weight are uniformly mixed, and obtain additive of the present invention after planetary ball mill ball milling, and 80 revs/min of drum's speed of rotation, ball
Grind 1h.
Lube oil additive usage amount of the present invention is 98 parts of 2 parts of lube oil additive of the present invention of lubricating oil addition.
Embodiment 3
A kind of Composite Nanoparticles as Additive in Lubricating Oil with self-repair function, constituent are as follows in parts by mass: modified
30 parts of composite nanoparticle, 20 parts of fine mineral micro mist, 10 parts of sodium alkyl benzene sulfonate, 6 parts of antiwear additive and 5 parts of preservative.
The modified composite nanoparticle is prepared by following methods:
(1) copper chloride and sodium hydroxide are weighed respectively, and are configured to the water that mass concentration is respectively 3mol/l and 3mol/l
Solution is gradually dropped sodium hydroxide solution according to volume ratio 1:5 while stirring copper chloride solution, obtains uniform hydrogen-oxygen
Change copper suspension；
(2) using deionized water washing step (1) gained Kocide SD suspension 3-5 times, then according to solid-to-liquid ratio 1g:
Composite nanoparticle is added in 3ml, and stirring obtains mixed liquor A afterwards for 24 hours, and mixed liquor A two volumes are then added in whipping process
, volumetric concentration be 30% formic acid solution, persistently stir 12h, obtain mixture B；
(3) oleic acid, petroleum ether and mixture B are mixed evenly according to volume ratio 1:1:1, add and with 80 DEG C at
Ultrasonic reaction 5h, and with ball milling 12h in planetary ball mill, separating obtained product is then centrifuged for, with 50 DEG C in vacuum desiccator
Lower drying for 24 hours, obtains modified composite nanoparticle.
Composite nanoparticle is by nano-titanium dioxide, nano graphite powder and nm-class boron nitride according to quality in step (2)
It is obtained by mixing than 1:3:1.
The revolving speed of planetary ball mill is 250 revs/min in step (3).
The fine mineral micro mist is after being mixed by palygorskite powder, silicon dioxide powder according to mass ratio 1:1, after ball milling
It obtains, for 24 hours, 300 revs/min of drum's speed of rotation, the average grain diameter for obtaining mixture is 70-100nm to ball milling.
The preservative is molybdenum dialkyldithiocarbamacompositions.
The antiwear additive is sulfide isobutene.
A kind of preparation method of the Composite Nanoparticles as Additive in Lubricating Oil with self-repair function, comprising the following steps:
(1) it prepares modified composite nanoparticle: weighing copper chloride and sodium hydroxide respectively, and be configured to mass concentration difference
Sodium hydroxide is gradually dropped according to volume ratio 1:5 while stirring copper chloride solution for the aqueous solution of 3mol/l and 3mol/l
Solution obtains uniform Kocide SD suspension；
(2) using deionized water washing step (1) gained Kocide SD suspension 5 times, then according to solid-to-liquid ratio 1g:3ml
Be added composite nanoparticle, stirring obtain mixed liquor A afterwards for 24 hours, then in whipping process be added mixed liquor A two volumes,
The formic acid solution that volumetric concentration is 30%, persistently stirs 12h, obtains mixture B；
(3) oleic acid, petroleum ether and mixture B are mixed evenly according to volume ratio 1:1:1, add and with 80 DEG C at
Ultrasonic reaction 5h, and with ball milling 12h in planetary ball mill, separating obtained product is then centrifuged for, with 50 DEG C in vacuum desiccator
Lower drying for 24 hours, obtains modified composite nanoparticle；
(4) it after mixing palygorskite powder, silicon dioxide powder according to mass ratio 1:1, is obtained after ball milling, drum's speed of rotation
300 revs/min, for 24 hours, the average grain diameter for obtaining mixture is 70-100nm to ball milling, obtains fine mineral micro mist；
(5) will modified composite nanoparticle, fine mineral micro mist, sodium alkyl benzene sulfonate, antiwear additive and preservative according to
Parts by weight are uniformly mixed, and obtain additive of the present invention after planetary ball mill ball milling, and 80 revs/min of drum's speed of rotation, ball
Grind 1h.
Lube oil additive usage amount of the present invention is 98 parts of 2 parts of lube oil additive of the present invention of lubricating oil addition.
Comparative example 1
A kind of Composite Nanoparticles as Additive in Lubricating Oil with self-repair function, constituent are as follows in parts by mass: compound
30 parts of nanoparticle, 20 parts of fine mineral micro mist, 10 parts of sodium alkyl benzene sulfonate, 6 parts of antiwear additive and 5 parts of preservative.
Composite nanoparticle is to be mixed by nano-titanium dioxide, nano graphite powder and nm-class boron nitride according to mass ratio 1:3:1
It closes and obtains.
The fine mineral micro mist is after being mixed by palygorskite powder, silicon dioxide powder according to mass ratio 1:1, after ball milling
It obtains, for 24 hours, 300 revs/min of drum's speed of rotation, the average grain diameter for obtaining mixture is 70-100nm to ball milling.
The preservative is molybdenum dialkyldithiocarbamacompositions.
The antiwear additive is sulfide isobutene.
A kind of preparation method of the Composite Nanoparticles as Additive in Lubricating Oil with self-repair function, comprising the following steps:
(1) it after mixing palygorskite powder, silicon dioxide powder according to mass ratio 1:1, is obtained after ball milling, drum's speed of rotation
300 revs/min, for 24 hours, the average grain diameter for obtaining mixture is 70-100nm to ball milling, obtains fine mineral micro mist；
(2) by composite nanoparticle, fine mineral micro mist, sodium alkyl benzene sulfonate, antiwear additive and preservative according to weight
It part is uniformly mixed, obtains additive of the present invention after planetary ball mill ball milling, 80 revs/min of drum's speed of rotation, ball milling 1h.
Lube oil additive usage amount of the present invention is 98 parts of 2 parts of lube oil additive of the present invention of lubricating oil addition.
The present embodiment formula is except commercially available finished product nanoparticle is used, i.e., without modification, remaining is the same as embodiment 3.
Comparative example 2
A kind of Composite Nanoparticles as Additive in Lubricating Oil with self-repair function, constituent are as follows in parts by mass: modified
30 parts of composite nanoparticle, 10 parts of sodium alkyl benzene sulfonate, 6 parts of antiwear additive and 5 parts of preservative.
The modified composite nanoparticle is prepared by following methods:
(1) copper chloride and sodium hydroxide are weighed respectively, and are configured to the water that mass concentration is respectively 3mol/l and 3mol/l
Solution is gradually dropped sodium hydroxide solution according to volume ratio 1:5 while stirring copper chloride solution, obtains uniform hydrogen-oxygen
Change copper suspension；
(2) using deionized water washing step (1) gained Kocide SD suspension 3-5 times, then according to solid-to-liquid ratio 1g:
Composite nanoparticle is added in 3ml, and stirring obtains mixed liquor A afterwards for 24 hours, and mixed liquor A two volumes are then added in whipping process
, volumetric concentration be 30% formic acid solution, persistently stir 12h, obtain mixture B；
(3) oleic acid, petroleum ether and mixture B are mixed evenly according to volume ratio 1:1:1, add and with 80 DEG C at
Ultrasonic reaction 5h, and with ball milling 12h in planetary ball mill, separating obtained product is then centrifuged for, with 50 DEG C in vacuum desiccator
Lower drying for 24 hours, obtains modified composite nanoparticle.
Composite nanoparticle is by nano-titanium dioxide, nano graphite powder and nm-class boron nitride according to quality in step (2)
It is obtained by mixing than 1:3:1.
The revolving speed of planetary ball mill is 250 revs/min in step (3).
The preservative is molybdenum dialkyldithiocarbamacompositions.
The antiwear additive is sulfide isobutene.
A kind of preparation method of the Composite Nanoparticles as Additive in Lubricating Oil with self-repair function, comprising the following steps:
(1) it prepares modified composite nanoparticle: weighing copper chloride and sodium hydroxide respectively, and be configured to mass concentration difference
Sodium hydroxide is gradually dropped according to volume ratio 1:5 while stirring copper chloride solution for the aqueous solution of 3mol/l and 3mol/l
Solution obtains uniform Kocide SD suspension；
(2) using deionized water washing step (1) gained Kocide SD suspension 5 times, then according to solid-to-liquid ratio 1g:3ml
Be added composite nanoparticle, stirring obtain mixed liquor A afterwards for 24 hours, then in whipping process be added mixed liquor A two volumes,
The formic acid solution that volumetric concentration is 30%, persistently stirs 12h, obtains mixture B；
(3) oleic acid, petroleum ether and mixture B are mixed evenly according to volume ratio 1:1:1, add and with 80 DEG C at
Ultrasonic reaction 5h, and with ball milling 12h in planetary ball mill, separating obtained product is then centrifuged for, with 50 DEG C in vacuum desiccator
Lower drying for 24 hours, obtains modified composite nanoparticle；
(4) modified composite nanoparticle, sodium alkyl benzene sulfonate, antiwear additive and preservative are mixed according to parts by weight
It is even, obtain additive of the present invention after planetary ball mill ball milling, 80 revs/min of drum's speed of rotation, ball milling 1h.
Lube oil additive usage amount of the present invention is 98 parts of 2 parts of lube oil additive of the present invention of lubricating oil addition.
The present embodiment formula is in addition to without using fine mineral micro mist, remaining is the same as embodiment 3.
Test experiments
The base oil for taking ExxonMobil Chemical to produce is as lubricating oil, according to base oil: additive is the weight of 98:2
Portion rate is separately added into lube oil additive obtained by 1-3 of the embodiment of the present invention, comparative example 1-2, and comparative example 3 is arranged, and adds commercially available
Copper nanoparticle is as additive (Suzhou Chang Hu nanosecond science and technology Co., Ltd, base oil: copper powder=98:2)；Setting comparative example 4 (is pressed
The lube oil additive that specification request for utilization number is 200710121988.7), it is arranged and is arranged blank control, i.e., does not add and appoint
What additive, is uniformly mixed, and after standing 72h, observes lubricating oil form.Ultrasound 4h is distinguished again, and in 2000r/min
After being centrifuged 30min, then after standing 72h, lubricating oil form is observed again, records experimental result, as shown in table 1 below:
1 dispersion experiment test result of table
The data from table it will be seen that using additive obtained by 1-3 of the embodiment of the present invention lubricating oil, it is uniform steady
Fixed, stability is preferable, and comparative example 1-4 is being stood with after subsequent ultrasonic processing, different degrees of layering occurs.
Spectrophotometer, the ultraviolet suction of lubricating oil obtained by testing example, comparative example 1-4 and blank control group are used simultaneously
Spectrum is received to change with time.Every kind of substance has respectively different molecules, atomic and molecular structure, absorbs the energy of light energy
Power difference, therefore substance possesses fixed, distinctive absorption spectrum curve, it can be according to certain characteristic waves on absorption spectrum
The content of the height measurement substance of the absorbance of strong point.Specific experiment result is as shown in Fig. 1, it can be seen from the figure that with
The extension of time of repose, its UV absorption intensity of comparative example 1-4 are decreased obviously, it is seen that the absorbance in light area gradually increases, explanation
Particle generates precipitating in oil liquid.And the oil sample of embodiment, with time of repose extension UV absorption intensity and absorbance change not
Greatly, illustrate that particle can be with stable dispersion in oil liquid.
Meanwhile tribological property test and selfreparing reality are carried out to lube oil additive obtained by 1-3 of the embodiment of the present invention
It tests.
According to the maximum of GB/T3142-1982 load carrying capacity of lubricant measuring method (four ball method) measurement composite granule without seizing
Close load PB value and wear scar diameter D；When carrying out long according to SH/TO189-1992 lubrication oil antiwear damage performance measurement method (four ball method)
Between wear test；Sample mill spot is observed with optical microscopy.
| PB/N | D/mm | |
| Embodiment 1 | 471 | 0.331 |
| Embodiment 2 | 476 | 0.330 |
| Embodiment 3 | 477 | 0.330 |
| Comparative example 1 | 432 | 0.348 |
| Comparative example 2 | 435 | 0.345 |
| Comparative example 3 | 425 | 0.362 |
| Comparative example 4 | 426 | 0.366 |
| Blank control | 352 | 0.379 |
Selfreparing experimental method: it is Gr15 steel that this, which tests lower sample plate material, and upper sample pin material is common grey mouth casting
Iron HT250.This experiment first uses base oil, 4h wear test is carried out under the pressure of 400N load, after the test, same
The same area of one block of plate carries out 6h wear test using the lubricating oil that 3 gained additive of embodiment is added.It is repaired by comparison
Self-healing properties are probed into the variation of front and back friction pattern.It is illustrated in figure 2 and repairs the surface topography map that front and back examination is faced upward, it can in figure
To find out, before reparation, specimen surface polishing scratch is obvious, and after lubricated, surface indentation is significantly reduced, it is seen then that nanoparticle
Son has carried out effective filling to its surface, plays the role of reducing friction and reducing wearing, the self-repairing capability of elevating mechanism.
It should be noted that above-described embodiment is only the section Example for realizing preferred embodiment of the invention, Er Feiquan
Portion's embodiment.Obviously, it is based on the above embodiment of the present invention, those of ordinary skill in the art are not making creative work
Under the premise of other all embodiments obtained, should fall within the scope of the present invention.
Claims (8)
1. a kind of Composite Nanoparticles as Additive in Lubricating Oil with self-repair function, which is characterized in that constituent is in parts by mass
It is as follows: modified composite nanoparticle 20-30 parts, 10-20 parts of fine mineral micro mist, 5-10 parts of sodium alkyl benzene sulfonate, antiwear additive 3-6
Part and 3-5 parts of preservative.
2. according to claim 1 with the Composite Nanoparticles as Additive in Lubricating Oil of self-repair function, which is characterized in that described to change
Property composite nanoparticle is prepared by following methods:
(1) copper chloride and sodium hydroxide are weighed respectively, and are configured to the aqueous solution that mass concentration is respectively 3mol/l and 3mol/l,
According to volume ratio 1:5 while stirring copper chloride solution, it is gradually dropped sodium hydroxide solution, it is outstanding to obtain uniform Kocide SD
Turbid；
(2) using Kocide SD suspension 3-5 times obtained by deionized water washing step (1), then add according to solid-to-liquid ratio 1g:3ml
Enter composite nanoparticle, stirring obtains mixed liquor A afterwards for 24 hours, and mixed liquor A two volumes, body are then added in whipping process
The formic acid solution that product concentration is 30%, persistently stirs 12h, obtains mixture B；
(3) oleic acid, petroleum ether and mixture B are mixed evenly according to volume ratio 1:1:1, add and with 80 DEG C at ultrasound
React 5h, and with ball milling 12h in planetary ball mill, be then centrifuged for separating obtained product, in vacuum desiccator 50 DEG C do
It is dry for 24 hours, obtain modified composite nanoparticle.
3. according to claim 2 with the Composite Nanoparticles as Additive in Lubricating Oil of self-repair function, which is characterized in that step
(2) in composite nanoparticle be by nano-titanium dioxide, nano graphite powder and nm-class boron nitride according to mass ratio 1:3:1 mixing and
?.
4. according to claim 2 with the Composite Nanoparticles as Additive in Lubricating Oil of self-repair function, which is characterized in that step
(3) revolving speed of planetary ball mill is 250 revs/min in.
5. according to claim 1 with the Composite Nanoparticles as Additive in Lubricating Oil of self-repair function, which is characterized in that described super
Thin mineral micro powder is after being mixed by palygorskite powder, silicon dioxide powder according to mass ratio 1:1, to obtain after ball milling, ball milling for 24 hours,
300 revs/min of drum's speed of rotation, the average grain diameter for obtaining mixture is 70-100nm.
6. according to claim 1 with the Composite Nanoparticles as Additive in Lubricating Oil of self-repair function, which is characterized in that described anti-
Rotten agent is zinc dialkyl dithiocarbamate or molybdenum dialkyldithiocarbamacompositions.
7. according to claim 1 with the Composite Nanoparticles as Additive in Lubricating Oil of self-repair function, which is characterized in that described anti-
Grinding agent is sulfide isobutene or kodalk.
8. a kind of preparation side of the Composite Nanoparticles as Additive in Lubricating Oil described in claim 1-7 any one with self-repair function
Method, which comprises the following steps:
(1) it prepares modified composite nanoparticle: weighing copper chloride and sodium hydroxide respectively, and be configured to mass concentration and be respectively
It is molten to be gradually dropped sodium hydroxide according to volume ratio 1:5 while stirring copper chloride solution for the aqueous solution of 3mol/l and 3mol/l
Liquid obtains uniform Kocide SD suspension；
(2) using Kocide SD suspension 3-5 times obtained by deionized water washing step (1), then add according to solid-to-liquid ratio 1g:3ml
Enter composite nanoparticle, stirring obtains mixed liquor A afterwards for 24 hours, and mixed liquor A two volumes, body are then added in whipping process
The formic acid solution that product concentration is 30%, persistently stirs 12h, obtains mixture B；
(3) oleic acid, petroleum ether and mixture B are mixed evenly according to volume ratio 1:1:1, add and with 80 DEG C at ultrasound
React 5h, and with ball milling 12h in planetary ball mill, be then centrifuged for separating obtained product, in vacuum desiccator 50 DEG C do
It is dry for 24 hours, obtain modified composite nanoparticle；
(4) it after mixing palygorskite powder, silicon dioxide powder according to mass ratio 1:1, is obtained after ball milling, drum's speed of rotation 300
Rev/min, for 24 hours, the average grain diameter for obtaining mixture is 70-100nm to ball milling, obtains fine mineral micro mist；
(5) composite nanoparticle, fine mineral micro mist, sodium alkyl benzene sulfonate, antiwear additive and preservative will be modified according to weight
It part is uniformly mixed, obtains additive of the present invention after planetary ball mill ball milling, 80 revs/min of drum's speed of rotation, ball milling 1h.
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