CN108977253A - A kind of lubricating oil complex additive, preparation method and lubricating oil - Google Patents
A kind of lubricating oil complex additive, preparation method and lubricating oil Download PDFInfo
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- CN108977253A CN108977253A CN201811074753.1A CN201811074753A CN108977253A CN 108977253 A CN108977253 A CN 108977253A CN 201811074753 A CN201811074753 A CN 201811074753A CN 108977253 A CN108977253 A CN 108977253A
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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
- C10M161/00—Lubricating compositions characterised by the additive being a mixture of a macromolecular compound and a non-macromolecular compound, each of these compounds being essential
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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
- C10M2201/04—Elements
- C10M2201/041—Carbon; Graphite; Carbon black
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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
- C10M2201/04—Elements
- C10M2201/05—Metals; Alloys
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2227/00—Organic non-macromolecular compounds containing atoms of elements not provided for in groups C10M2203/00, C10M2207/00, C10M2211/00, C10M2215/00, C10M2219/00 or C10M2223/00 as ingredients in lubricant compositions
- C10M2227/04—Organic non-macromolecular compounds containing atoms of elements not provided for in groups C10M2203/00, C10M2207/00, C10M2211/00, C10M2215/00, C10M2219/00 or C10M2223/00 as ingredients in lubricant compositions having a silicon-to-carbon bond, e.g. organo-silanes
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2020/00—Specified physical or chemical properties or characteristics, i.e. function, of component of lubricating compositions
- C10N2020/01—Physico-chemical properties
- C10N2020/055—Particles related characteristics
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- 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
- C10N2030/04—Detergent property or dispersant property
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- 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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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Organic Chemistry (AREA)
- Lubricants (AREA)
Abstract
The present invention provides a kind of lubricating oil complex additives, are prepared by silane coupling agent, graphene and copper nano-wire；The mass ratio of the graphene and copper nano-wire is 1:(0.5~2)；The ratio between quality and the volume of silane coupling agent of the graphene are 1mg:(0.1~3.5) mL；The diameter of the copper nano-wire is 20~50nm；The length of the copper nano-wire is 10~900nm.Copper nano-wire and the effect of graphene compound system and steel ball surface form the good film layer of antiwear and friction reduction property；Meanwhile the layer structure of copper nano-wire and graphene can improve antifriction and the abrasion resistance of lubricating oil, even up to certain selfreparing effect performance makes greasy property be enhanced.By silanization treatment, its dissolubility in the oil is improved, improves its overall performance that rubs.The present invention also provides the preparation methods and lubricating oil of a kind of lubricating oil complex additive.
Description
Technical field
The invention belongs to lube oil additive technical field more particularly to a kind of lubricating oil complex additives, its preparation side
Method and lubricating oil.
Background technique
In order to improve the performance of lubricant, suitable additive can be added in certain lubricants.Pass through different lubrications
Oil additive can greatly promote antifriction and the abrasion resistance of lubricating oil, even up to certain selfreparing effect.Therefore it develops
Different lubricant additives improves the fretting wear of component of machine, prolongs its service life and reduces energy consumption and have become
For a current research hotspot.The admixed with additives to hold water assigns new property to lubricant, meets higher
It is required that.Lubricating oil is set more efficiently to play a role in finishing and transmission application.
Since 19th century, scientist starts to have carried out extensive research to the material in nanoscale, receives with all kinds of
Rice material is come out one after another, and the research of nano material is increasingly becoming a hot spot of scholars' research.Nano material compares table
Area is larger, Active sites number is more, has good heat resistance, antifriction, wear-resistant and extreme pressure property, this can guarantee it
Characteristic can stablize performance in lubricating oil, thus be widely used as lube oil additive.
In lubricating oil addition nanometer additive field, most addition particle is all single one kind, lubricating oil
Although performance has been improved, but there are no bring into play in complete set for many advantages of nanometer addition particle.Since in recent years,
The grinding of Nanocomposites additive make internal disorder or usurp have received it is extensive note that compound system nanoparticle refer to by two kinds or two kinds with
On the stable characteristic and the mechanism of action for being dispersed in lubricant, respectively having using different particles of nanoparticle, Neng Gouxian
Write the performance for improving lubricant.The tribological property that compound system nanoparticle is usually showed than single dose nanoparticle is more
It is excellent, therefore grinding to make internal disorder or usurp and be of great significance to compounding nanoparticle.
The guarantee for the tribological property that there is nano particle additive good dispersibility to be, nanoparticle itself have very
High polarity, so have very high chemical activity, the several factors such as surface energy height, oil-soluble difference, therefore nanoparticle is in the oil
Polymerization is easy to reunite.And compound its surface of nanoparticle can and chemical bond it is different, a possibility that more exacerbating reunion, thus point
Dissipating property difference is major issue of the nanoparticle in tribology.
Summary of the invention
The purpose of the present invention is to provide a kind of lubricating oil complex additive, preparation method and lubricating oil, in the present invention
Complex additive in lubricating oil good dispersion, have certain self-repair function, the performance of lubricating oil can be effectively improved.
The present invention provides a kind of lubricating oil complex additive, is prepared by silane coupling agent, graphene and copper nano-wire；
The mass ratio of the graphene and copper nano-wire is 1:(0.5~2)；
The ratio between quality and the volume of silane coupling agent of the graphene are 1mg:(0.1~3.5) mL；
The diameter of the copper nano-wire is 20~50nm；The length of the copper nano-wire is 10~900nm.
Preferably, the graphene with a thickness of 1~5nm.
Preferably, the mass ratio of the graphene and copper nano-wire is 1:1.
Preferably, the ratio between the quality of the graphene and the volume of silane coupling agent are 1mg:(0.2~3.2).
Preferably, the silane coupling agent is KH-560 silane coupling agent.
The present invention provides a kind of preparation method of lubricating oil complex additive, comprising the following steps:
A silane coupling agent) is dissolved in water, obtains silane coupler solution；
B) graphene and copper nano-wire are added in silane coupler solution, is stirred after ultrasonic disperse, obtains intermediate solution；
The mass ratio of the graphene and copper nano-wire is 1:(0.5~2)；
The ratio between quality and the volume of silane coupling agent of the graphene are 1mg:(0.1~3.5) mL；
The diameter of the copper nano-wire is 20~50nm；The length of the copper nano-wire is 10~900nm.
C) intermediate solution is dried, obtains lubricating oil complex additive.
Preferably, the time of the ultrasonic disperse is 10~50min；
The frequency of the ultrasonic disperse is 20KHz.
Preferably, the step B) in stir temperature be 50~100 DEG C；
The step B) in stir time be 0.1~1 hour.
Preferably, the temperature of the drying is 90~120 DEG C；
The time of the drying is 1~5 hour.
The present invention provides a kind of lubricating oil, including lubricating oil complex additive described above；
The additive amount of the lubricating oil complex additive is 1~10mg/mL lubricating oil.
The present invention provides a kind of lubricating oil complex additives, are prepared by silane coupling agent, graphene and copper nano-wire
It arrives；The mass ratio of the graphene and copper nano-wire is 1:(0.5~2)；The quality of the graphene and the body of silane coupling agent
The ratio between product is 1mg:(0.1~3.5) mL；The diameter of the copper nano-wire is 20~50nm；The length of the copper nano-wire is 10
~900nm.Copper nano-wire and graphene compound system can improve the antiwear and friction reduction property of basic rouge to a certain extent, in height
Effect is especially significant under load.Under frictional force effect, to form antiwear and friction reduction property good for compound system and steel ball surface effect
Good film layer；Meanwhile the layer structure of copper nano-wire and graphene easily aligns in the secondary opposite sliding process of friction, change rubs
Wiping the movement between pair is the interlayer slip inside additive, reduces frictional resistance, improves the antifriction and wear resistence of lubricating oil
Can, even up to certain selfreparing effect performance makes greasy property be enhanced.By silanization treatment, simply
The dispersibility for efficiently improving copper nano-wire and graphene compounding nanoparticle, improves its dissolubility in the oil, improves
Its overall performance of rubbing.
Detailed description of the invention
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technical description to be briefly described, it should be apparent that, the accompanying drawings in the following description is only this
The embodiment of invention for those of ordinary skill in the art without creative efforts, can also basis
The attached drawing of offer obtains other attached drawings.
Fig. 1 is dispersion of the Different adding amount complex additive in lubricating oil in the embodiment of the present invention 1；
Fig. 2 is frictional force-friction coefficient curve that the lubricating oil of 2.5mg complex additive is added in the embodiment of the present invention 1；
Fig. 3 is the metallographic microscope for having smeared the friction sample of lube product in the embodiment of the present invention 1 after friction testing.
Specific embodiment
The purpose of the present invention is to provide a kind of lubricating oil complex additives, by silane coupling agent, graphene and copper nanometer
Line is prepared；
The mass ratio of the graphene and copper nano-wire is 1:(0.5~2)；
The ratio between quality and the volume of silane coupling agent of the graphene are 1mg:(0.1~3.5) mL；
The diameter of the copper nano-wire is 20~50nm；The length of the copper nano-wire is 10~900nm.
In the present invention, the silane coupling agent is preferably KH-560 silane coupling agent, and the thickness of the graphene is preferred
For 1~5nm, more preferably 2~4nm, most preferably 2~3nm；The diameter of the copper nano-wire is preferably 20~50nm, more excellent
It is selected as 25~45nm, most preferably 30~40nm；The length of the copper nano-wire is preferably 10~900nm, more preferably 50~
800nm, most preferably 100~700nm, specifically, in an embodiment of the present invention, can be 200nm.Above-mentioned length range
Copper nano-wire is able to maintain original length of copper nano-wire, after being added in lubricating oil, the process of friction before the use
In, copper nano-wire can fragment into segment, be easy to be filled into polishing scratch, realize self-repair function.
In the present invention, the mass ratio of the graphene and copper nano-wire is 1:(0.5~2), preferably 1:(1~1.5),
More preferably 1:1；The ratio between quality and the volume of silane coupling agent of the graphene are 1mg:(0.1~3.5) mL, preferably
1mg:(0.2~3.2) mL, specifically, in an embodiment of the present invention, can be 1mg:0.8mL, 1mg:1.6mL or 1mg:
0.4mL。
Copper nano-wire and graphene in the present invention are easily aligned in the secondary opposite sliding process of friction, and it is secondary to become friction
Between movement be additive inside interlayer slip, reduce frictional resistance, improve antifriction and the abrasion resistance of lubricating oil.
The present invention also provides a kind of preparation methods of lubricating oil complex additive, comprising the following steps:
A silane coupling agent) is dissolved in water, obtains silane coupler solution；
B) graphene and copper nano-wire are added in silane coupler solution, is stirred after ultrasonic disperse, obtains intermediate solution；
The mass ratio of the graphene and copper nano-wire is 1:(0.5~2)；
The ratio between quality and the volume of silane coupling agent of the graphene are 1mg:(0.1~3.5) mL；
The diameter of the copper nano-wire is 20~50nm；The length of the copper nano-wire is 10~900nm.
C) intermediate solution is dried, obtains lubricating oil complex additive.
The present invention is soluble in water by silane coupling agent, is configured to silane coupler solution, then by the silane coupling agent
The pH value of solution is adjusted to 5.5,5~10min of stirring to complete hydrolysis.
In the present invention, the volume fraction of the silane coupler solution is preferably 0.5~2.0%, that is, 0.5~2.0mL
Silane coupling agent is dissolved in the water of 100mL, and more preferably 1~1.5%.Specifically, in an embodiment of the present invention, can be
0.5%, 1.0% or 2.0%.
After obtaining silane coupler solution, graphene and copper nano-wire are added in silane coupler solution the present invention, into
Row ultrasonic disperse, is then stirred again, coats copper nano-wire and graphene by silane coupling agent, obtains intermediate solution.
In the present invention, the type of the graphene, copper nano-wire and silane coupling agent, source and dosage and above stone
Black alkene, copper nano-wire and the type of silane coupling agent, source are consistent with dosage, and details are not described herein.
Siloxy has reactivity to inorganic matter, and organic functional base has reactivity or compatibility to organic matter.Therefore,
When silane coupling agent between inorganic between organic interface, organic matrix-silane coupling agent-inorganic matrix combination can be formed
Layer, the present invention are wrapped up graphene and copper nano-wire using silane coupling agent, improve the dispersibility of compounding particle.
The frequency of the ultrasonic disperse is preferably 20KHz；The time of the ultrasonic disperse is preferably 10~50min, more excellent
It is selected as 20~40min, most preferably 30min.
The temperature of the stirring is preferably 50~100 DEG C, more preferably 60~90 DEG C, most preferably 70~80 DEG C；It is described
The time of stirring is preferably 0.1~1 hour, more preferably 0.2~0.8 hour, most preferably 0.5~0.6 hour.
Finally intermediate solution is dried, obtaining chip solid is lubricating oil complex additive, by the addition of sheet
Agent is ground, and lubricating oil complex additive powder is obtained, and can be directly appended to use in lubricating oil.
The temperature of the drying is preferably 90~120 DEG C, and more preferably 100~110 DEG C；The time of the drying is preferably
1~5 hour, more preferably 2~4 hours.The drying is preferably dried in an oven.
The present invention also provides a kind of lubricating oil, including lubricating oil complex additive described above.
Preferably, the additive amount of the lubricating oil complex additive be 1~10mg/mL lubricating oil, more preferably 1.25~
5mg/mL lubricating oil, specifically, in an embodiment of the present invention, can be 5mg/mL lubricating oil, 2.5mg/mL lubricating oil or
1.25mg/mL lubricating oil.
Lubricating oil complex additive in the present invention is suitable for most of lubricating oil that market is sold.
The lubricating oil complex additive is added in lubricating oil by the present invention, then stirs in ultrasonic wave nano grinder
2 hours are crushed to get the finely dispersed lubricating oil of additive is arrived.
The present invention provides a kind of lubricating oil complex additives, are prepared by silane coupling agent, graphene and copper nano-wire
It arrives；The mass ratio of the graphene and copper nano-wire is 1:(0.5~2)；The quality of the graphene and the body of silane coupling agent
The ratio between product is 1mg:(0.1~3.5) mL；The diameter of the copper nano-wire is 20~50nm；The length of the copper nano-wire is 10
~900nm.Copper nano-wire and graphene compound system can improve the antiwear and friction reduction property of basic rouge to a certain extent, in height
Effect is especially significant under load.Under frictional force effect, to form antiwear and friction reduction property good for compound system and steel ball surface effect
Good film layer；Meanwhile the layer structure of copper nano-wire and graphene easily aligns in the secondary opposite sliding process of friction, change rubs
Wiping the movement between pair is the interlayer slip inside additive, reduces frictional resistance, improves the antifriction and wear resistence of lubricating oil
Can, even up to certain selfreparing effect performance makes greasy property be enhanced.By silanization treatment, simply
The dispersibility for efficiently improving copper nano-wire and graphene compounding nanoparticle, improves its dissolubility in the oil, improves
Its overall performance of rubbing.
In order to further illustrate the present invention, with reference to embodiments to a kind of lubricating oil compounding addition provided by the invention
Agent, preparation method and lubricating oil are described in detail, but cannot be understood as limiting the scope of the present invention.
Embodiment 1
First 0.5mLKH-560 silane coupling agent is dissolved in 100mL water, is made into 0.5% solution.Then by pH tune
To 5.5,5min complete hydrolysis is stirred.
Then by 0.625mg copper nano-wire (length of copper nano-wire is 200nm, and diameter is 30nm) and 0.625mg graphite
Alkene is added in the silane coupler solution after configured 100ml hydrolysis, ultrasonic disperse 30min is then carried out, at 80 DEG C
0.5h is stirred with blender, coats copper nano-wire and graphene by silane coupling agent；
The dry 2h in 100 DEG C of baking oven；It is chip solid after the completion of dry, finely ground, resulting powder is to be modified
Copper nano-wire graphene composite powder.
Copper nano-wire graphene composite powder in embodiment 1 is added to 100mL base grease as complex additive
In oily (Mobil 5W-40 type machine oil), stirring crushes 2h in ultrasonic wave nano grinder, obtains lube product.
In Fig. 1, it is followed successively by the lubrication for the composite granule being added in 1.25mg, 2.5mg and 5mg embodiment 1 from left to right
Oil, it can be seen that the nanometer addition compound of the copper nano-wire graphene compound system lubricating oil of different proportion is uniformly dispersed, not
There is reunion.
Fig. 2 is rubbing of measuring in the case where vertical load is 10N of the lubricating oil for the composite granule being added in 2.5mg embodiment 1
Power-friction coefficient curve is wiped, it can be concluded that, frictional force average out to 0.8916N, coefficient of friction average out to 0.089 lubricates by Fig. 2
Significant effect improves lubricant effect.
Fig. 3 is that the lubricating oil for the composite granule being added in 2.5mg embodiment 1 is applied to 5CrNiMo specimen surface, into
Metallographic microscope after row friction testing.A figure is the blank sample without smearing any lubricating oil, and b figure is to have smeared to be added to 2.5mg
The sample of the lubricating oil of composite granule in embodiment 1, by being can be seen that in figure without smearing copper nano-wire graphene compounding
The specimen surface of system lubricating oil has the pit of a large amount of ditch dug with a plow and some peelings, this is the typical case of abrasive wear.Copper is smeared
The surface of the sample wear track of nano wire graphene compound system lubricating oil is smooth, and ditch dug with a plow width is narrow, depth as shallow, peeling pit and
Ditch significantly reduces.
Embodiment 2
First 2.0mLKH-560 silane coupling agent is dissolved in 100mL water, is made into 2.0% solution.Then by pH tune
To 5.5,5min complete hydrolysis is stirred.
Then by 1.25mg copper nano-wire (length of copper nano-wire is 200nm, and diameter is 30nm) and 1.25mg graphene
In silane coupler solution after being added to configured 100ml hydrolysis, ultrasonic disperse 30min is then carried out, is used at 80 DEG C
Blender stirs 0.5h, coats copper nano-wire and graphene by silane coupling agent；
The dry 2h in 100 DEG C of baking oven；It is chip solid after the completion of dry, finely ground, resulting powder is to be modified
Copper nano-wire graphene composite powder.
Copper nano-wire graphene composite powder in embodiment 2 is added to 100mL base grease as complex additive
In oily (Mobil 5W-40 type machine oil), stirring crushes 2h in ultrasonic wave nano grinder, obtains lube product.
Embodiment 3
First 1.0mLKH-560 silane coupling agent is dissolved in 100mL water, is made into 1.0% solution.Then by pH tune
To 5.5,5min complete hydrolysis is stirred.
Then 2.5mg copper nano-wire (length of copper nano-wire is 200nm, and diameter is 30nm) and 2.5mg graphene are added
Enter into the silane coupler solution after configured 100ml hydrolysis, then carry out ultrasonic disperse 30min, with stirring at 80 DEG C
Device stirring 0.5h is mixed, coats copper nano-wire and graphene by silane coupling agent；
The dry 2h in 100 DEG C of baking oven；It is chip solid after the completion of dry, finely ground, resulting powder is to be modified
Copper nano-wire graphene composite powder.
Copper nano-wire graphene composite powder in embodiment 3 is added to 100mL base grease as complex additive
In oily (Mobil 5W-40 type machine oil), stirring crushes 2h in ultrasonic wave nano grinder, obtains lube product.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
Claims (10)
1. a kind of lubricating oil complex additive, is prepared by silane coupling agent, graphene and copper nano-wire；
The mass ratio of the graphene and copper nano-wire is 1:(0.5~2)；
The ratio between quality and the volume of silane coupling agent of the graphene are 1mg:(0.1~3.5) mL；
The diameter of the copper nano-wire is 20~50nm；The length of the copper nano-wire is 10~900nm.
2. lubricating oil complex additive according to claim 1, which is characterized in that the graphene with a thickness of 1~
5nm。
3. lubricating oil complex additive according to claim 1, which is characterized in that the matter of the graphene and copper nano-wire
Amount is than being 1:1.
4. lubricating oil complex additive according to claim 1, which is characterized in that the quality and silane of the graphene are even
Joining the ratio between volume of agent is 1mg:(0.2~3.2).
5. lubricating oil complex additive according to claim 1, which is characterized in that the silane coupling agent is KH-560 silicon
Alkane coupling agent.
6. a kind of preparation method of lubricating oil complex additive, comprising the following steps:
A silane coupling agent) is dissolved in water, obtains silane coupler solution；
B) graphene and copper nano-wire are added in silane coupler solution, is stirred after ultrasonic disperse, obtains intermediate solution；
The mass ratio of the graphene and copper nano-wire is 1:(0.5~2)；
The ratio between quality and the volume of silane coupling agent of the graphene are 1mg:(0.1~3.5) mL；
The diameter of the copper nano-wire is 20~50nm；The length of the copper nano-wire is 10~900nm；
C) intermediate solution is dried, obtains lubricating oil complex additive.
7. preparation method according to claim 6, which is characterized in that the time of the ultrasonic disperse is 10~50min；
The frequency of the ultrasonic disperse is 20KHz.
8. preparation method according to claim 6, which is characterized in that the step B) in stir temperature be 50~100
℃；
The step B) in stir time be 0.1~1 hour.
9. preparation method according to claim 6, which is characterized in that the temperature of the drying is 90~120 DEG C；
The time of the drying is 1~5 hour.
10. a kind of lubricating oil, including lubricating oil complex additive described in Claims 1 to 5 any one or claim 6~
Lubricating oil complex additive made from preparation method described in 9 any one；
The additive amount of the lubricating oil complex additive is 1~10mg/mL lubricating oil.
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