CN109097155A - A kind of preparation method lubricating nanometer additive - Google Patents
A kind of preparation method lubricating nanometer additive Download PDFInfo
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- CN109097155A CN109097155A CN201811066419.1A CN201811066419A CN109097155A CN 109097155 A CN109097155 A CN 109097155A CN 201811066419 A CN201811066419 A CN 201811066419A CN 109097155 A CN109097155 A CN 109097155A
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- Prior art keywords
- lubricating
- nanometer
- surface modifier
- preparation
- carbon crystal
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Classifications
-
- 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
- C10M125/00—Lubricating compositions characterised by the additive being an inorganic material
- C10M125/02—Carbon; Graphite
-
- 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
- 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
-
- 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
-
- 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
- C10M2201/14—Inorganic compounds or elements as ingredients in lubricant compositions inorganic compounds surface treated with organic compounds
-
- 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
-
- 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
- C10N2030/08—Resistance to extreme temperature
-
- 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
- C10N2030/56—Boundary lubrication or thin film lubrication
Abstract
The invention discloses a kind of preparation methods for lubricating nanometer additive, comprising the following steps: carbon crystal is carried out shearing using wet type dispersing and milling method and forms it into micron particles；Addition surface modifier, which continues to grind, in grinding slurry forms it into nanoparticle, and the surface modifier includes at least two functional groups, and one of functional group is less than or equal to 720 for being implanted into nanometer fission surface, the relative molecular weight of the surface modifier.The lubrication nanometer additive prepared using the method for this programme; it is added into various lubricating oil; form stable suspension; contain millions of ultra-dispersed carbon crystal nano particles in this every liter of lubricating oil; they can be combined in friction process with the surface of solids, form smooth protective layer, while clogging Micro scratching; to which friction and wear be greatly lowered, especially acted under the conditions of heavy duty, low speed and high-temperature vibrating more significant.
Description
Technical field
A kind of product of the present invention nanosizing preparation field, and in particular to preparation method for lubricating nanometer additive.
Background technique
History of the super carbon crystal nano powder as the research existing more than ten years of lube oil additive, disperses in an adequate manner
A kind of stable suspension is formed in various lubricating oil, and millions of ultra-fine metal particles are contained in every liter of solution, they
Rolling lubrication protective layer is formed in conjunction with the surface of solids, while Micro scratching being clogged, and abrasion and friction can be greatly lowered, especially
It is acted under heavy duty, low speed and high-temperature condition more significant.But it is limited always by super carbon crystal fine powder production technology and cost
Mature product does not appear on the market.
Have chemical company and the newly established nano-dispersion liquid company of more families on the market at present, declares to can provide one
The nano-dispersion liquid of a little standards, but because most nano-dispersion liquid on the market is not modified by tailoring at all, institute
The nanometer grade powder of addition is easy due to modified to be agglomerated again, is not easy to be spread out, and leads to expected nanometer phenomenon not
There is generation, therefore it still can not directly be made to be applied to the exploitation of final nanoscale product and application.
Summary of the invention
In order to solve the above-mentioned technical problem the present invention provides a kind of preparation method for lubricating nanometer additive.
The present invention is achieved through the following technical solutions:
A kind of preparation method lubricating nanometer additive, comprising the following steps:
A, carbon crystal is carried out by shearing using wet type dispersing and milling method and forms it into micron particles；
B, surface modifier is added in grinding slurry continues grinding and form it into nanoparticle, the surface modifier includes extremely
Shao Liangge functional group, for being implanted into nanometer fission surface, the relative molecular weight of the surface modifier is small for one of functional group
In equal to 720.
Before entering interface modification technology, material dispersion is ground to micron or sub-micron grade, but reach very much nanometer
Partial size.Its main cause is the specific surface of powder at this time after the granular size of material disperses grinding nanoscale by mechanical force
Product sharply increase, Fan Dewaer stress effect and Brownian movement are more obvious, powder thus be easy it is agglomerated together once again, so not
How pipe disperses to grind again, and Come always can drop any more in partial size, can only generally disperse to be ground to 100 ~ 200 nm just can not again by
Partial size is toward decline, the reason is that the specific surface area of powder rapidly rises and Fan get Wa Erli is imitated when partial size is less than 300 nm
It should aggravate, powder is in highly unstable and extremely easy reunites again at this time.Solve the problems, such as this, it is necessary to use chemical machinery system
Standby method: above-mentioned surface modifier is done into surface face to nano-powder and is modified, reunites again to avoid nano-powder, disperses always
It is ground to until partial size reaches requirement requirement.This programme is less than or equal to C60 using above-mentioned lower molecular weight and relative molecular weight
Relative molecular weight 720 molecular weight be functional group as surface modifier, using the theory of solution chemistry, compared with small molecule
The chemical bond of amount is formed by functional group, will be easier to be implanted on the surface of nano-powder.Selected surface modifier
Simultaneously have a following two functional group: a functional group design is implanted into nanometer fission surface, it is therefore an objective to make nano powder surface
A constant phase state is formed, to avoid seperated generation of reuniting again；The design of another functional group is needed according to the nano powder in the future
The performance requirement of body determines the functional group of surface additive, occurs to avoid incompatible phenomenon.Because of this surface modifier system
Standby used wet type dispersing and milling method, so selected surface modifier need can be compatible with used solvent, although
The molecular weight very little of selected surface modifier.But still it can be in the film of nanoparticle surface generation 2-5nm thickness, enough
It generates a three-dimensional protective layer and supports the stability of nanoparticle.This programme uses wet type dispersing and milling method, because being wet
Therefore formula also can select smaller abrading-ball so the variation of slurry temperature is less susceptible to rapidly rise because of grinding, and such as 0.05-
0.1 mm abrading-ball is abrasive media, then the high mixing speed for example about 10 ~ 16m/s for grinder of arranging in pairs or groups, to shorten dispersion grinding
And the time needed for reaction.The lubrication nanometer additive prepared using the method for this programme, is added into various lubricating oil,
Stable suspension is formed, millions of ultra-dispersed carbon crystal nano particles are contained in this every liter of lubricating oil, they are rubbed
Can be combined with the surface of solids in journey, form smooth protective layer, while clogging Micro scratching, thus be greatly lowered friction and
Abrasion especially acts under the conditions of heavy duty, low speed and high-temperature vibrating more significant.
Preferably, further include the drying process to nanoparticle, the drying process the following steps are included:
Slurry after grinding is precipitated；
The method that moisture in sediment is removed as an azeotrope under reduced pressure is existed with the mixture of n-butanol and wet gel
Moisture is removed under conditions of azeotropic at less than 95 DEG C.Dry process nature is that a heat and mass transport makes moisture and small point
The process of sub- substance volatilization, nano material dry rate, temperature, equipment etc. are to nano material partial size and are dispersed with very high point
System.The method that this programme uses azeotropic distillation ,-O the H of nanoparticle surface is by-OC4 H9 Group replaces, the table of particle
Face can substantially reduce, to prevent reunion.
Preferably, step B is ground using homogenous disperse machine, the shear rate of the homogenous disperse machine is 180.00
Rpm to 220.00 rpm, the speed of rotor are 60m/s to 66m/s.Dispersion layering is dispersed phase in external force i.e. gravity or centrifugal force
Under effect, floating or the result sunk in continuous phase.Under the static conditions for ignoring Brownian movement effect, Stokes can be used
Law describes, i.e., dispersed phase spheric granules is determined by following formula due to the sinking speed v of gravity:
；
In formula: ρ s-ρ is the density contrast of dispersed phase and continuous phase, and g is acceleration of gravity, and d is dispersion particle diameter, and μ is to connect
The viscosity of continuous phase.If the continuous phase density of the density ratio of dispersion particle is big, particles sink, speed v is positive value, conversely, particle
It floats, speed is negative value.Sinking speed is big, and slurry is easy for being layered.If keeping stable system, sedimentation speed must be just reduced
Degree, can be by reducing dispersed phase Solids Particle Diameter d for specific slurry.Because only that when partial size reduces to continuous phase liquid
When body molecular size, particle could stablize, be evenly dispersed in liquid and do not separate.By above analysis, we can be with
Find out, to improve the stability of suspension, the partial size of dispersion particle should be tiny as far as possible.It should be understood that being done according to forefathers
Numerous studies discovery, with the reduction of grain graininess, although particle centrifugation caused by gravity becomes secondary factor,
But since the spacing between particle reduces, for example Van der Waals force plays important decisive role to the binding force between particle.
In addition, when particle diameter is less than a certain fine size, at this point, the Brownian movement effect of particle cannot have ignored, so by
In the Brownian movement of fine particle, and to generate between particle and intensely collide.If stabilizer is not added, these situations can all be led
Particle agglomeration is caused, the stabilization to system is unfavorable.So the thinner grain diameter not the better in the dispersion of slurry, slurry is regarded
Depending on the characteristic of material.Dispersion seeks to characteristic and feature according to material, reduces the granularity of dispersion particle, it is made to be distributed in one
A relatively narrow size range, and reach the mutual balance of suction and repulsion, to guarantee the stabilization of slurry system.Homogenous disperse machine
High revolving speed and shear rate be most important for obtaining ultra-fine fine suspension.By the revolving speed of homogenous disperse machine and shearing speed
Rate controls within the above range, and the turbulent flow combination motor speed as caused by shearing force can make particle size range small to nanoscale.
Further, the shear rate of the homogenous disperse machine is 200.00 rpm, and the speed of rotor can achieve 66m/
s。
Compared with prior art, the present invention having the following advantages and benefits:
1, the lubrication nanometer additive prepared using the method for this programme, is added into various lubricating oil, is formed stable
Suspension, containing millions of ultra-dispersed carbon crystal nano particles in this every liter of lubricating oil, they can be in friction process
The surface of solids combines, and forms smooth protective layer, while clogging Micro scratching, so that friction and wear is greatly lowered, especially
It is acted under the conditions of heavy duty, low speed and high-temperature vibrating more significant.
Specific embodiment
To make the objectives, technical solutions, and advantages of the present invention clearer, below with reference to embodiment, the present invention is made
Further to be described in detail, exemplary embodiment of the invention and its explanation for explaining only the invention, are not intended as to this
The restriction of invention.
Embodiment 1
A kind of preparation method lubricating nanometer additive, comprising the following steps:
A, carbon crystal is carried out by shearing using wet type dispersing and milling method and forms it into micron particles；
B, surface modifier is added in grinding slurry continues grinding and form it into nanoparticle, the surface modifier includes extremely
Shao Liangge functional group, the relative molecular weight of the surface modifier are less than or equal to 720, and one of functional group receives for being implanted into
The seperated surface of rice, depending on another functional group needs the interface being added according to the functional requirement of the nano-powder later, to avoid
Incompatible phenomenon occurs.For example: when the functional requirement of nano-powder is anticorrosive paint, selecting ZrO2It is implanted into C60, is mixed into
Anticorrosive paint original slurry material show fabulous intermiscibility, and agglomeration will not be generated.
Embodiment 2
Principle based on embodiment, the present embodiment enumerate a detailed mode of having a try and are described.
A, carbon crystal is carried out by shearing using wet type dispersing and milling method and forms it into micron particles, which can be used height and cut
Dispersion machine, three roller dispersion machines, ball mill etc. is cut to shear super carbon crystal.
B, in grinding slurry be added surface modifier continue grinding form it into nanoparticle, the surface modifier packet
At least two functional groups are included, one of functional group needs to be somebody's turn to do according to later for being implanted into nanometer fission surface, another functional group
Depending on the interface that the functional requirement of nano-powder is added, occur to avoid incompatible phenomenon.The step can be used according to willing public affairs
Department develops ERX2000 ultra high shear dispersion machine machine on the basis of ERS2000 series and realizes, controls the homogenous disperse machine
Shear rate is in 180.00 rpm to 220.00 rpm, and the speed of rotor is in 60m/s to 66m/s.In the velocity interval, by cutting
Turbulent flow caused by shear force combines the motor specially developed particle size range can be made small to nanoscale.Shearing force is stronger, lotion
Grain is narrower through being distributed.Since energy density is high, other aid dispersion equipment are not necessarily to, can achieve common high pressure homogenizer
Granular size under 400BAR pressure.
When being prepared using chemical machinery, the agitating ball mill process modified in the dispersion grinding of nano-powder and surface
In, many advantages are embodied, and play important role.This system uses wet type dispersing and milling method, because being wet
Therefore formula also can select smaller abrading-ball so the variation of slurry temperature is less susceptible to rapidly rise because of grinding, and such as 0.05-
0.1 mm abrading-ball is abrasive media, then the high mixing speed for grinder of arranging in pairs or groups, about 10 ~ 16 m/s, to shorten dispersion grinding
And the time needed for reaction.
The modified existing method in surface has very much, adjusts pH value, the macromolecule of tool high molecular weight or monomer for example to work as point
Powder is to allow steric repulsion active force Come to form the stable state of solid and solid, solid and liquid.But the above method is uncomfortable
The use in the Particle size requirements for the slurry to be dispersed or be ground are less than 100 nm the case where, at this point, according to tool high molecular weight
Macromolecule or monomer can have the following problems to work as dispersing agent: when fission is by nanosizing, most of volume in slurry by
The macromolecule or monomer of high molecular weight are formed by occupied by barrier, and slurry is likely to encounter following problem at this time: 1, it is solid at
Divide and be greatly reduced, is generally 35 % or less；2, the viscosity of slurry thus improves, the movement of small abrading-ball in unfavorable grinder,
Cause last partial size that can not fall Come；3, powder is easy to produce the phenomenon that reuniting again, causes nano particle that can not generate.We
For case using the functional group of the organic acid of low molecular weight as surface modifier, which has following two function simultaneously
Group: a functional group design is implanted into nanometer fission surface, it is therefore an objective to so that nano powder surface is formed constant phase state, to keep away
Exempt from seperated generation of reuniting again；The design of another functional group needs to determine surface according to the performance requirement of the nano-powder in the future
The functional group of additive.Occur to avoid incompatible phenomenon.After the surface modifier is added: 1, solid ingredient can greatly improve
To 35-45 % or more；2, partial size can drop to the size of demand partial size of powder；3, the viscosity of slurry no longer by
Particle diameter decline influence and steeply rise；4, powder will be not likely to produce agglomeration again, even if being added to rear end preparation material
When particle be still nanoparticle.
C, nanoparticle is dried, comprising the following steps:
Slurry after grinding is precipitated；
The method that moisture in sediment is removed as an azeotrope under reduced pressure, with the mixture of n-butanol and wet gel
Moisture is removed under conditions of azeotropic at less than 95 DEG C.
Carbon crystal powder average grain diameter is in regular engine oil in progress antiwear and antifriction, as a result the carbon nano-particles of 50nm are added to
It was found that: carbon crystal nanoparticle shows good abrasion resistance, can be substantially reduced the secondary abrasion loss of friction；Carbon crystal is added simultaneously
Nanoparticle and dispersing agent can further improve the abrasion resistance of oil product；For coefficient of friction, carbon crystal nanoparticle is only being added
Period of the day from 11 p.m. to 1 a.m coefficient of friction is increased slightly compared with base oil.Analyzing its reason may be to be divided in base oil due to carbon crystal nanoparticle
Dissipating unevenly makes oil product be deteriorated in the adsorptivity of surface of friction pair, i.e., oiliness is deteriorated.Carbon crystal nanoparticle is added at the same time and is divided
After powder, coefficient of friction has reduction by a relatively large margin compared with base oil, this is because dispersing agent can make carbon crystal nanoparticle equal
It is even to be dispersed in base oil, keep it not easy to reunite in friction process, to show good tribological property.
| Project | Base oil | + 0.5% copper nano-particle of base oil | + 0.5% copper nano-particle of base oil+dispersing agent |
| Wear scar width/mm | 2.90 | 0.91 | 0.73 |
| Minimized friction coefficient | 0.091 | 0.093 | 0.079 |
| Maximum friction coefficient | 0.100 | 0.105 | 0.084 |
Carbon crystal nanoparticle is surface modified, and solves the dispersion of the carbon crystal nanoparticle in lubricating oil, is used
The carbon crystal nanoparticle partial size about 30nm of above method synthesis has more superior wear-resistant and anti-extreme pressure energy.Compared with underload
Under, since the carbon crystal nanoparticle deposited on friction surface is attached on lubricant oil surface film, under high loads, a large amount of carbon crystal
Nanoparticle is deposited in friction surface, and the skin covering of the surface to form low shear strength is sprawled in melting under the high temperature and pressure of contact zone,
At this moment directly support load isolation substrate contact is carbon crystal nanoparticle, since carbon has lower shear strength,
Good antifriction antiwear is presented under high load capacity.The carbon crystal nanoparticle adsorbed close friction surface under moderate duty, due to carbon
Brilliant almost spherical, granularity control between 10 ~ 50nm.The addition of grit carbon crystal powder plays a kind of similar " ball bearing ",
Coefficient of friction and abrasion loss is set to be in lower value；Increase with load or speed improves, carbon crystal ball effect, which greatly inhibits, rubs
The rising for wiping coefficient, greatly reduces the abrasion of metal surface.
The lubrication nanometer additive prepared using this programme, realize super carbon crystal nanoparticle in oil base to it is wear-resistant, subtract
It rubs the quantum size effect and skin effect excellent with extreme pressure property additive, super carbon crystal additive can show special height
Bearing capacity performance, with the incomparable superiority of conventional solid lubricant.The super carbon crystal of nanoscale is added in lubricating oil
Additive is remarkably improved its greasy property and bearing capacity, especially suitable for the lubrication occasion under harsh conditions.
Above-described specific embodiment has carried out further the purpose of the present invention, technical scheme and beneficial effects
It is described in detail, it should be understood that being not intended to limit the present invention the foregoing is merely a specific embodiment of the invention
Protection scope, all within the spirits and principles of the present invention, any modification, equivalent substitution, improvement and etc. done should all include
Within protection scope of the present invention.
Claims (4)
1. a kind of preparation method for lubricating nanometer additive, which comprises the following steps:
A, carbon crystal is carried out by shearing using wet type dispersing and milling method and forms it into micron particles；
B, surface modifier is added in grinding slurry continues grinding and form it into nanoparticle, the surface modifier includes extremely
Shao Liangge functional group, for being implanted into nanometer fission surface, the relative molecular weight of the surface modifier is small for one of functional group
In equal to 720.
2. a kind of preparation method for lubricating nanometer additive according to claim 1, which is characterized in that further include to receiving
The drying process of rice corpuscles, the drying process the following steps are included:
Slurry after grinding is precipitated；
The method that moisture in sediment is removed as an azeotrope under reduced pressure is existed with the mixture of n-butanol and wet gel
Moisture is removed under conditions of azeotropic at less than 95 DEG C.
3. a kind of preparation method for lubricating nanometer additive according to claim 1, which is characterized in that step B is utilized
Homogenous disperse machine is ground, and the shear rate of the homogenous disperse machine is 180.00 rpm to 220.00 rpm, the speed of rotor
For 60m/s to 66m/s.
4. a kind of preparation method for lubricating nanometer additive according to claim 3, which is characterized in that the homogeneous point
The shear rate for dissipating machine is 200.00 rpm, and the speed of rotor can achieve 66m/s.
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| CN201811066419.1A CN109097155A (en) | 2018-09-13 | 2018-09-13 | A kind of preparation method lubricating nanometer additive |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201811066419.1A CN109097155A (en) | 2018-09-13 | 2018-09-13 | A kind of preparation method lubricating nanometer additive |
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|---|---|---|---|---|
| EP0634473A2 (en) * | 1993-07-15 | 1995-01-18 | Fujikura Kasei Co., Ltd. | Electrorheological fluid composition |
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| CN104152035A (en) * | 2014-08-12 | 2014-11-19 | 安徽碳索材料科技有限公司 | Oil-based radiation heat-loss paint and preparation method thereof |
| CN104877496A (en) * | 2015-04-24 | 2015-09-02 | 安徽华强防水防腐材料有限公司 | Important component of crack-resistant insulated flame-retardant building material coating |
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2018
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| EP0634473A2 (en) * | 1993-07-15 | 1995-01-18 | Fujikura Kasei Co., Ltd. | Electrorheological fluid composition |
| CN1441037A (en) * | 2003-03-10 | 2003-09-10 | 刘曼一 | Solid-liquid suspension as lubricant oil |
| US20070009419A1 (en) * | 2005-07-11 | 2007-01-11 | Apollo Diamond, Inc | Carbon grit |
| CN103189433A (en) * | 2010-09-03 | 2013-07-03 | 卡博特公司 | Modified fillers and elastomeric composites comprising same |
| CN104152035A (en) * | 2014-08-12 | 2014-11-19 | 安徽碳索材料科技有限公司 | Oil-based radiation heat-loss paint and preparation method thereof |
| CN104877496A (en) * | 2015-04-24 | 2015-09-02 | 安徽华强防水防腐材料有限公司 | Important component of crack-resistant insulated flame-retardant building material coating |
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| PB01 | Publication | ||
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| AD01 | Patent right deemed abandoned |
Effective date of abandoning: 20220114 |
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| AD01 | Patent right deemed abandoned |