CN106147958A - A kind of lubricant oil composite and preparation method thereof - Google Patents
A kind of lubricant oil composite and preparation method thereof Download PDFInfo
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- CN106147958A CN106147958A CN201510189202.XA CN201510189202A CN106147958A CN 106147958 A CN106147958 A CN 106147958A CN 201510189202 A CN201510189202 A CN 201510189202A CN 106147958 A CN106147958 A CN 106147958A
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Abstract
The present invention relates to lubricating oil field, specifically provide a kind of lubricant oil composite and preparation method thereof.Described lubricant oil composite contains silicone oil base oil and the rubber particles with cross-linked structure prepared by cross-linking radiation method being dispersed in described silicone oil base oil, described silicone oil base oil is continuous phase, described rubber particles is dispersion phase, and relative to the described silicone oil base oil of 100 weight portions, the content of described rubber particles is 0.001-40 weight portion.The lubricant oil composite that the present invention provides can regulate viscosity effectively along with the change of temperature, compared with the lubricant oil composite containing the rubber particles by chemical crosslinking, its at low temperatures viscosity lower, and at high temperature viscosity is higher, therefore, it has good viscosity temperature characteristic.
Description
Technical field
The present invention relates to a kind of lubricant oil composite, the preparation method of described lubricant oil composite and by this
The lubricant oil composite that method prepares.
Background technology
The lifting each time of lubricating oil quality, is nearly all that the result developed broken through by oil dope.Nanometer
The new science and technology that science and technology was born as phase late 1980s, the application in lubricating oil is the most prominent
Going out, nanometre metal powder reduces friction, reduces abrasion when having become lubrication as novel solid lubricant
One of effective approach.The most domestic research to nanometer additive is scarcely out of swaddling-clothes, and this is mainly
Because nano-particle is difficult to or is difficult to be dissolved in oil, it is also difficult to be stably scattered in lubricating oil.Along with people
Deepening continuously to the research field of lubricating oil, find by reducing particle diameter, and with oleophylic macromolecule pair
After it is modified, additive shows excellent performance in lubricating oil, hence it is evident that improve base oil
Tribological property, there is good development prospect.
Prior art has had the report of a large amount of application about inorganic nano-particle in lubricating oil field
Road.Such as, CN1150958A discloses a kind of Low-density high temperature resistant wear-resistant self-lubricating nano particle filling
Strengthening polymer composite, it is made up of thermoplasticity heat-resistant polymer and nanoparticle, described nanometer
Microgranule includes nano-silicon nitride, nanometer silicon carbide and nano silicon, and this product has excellent profit certainly
Slip energy.CN1301319C discloses a kind of lubricant oil composite containing nano silicon dioxide particles,
This lubricant oil composite is the lubricating oil extreme pressure of a kind of function admirable, antiwear composite, and this technical scheme is adopted
Nanometer is achieved in order to the mode of base oil and nano silicon and interpolation dispersing aid and synergist
The dispersion of silicon dioxide microparticle.CN1180079A and CN1354056A individually discloses and repaiies through fatty acid
Decorations metal-oxide or the nano powder of hydroxide and through sulfur-bearing for the organic compound modified gold of phosphorus
Belong to the copper nano particles application in lubricating oil field.CN1827753A discloses a kind of fluorine-containing rare earth nano
Lube oil additive and preparation method thereof, this additive includes base oil and itrogenous organic substance Surface coating
Rare earth fluoride nanoparticle.CN101058760A discloses a kind of nano ceramic lubricating oil and preparation thereof
Method, it contains the composition of traditional lubrication oil, and with the addition of modified Nano on the basis of traditional lubrication oil
Ceramic particle, it belongs to the preparation field of mechanical movement lubricating oil medium, is particularly well-suited to automobile industry
Lubricating oil used and preparation method thereof.In the invention, successfully prepared stably by pre-dispersed method
The concentrated solution of scattered nano-ceramic particle, and then prepare nano-ceramic particle weight percentage and be
The nano ceramics machine oil of 0.00001%-5%.CN101235337B discloses one and is applicable to automobile internal
Machine or the slipper of power transmitting apparatus or sliding component are to significantly reduce the lubrication line of oils of coefficient of friction
Compound, this lubricant oil composite contains lubricating oil base oil, oxygen-containing organic compound, diamond nano
Granule and diamond nano-particles dispersant.CN101555430A discloses a kind of lubricant oil composite,
It contains oil base stock and nano carbon microsphere, and described nano carbon microsphere surface grafting has alkyl so that it is be scattered in base
In plinth oil plant, described nano carbon microsphere be hollow structure or be filled with metal, metal alloy, metal-oxide,
Metal carbides, metal sulfide, metal nitride or metal boride.
Additionally, in addition to inorganic nano-particle, also have some to lead at lubricating oil about organic fine particles gel
The report of the application in territory.Such as, the patent of Rhein Chemie Rheinau GmbH's application
CN1856527A, CN1840622A and CN1861673A disclose a kind of non-crosslinkable organic
Micro gel in medium and the micro gel of crosslinking are for the temperature of modified non-crosslinked organic media
Degree relies on the purposes of performance.But, this several patents application is pointed out bar none, described micro gel
Be all use chemical crosslinking mode (such as, by with polyfunctional compound's crosslinking copolymerization or passed through
Oxide cross-links) micro gel for preparing rather than the micro gel with high-energy radiation crosslinking.On
State the micro gel that patent application thinks that high-energy radiation cross-links to be actually unable in preparing on an industrial scale, radiation
Property cobalt source the using with serious safety problem, and by the micro gel of crosslinking with radiation of high-energy radiation
Time in plastic matrix, can occur to tear effect between substrate and dispersion phase, thus compromise and contain
There are the mechanical performance of the plastics of this micro gel, swelling behavior, stress corrosion cracking performance etc..But,
Rhein Chemie Rheinau GmbH application patent CN1856527A, CN1840622A and
The viscosity temperature characteristic of the lubricant oil composite disclosed in CN1861673A is poor, gluing of this lubricant oil composite
Spend along with the reduction of temperature can be increased dramatically, and along with the rising of temperature can strongly reduce, but at low temperature
Lower viscosity is excessive or the at high temperature too small application the most not utilizing lubricant oil composite of viscosity, and this will be very
The application of this lubricant oil composite is limited in big degree.Therefore, need exploitation one badly and have the most viscous
The lubricant oil composite of warm nature energy.
Summary of the invention
The invention aims to the defect overcoming existing lubricant oil composite viscosity temperature characteristic poor, and
There is provided a kind of and there is the lubricant oil composite of excellent viscosity temperature characteristic, the preparation method of a kind of lubricant oil composite
And the lubricant oil composite prepared by the method.
The present inventor finds after further investigation, Rhein Chemie Rheinau GmbH's application
Above-mentioned several patents CN1856527A, CN1840622A and CN1861673A disclosed lubrication line of oils
Dispersion phase in compound is to use polyfunctional compound or peroxide to be obtained by chemical crosslinking mode
Micro gel, although the lubricant oil composite containing this microgel particle can reduce organic to a certain extent
The coefficient of friction of medium, but the viscosity of these lubricant oil composites is influenced by temperature relatively big, and temperature is too
High (viscosity is the least) or the lowest (viscosity is the biggest) all can limit the use of this lubricant oil composite, is suitable for
Temperature range is narrower.And the rubber particles with cross-linked structure prepared by cross-linking radiation method is with logical
Cross the silicon rubber with cross-linked structure using polyfunctional compound or peroxide to carry out chemical crosslinking preparation
Micelle has diverse microstructure.When the dispersion phase in lubricant oil composite is for hand over by irradiation
When prepared by linked method has the rubber particles of cross-linked structure, corresponding lubricant oil composite has well
Viscosity temperature characteristic, it is possible to very well regulate viscosity along with the change of temperature, reduce low temperature viscosity and also carry
High high temperature viscosity, therefore, it can make up the shadow caused viscosity due to the change of temperature to a great extent
Ring.Additionally, high-energy radiation the most very cleaning, safety and the efficient energy, the most by a lot
Developed country is widely used for the fields such as health care, food processing, commercial production, is employingization on the contrary
Learn cross-linking method (peroxide) and there is some very important problems, as the highest in production efficiency, peroxide
Compound residual and the environmental pollution etc. that may cause, these all can limit its application.
Additionally, due to silicone oil base oil is basically identical with the chemical constitution of rubber particles, according to structure phase
Like compatibility principle, both are fully compatible, and rubber particles will significantly improve the limit of silicone oil base oil
Boundary's greasy property, and improve viscosity temperature characteristic and antiwear and friction reduction property further, this is for promoting silicone oil basis
The greasy property of oil, widen the equal important in inhibiting of range of application of silicone oil base oil.
Based on above-mentioned discovery, the present inventor completes the present invention.
Specifically, the invention provides a kind of lubricant oil composite, wherein, described lubricant oil composite contains
Have silicone oil base oil and be dispersed in described silicone oil base oil by prepared by cross-linking radiation method having
The rubber particles of cross-linked structure, described silicone oil base oil is continuous phase, and described rubber particles is dispersion
Phase, and relative to the described silicone oil base oil of 100 weight portions, the content of described rubber particles is
0.001-40 weight portion.
Present invention also offers the preparation method of a kind of lubricant oil composite, the method includes silicone oil basis
Fat liquor is entered successively with the rubber particles emulsion with cross-linked structure prepared by cross-linking radiation method
Row mixing, altogether breakdown of emulsion and redispersion, and relative in the described silicone oil basis fat liquor of 100 weight portions
Silicone oil base oil, the consumption of the solid content of described rubber particles emulsion is 0.001-40 weight portion.
Additionally, present invention also offers the lubricant oil composite prepared by said method.
The lubricant oil composite that the present invention provides can regulate viscosity effectively along with the change of temperature, and contains
The lubricant oil composite having the rubber particles by chemical crosslinking is compared, and it is viscous under low temperature (40 DEG C)
Spend lower, and viscosity is higher under high temperature (100 DEG C), it is possible to meet temperature and reach more than 200 DEG C occasions
Use requirement, therefore, significantly widened the use temperature range of this lubricant oil composite.
Additionally, the lubricant oil composite that the present invention provides can be used for blends engine oil, gear oil, hydraulic pressure
Other hot industry oil such as oil, are particularly applied to the field such as electromotor higher to viscosity temperature characteristic requirement
Oil, it is adaptable to regulation viscosity temperature characteristic poor with double ring arene, polycyclic aromatic hydrocarbon and non-hydrocarbons base oil be
The viscosity temperature characteristic of the lubricating composition of key component, easily can adjust according to the demand in different operating place
Save out the lubricating oil with different viscosity temperature characteristic.
Other features and advantages of the present invention will be described in detail in detailed description of the invention part subsequently.
Detailed description of the invention
Hereinafter the detailed description of the invention of the present invention is described in detail.It should be appreciated that this place is retouched
The detailed description of the invention stated is merely to illustrate and explains the present invention, is not limited to the present invention.
The lubricant oil composite that the present invention provides contains silicone oil base oil and is dispersed in described silicone oil base oil
In the rubber particles with cross-linked structure prepared by cross-linking radiation method, described silicone oil base oil
For continuous phase, described rubber particles is dispersion phase, and relative to the described silicone oil basis of 100 weight portions
Oil, the content of described rubber particles is 0.001-40 weight portion.Wherein, described rubber particles is at silicon
In stable dispersion state in oil base oil.
The lubricant oil composite provided according to the present invention, as discussed previously with respect to described in 100 weight portions
Silicone oil base oil, the content of described rubber particles is 0.001-40 weight portion.But so that Silicon-oil-based
Plinth oil and rubber particles play more preferable coordinated effect, and and then make the lubricant oil composite obtained
There is more preferable viscosity temperature characteristic, it is preferable that relative to the described silicone oil base oil of 100 weight portions, described
The content of rubber particles is 0.001-10 weight portion, more preferably 0.001-5 weight portion.
The lubricant oil composite provided according to the present invention, it is preferable that the mean diameter of described rubber particles
For 20-2000nm, more preferably 50-1000nm, particularly preferably 70-500nm.When by described silicon rubber
When the mean diameter of micelle controls within the above range, it is possible to more effectively regulate lubricant oil composite
Viscosity, has the cold start-up of more preferable temperature pumping and mobile performance, beneficially plant equipment, and at height
It is also beneficial to be formed thicker oil film under temperature, reduces mantle friction, i.e. be suitable for broader use temperature
Scope.
The lubricant oil composite provided according to the present invention, it is preferable that the gel content of described rubber particles
It is more than 60 weight %, more than more preferably 75 weight %, more than particularly preferably 80 weight %.When
When the gel content of described rubber particles is controlled within the above range, it is possible to along with temperature change more
Effectively regulate the viscosity of lubricant oil composite, be suitable for broader use temperature range.In the present invention,
Described gel content be this area for characterizing a kind of Common Parameters of rubber cross degree, its according to
Method disclosed in CN1402752A records.
The kind of described rubber particles is not particularly limited by the present invention, for example, it is possible to selected from methyl
Rubber particles (including dimethyl silicone rubber particle), ethyl rubber particles, hydroxyl rubber particles,
Hydrogeneous methyl silicone rubber particle, hydrogeneous hydroxyl rubber particles, methyl vinyl silicone rubber particle, methyl
Ethenylphenyl rubber particles, methyl ethylene trifluoro propyl rubber particles, phenylene silicone rubber grain
In son, phenylene ether base rubber particles, nitrile silicone rubber particle, silicon boron rubber particles and fluorosioloxane rubber particle
At least one.
Additionally, the rubber particles that the present invention provides preferably has equal phase structure.In the present invention, described
" equal phase structure " refers to observe under existing microtechnique, does not find layering, divides in rubber particles
The most homogeneous equal phenomenon.
The lubricant oil composite provided according to the present invention, the high-energy ray source used by described cross-linking radiation is concrete
At least one in cobalt source, ultraviolet, high-energy electron accelerator can be selected from, it is preferable that described high energy is penetrated
The wavelength of line source is less than 0.1 μm, for example, cobalt source.Additionally, generally, the dosage of irradiation should make
The gel content obtaining the rubber particles after rubber latex cross-linking radiation reaches more than 60 weight %, preferably
Reach more than 75 weight %, more than more preferably up to 80 weight %.Specifically, the dosage of irradiation is permissible
For 0.1-30Mrad, preferably 0.5-20Mrad.
The kind of described silicone oil base oil is not particularly limited by the present invention, can be unmodified silicone oil,
Can also be unmodified silicone oil, it is also possible to for the mixture of modified silicon oil Yu unmodified silicone oil.
Specifically, the example of described unmodified silicone oil includes but not limited to: methyl-silicone oil, ethyl silicon oil,
Phenyl silicone oil, Methyl Hydrogen Polysiloxane Fluid, methyl phenyl silicone oil, methylchlorophenyl silicone oil, methyl ethoxy silicon
Oil, methyl trifluoro propyl silicone oil, methyl vinyl silicon oil, methylhydroxy silicone oil, ethyl containing hydrogen silicone oil,
Hydroxyl hydrogen silicone oil and containing at least one in nitrile silicone, preferably methyl-silicone oil.
Described unmodified silicone oil refer to use some modified group to substitute the part methyl group in silicone oil and
The modified silicon oil obtained, modified silicon oil is not only a kind of extraordinary silicon with common dimethicone speciality
Oil, and according to import different modified groups, silicone oil is endowed multiple new characteristic, as water solublity,
The compatibility or with the reactivity of various other materials, coating etc..The example of described modified silicon oil include but
Be not limited to: amino-modified silicone oil, epoxy-modified silicone oil, polyether modified silicon oil, Carboxyl Modified Polydimethylsiloxane,
Alcoholic extract hydroxyl group modified silicon oil, phenolic group modified silicone oil, sulfhydryl modified silicone oil, polysiloxane-polyethers are embedding
Section modification by copolymerization silicone oil, alkyl and polyether modified silicon oil, alkyl ether polyether silicone oil, epoxy radicals are polyether-modified
Silicone oil, amino-polyether block silicone oil, glycerol ether silicone oil, phosphoric acid cruel base silicone oil, glycosyl polyethers silicone oil and
At least one in Radix Betae base silicone oil.
Additionally, the lubricant oil composite that the present invention provides can also be containing conventional additive.Described interpolation
The kind of agent includes but not limited to: age resistor, antiwear additive, antilubricant, antioxidant, anti-foaming agent, antirust
Agent, detersive, dispersant, pigment, extreme pressure composition, friction protection compositions, detersive, coupling
At least one in agent etc..The consumption of described additive can be the conventional selection of this area, to this ability
Field technique personnel all can know, therefore not to repeat here.
The preparation method of lubricant oil composite that the present invention provides include by silicone oil basis fat liquor with pass through
The rubber particles emulsion of cross-linked structure that prepared by cross-linking radiation method have carries out mixing successively, breakdown of emulsion altogether
With redispersion, and relative to the silicone oil base oil in the described silicone oil basis fat liquor of 100 weight portions, institute
The consumption of the solid content stating rubber particles emulsion is 0.001-40 weight portion.
According to the preparation method of the lubricant oil composite that the present invention provides, as discussed previously with respect to 100 weights
Silicone oil base oil in the described silicone oil basis fat liquor of amount part, the solid content of described rubber particles emulsion
Consumption be 0.001-40 weight portion.But so that silicone oil base oil and rubber particles play preferably
Coordinated effect, and and then make the lubricant oil composite obtained have more preferable viscosity temperature characteristic, it is preferable that
Relative to the silicone oil base oil in the described silicone oil basis fat liquor of 100 weight portions, described rubber particles
The consumption of the solid content of emulsion is 0.001-10 weight portion, more preferably 0.001-5 weight portion.
According to the preparation method of the lubricant oil composite that the present invention provides, silicon in the fat liquor of described silicone oil basis
The content of oil base oil and the solid content of rubber particles emulsion can be each independently 10 weight % with
On, preferably it is each independently more than 20 weight %, is more preferably each independently more than 30 weight %.
Preparation method according to the lubricant oil composite that the present invention provides, it is preferable that described rubber particles
In emulsion, the mean diameter of rubber particles is 20-2000nm, more preferably 50-1000nm, the most excellent
Elect 70-500nm as.
Preparation method according to the lubricant oil composite that the present invention provides, it is preferable that described rubber particles
In emulsion, the gel content of rubber particles is more than 60 weight %, more than more preferably 75 weight %,
More than particularly preferably 80 weight %.When by the gel of rubber particles in described rubber particles emulsion
When content controls within the above range, it is possible to along with the change of temperature more effectively regulates lubricant oil composite
Viscosity, be suitable for broader use temperature range.
Rubber particles in described rubber particles emulsion preferably has equal phase structure.In the present invention,
Described " equal phase structure " refers to observe under existing microtechnique, the rubber particles in rubber particles emulsion
The most do not find the most homogeneous phenomenons such as layering, split-phase.
The rubber particles emulsion that the present invention provides is prepared by cross-linking radiation by silicone rubber emulsion.?
In the preparation process of described rubber particles emulsion, the high-energy ray source used by cross-linking radiation specifically can be selected
At least one in cobalt source, ultraviolet, high-energy electron accelerator, it is preferable that described high-energy ray source
Wavelength is less than 0.1 μm, for example, cobalt source.Additionally, generally, the dosage of irradiation should make rubber
The gel content of the rubber particles after emulsion cross-linking radiation reaches more than 60 weight %, preferably reaches 75
More than weight %, more than more preferably up to 80 weight %.Specifically, the dosage of irradiation can be
0.1-30Mrad, preferably 0.5-20Mrad.
Described rubber particles emulsion can be commercially available, it is also possible to known to art technology
Various methods prepare.Such as, described rubber particles emulsion can be according to applicant of the present invention
In the international patent application WO01/40356 (priority date 1999 that JIUYUE in 2000 is submitted on the 18th
December 3 days) and the international patent application submitted June 15 calendar year 2001 of applicant of the present invention
WO01/98395 (priority date on June 15th, 2000) prepares during fully vulcanized powder rubber selected
Emulsion carry out cross-linking radiation and obtain.Additionally, the example of described rubber particles emulsion includes but not limited to:
Methyl silicone rubber particle emulsion (including dimethyl silicone rubber particle emulsion), ethyl rubber particles emulsion,
Hydroxyl rubber particles emulsion, hydrogeneous methyl silicone rubber particle emulsion, hydrogeneous hydroxyl rubber particles emulsion,
Methyl vinyl silicone rubber particle emulsion, methyl vinyl phenyl rubber particles emulsion, methyl ethylene
Trifluoro propyl rubber particles emulsion, phenylene silicone rubber particle emulsion, phenylene ether base rubber particles breast
In liquid, nitrile silicone rubber particle emulsion, silicon boron rubber particles emulsion and fluorosioloxane rubber particle emulsion at least one
Kind.In described rubber particles emulsion, the gel content of rubber particles is preferably more than 60 weight %,
More than more preferably 75 weight %, more than particularly preferably 80 weight %.Described rubber particles emulsion
The mean diameter of middle rubber particles is preferably 20-2000nm, more preferably 50-1000nm, the most excellent
Elect 70-500nm as.Additionally, each rubber particle in described rubber particles emulsion is homogeneous
, under existing microscopy, i.e. in microgranule, do not find the most homogeneous phenomenons such as layering, split-phase.
Additionally, in the cross-linking radiation preparation process of described rubber particles emulsion, crosslinking can not be used
Auxiliary agent, it is possible to use crosslinking coagent.Described crosslinking coagent can be selected from simple function group crosslinking coagent, two
Functional group's crosslinking coagent, trifunctional crosslinking coagent, four-functional group crosslinking coagent and five functional groups are to submit
Connection auxiliary agent in any one.The example of described simple function group crosslinking coagent includes but not limited to: (methyl)
In 1-Octyl acrylate, (methyl) Isooctyl acrylate monomer, (methyl) glycidyl acrylate at least one
Kind；The example of described two functional group's crosslinking coagents includes but not limited to: 1,4-butanediol two (methyl) third
Olefin(e) acid ester, 1,6-HD two (methyl) acrylate, diethylene glycol two (methyl) acrylate,
Triethylene glycol two (methyl) acrylate, neopentyl glycol two (methyl) acrylate, divinylbenzene
In at least one；The example of described trifunctional crosslinking coagent includes but not limited to: trimethylolpropane
Three (methyl) acrylate and/or tetramethylolmethane three (methyl) acrylate；Described four-functional group cross-links
The example of auxiliary agent includes but not limited to: tetramethylolmethane four (methyl) acrylate and/or ethoxyquin Ji Wusi
Alcohol four (methyl) acrylate；The example of the described five above crosslinking coagents of functional group includes but not limited to:
Dipentaerythritol five (methyl) acrylate.In this article, described (methyl) acrylate refers to third
Olefin(e) acid ester or methacrylate.These crosslinking coagents can be applied in combination in any way, as long as they
Contribute to cross-linking under irradiation.Additionally, the addition of described crosslinking coagent is generally dry glue in latex
0.1-10 weight % of weight, preferably 0.5-9 weight %, more preferably 0.7-7 weight %.
Additionally, the preparation method of the lubricant oil composite of present invention offer can also include additive and silicon
Oil base oil emulsion and rubber particles emulsion together mix.
Silicone oil base oil and the kind of additive in the fat liquor of described silicone oil basis have been described above
Being described, therefore not to repeat here.
According to a kind of detailed description of the invention of the present invention, described silicone oil basis fat liquor is by toward silicone oil basis
Oil adds emulsifying agent, then utilizes emulsifying device to carry out emulsifying and obtain.Wherein, described emulsifying agent
Kind can be the conventional selection of this area, for example, it is possible to selected from existing various non-ionic surface actives
Agent, cationic surfactant, anion surfactant, amphoteric surfactant, polyacrylamide
At least one in the non-ionic additive that emulsifying agent, esters non-ionic additive and terminal hydroxy group are closed, is specially
As well known to those skilled in the art, therefore not to repeat here.Additionally, described emulsifying device can stir selected from emulsifying
Mix at least one in machine, colloid mill and homogenizer.
Described mixing, the altogether mode of breakdown of emulsion and redispersion are not particularly limited, as long as can by the present invention
Rubber particles is effectively dispersed in silicone oil base oil thus obtains using silicone oil base oil as continuously
Lubricant oil composite mutually and with rubber particles as dispersion phase.One according to the present invention is preferably
Embodiment, the mode of described mixing, common breakdown of emulsion and redispersion includes: (1) is by described rubber particles
Emulsion is added in the fat liquor of described silicone oil basis and is mixed by mechanical agitation so that described rubber particles
Emulsion dispersion, in the fat liquor of described silicone oil basis, obtains preliminary scattered compositions；(2) by the beginning of described
Walk scattered compositions and carry out common breakdown of emulsion, then remove moisture therein, obtain breakdown of emulsion liquid；(3) by institute
State breakdown of emulsion liquid and carry out redispersion, until the mean diameter of the rubber particles after Fen San reaches 20-2000nm
In the range of, preferably reach in the range of 50-1000nm, in the range of more preferably up to 70-500nm.
Rubber particles is enabled to original grain by the way of this preferred mixing, altogether breakdown of emulsion and redispersion
Footpath is dispersed in silicone oil base oil, and the viscosity temperature characteristic of the lubricant oil composite obtained is more preferably.
Mechanical agitation mixing described in step (1) can be entered in existing various mechanical mixing equipments
OK, for example, it is possible to carry out in the mechanical mixing equipment such as homogenizer, kneader.The present invention is to institute
The condition stating mechanical agitation mixing is also not particularly limited, as long as being prepared by cross-linking radiation method making
The rubber particles emulsion with cross-linked structure and the performance of silicone oil basis fat liquor there is no any change
On the premise of, make the rubber particles emulsion dispersion with cross-linked structure prepared by cross-linking radiation method
Or be suspended in the fat liquor of silicone oil basis, these those skilled in the art all can be known, do not make at this
Repeat.
The mode being total to breakdown of emulsion in step (2) is not particularly limited by the present invention, it is for instance possible to use
Add at least one in demulsifier, centrifugation, heated and stirred, lyophilization and vacuum drying to carry out altogether
Breakdown of emulsion.
Redispersion described in step (3) can homogenizer, bead mill, three-roll grinder,
In single screw extrusion machine, multi-screw extruder, kneader, dissolvers and ultrasonic disperser at least one
Plant in mixing apparatus and carry out, preferably carry out in homogenizer, three-roll grinder and ultrasonic disperser, this
Three kinds of preferred mixing apparatus have fairly simple excellent of processing output height, good mixing effect, follow-up cleaning
Point.Most preferably, being redispersed in homogenizer described in step (3) is carried out.In dispersive process,
According to different dust dispersion quality requirements, need to cool down cycles samples, then iterate through mixing apparatus and carry out
Repeatedly disperse, until the mean diameter of the rubber particles being dispersed in silicone oil base oil reaches
In the range of 20-2000nm, in the range of preferably reaching 50-1000nm, more preferably up to 70-500nm model
In enclosing.Additionally, the condition of described redispersion is not particularly limited by the present invention, as long as making Silicon-oil-based
Plinth oil and rubber particles performance in dispersive process are not destroyed, and make the particle diameter of rubber particles
Reach 20-2000nm, preferably reach 50-1000nm, more preferably up to 70-500nm, to this
Those skilled in the art all can know, therefore not to repeat here.
Present invention also offers the lubricant oil composite prepared by said method.
Hereinafter will be described the present invention by embodiment.
(1) raw material used in embodiment and comparative example is as follows:
Simethicone emulsion, Beijing sea cowry think company produce, dimethyl-silicon oil content is 35 weight %,
Viscosity is 350cp (1cp=1mPa.s).
Simethicone emulsion, Beijing sea cowry think company produce, dimethyl-silicon oil content is 35 weight %,
Viscosity is 500cp.
Dimethyl silicone rubber emulsion, Sinopec produces, and the trade mark is vp-661, and solid content is 35 weight
%, gel content is 88 weight %, and wherein the mean diameter of silicone rubber is 100nm, sees under the microscope
Examine, in the dimethyl silicone rubber particle in this dimethyl silicone rubber emulsion, do not find layering, noted phase separation phenomena.
This dimethyl silicone rubber emulsion is by adding 15g trimethylolpropane toward 1kg dimethyl silicone rubber latex
Triacrylate, is stirred 1 hour mix homogeneously, is obtained by cobalt-60 radiosterilize afterwards, irradiation dose
20Mrad。
Peroxide crosslinking dimethyl silicone rubber emulsion is entered according to method disclosed in patent CN1840622A
Row prepare, rubber latex be dimethyl silicone rubber latex (with prepare dimethyl silicone rubber emulsion
The dimethyl silicone rubber latex that vp-661 is used is identical), the cross-linking agent of employing is cumyl peroxide
(DCP), dimethyl silicone rubber grain in the final peroxide crosslinking dimethyl silicone rubber particle emulsion obtained
Mean diameter 100nm of son, solid content is 35 weight %, and gel content is 88 weight %.
(2) viscosity of the lubricant oil composite in following example and comparative example: use HAAKE
RheoStress RS300 flow graph (subsidiary TC501 attemperating unit), C60/1 ° of Ti module are measured,
Test 40 DEG C respectively, 60 DEG C, 80 DEG C, viscosity at 100 DEG C.
Embodiment 1
Lubricant oil composite that this embodiment provides for the present invention is described and preparation method thereof.
By simethicone emulsion and the 1 weight portion dimethyl silicone rubber emulsion of 100 weight portion 350cp
Vp-661 mixes and carries out mechanical agitation uniformly, and then the oil bath high speed at 95 DEG C stirs (stirring speed
Degree for 10000rpm/min, lower with) 6 hours carry out common breakdown of emulsion, then remove water therein, broken
Emulsion.Above-mentioned breakdown of emulsion liquid homogenizing in high pressure homogenizer being circulated three times, homogenization pressure is 100MPa,
Obtaining lubricant oil composite, its viscosity is shown in Table 1.
Embodiment 2
Lubricant oil composite that this embodiment provides for the present invention is described and preparation method thereof.
By simethicone emulsion and the 3 weight portion dimethyl silicone rubber emulsions of 100 weight portion 350cp
Vp-661 mixes and carries out mechanical agitation uniformly, and then the oil bath high speed at 95 DEG C stirs to enter for 6 hours
Row breakdown of emulsion altogether, then removes water therein, obtains breakdown of emulsion liquid.By above-mentioned breakdown of emulsion liquid in high pressure homogenizer
Homogenizing circulates three times, and homogenization pressure is 100MPa, obtains lubricant oil composite, and its viscosity is shown in Table 1.
Embodiment 3
Lubricant oil composite that this embodiment provides for the present invention is described and preparation method thereof.
By simethicone emulsion and the 5 weight portion dimethyl silicone rubber emulsions of 100 weight portion 350cp
Vp-661 mixes and carries out mechanical agitation uniformly, and then the oil bath high speed at 95 DEG C stirs to enter for 6 hours
Row breakdown of emulsion altogether, then removes water therein, obtains breakdown of emulsion liquid.By above-mentioned breakdown of emulsion liquid in high pressure homogenizer
Homogenizing circulates three times, and homogenization pressure is 100MPa, obtains lubricant oil composite, and its viscosity is shown in Table 1.
Embodiment 4
Lubricant oil composite that this embodiment provides for the present invention is described and preparation method thereof.
By simethicone emulsion and the 7.5 weight portion dimethyl silicone rubber emulsions of 100 weight portion 350cp
Vp-661 mixes and carries out mechanical agitation uniformly, and then the oil bath high speed at 95 DEG C stirs to enter for 6 hours
Row breakdown of emulsion altogether, then removes water therein, obtains breakdown of emulsion liquid.By above-mentioned breakdown of emulsion liquid in high pressure homogenizer
Homogenizing circulates three times, and homogenization pressure is 100MPa, obtains lubricant oil composite, and its viscosity is shown in Table 1.
Embodiment 5
Lubricant oil composite that this embodiment provides for the present invention is described and preparation method thereof.
By simethicone emulsion and the 10 weight portion dimethyl silicone rubber emulsions of 100 weight portion 350cp
Vp-661 mixes and carries out mechanical agitation uniformly, and then the oil bath high speed at 95 DEG C stirs to enter for 6 hours
Row breakdown of emulsion altogether, then removes water therein, obtains breakdown of emulsion liquid.By above-mentioned breakdown of emulsion liquid in high pressure homogenizer
Homogenizing circulates three times, and homogenization pressure is 100MPa, obtains lubricant oil composite, and its viscosity is shown in Table 1.
Embodiment 6
Lubricant oil composite that this embodiment provides for the present invention is described and preparation method thereof.
By simethicone emulsion and the 1 weight portion dimethyl silicone rubber emulsion of 100 weight portion 500cp
Vp-661 mixes and carries out mechanical agitation uniformly, and then the oil bath high speed at 95 DEG C stirs to enter for 6 hours
Row breakdown of emulsion altogether, then removes water therein, obtains breakdown of emulsion liquid.By above-mentioned breakdown of emulsion liquid in high pressure homogenizer
Homogenizing circulates three times, and homogenization pressure is 100MPa, obtains lubricant oil composite, and its viscosity is shown in Table 2.
Embodiment 7
Lubricant oil composite that this embodiment provides for the present invention is described and preparation method thereof.
By simethicone emulsion and the 3 weight portion dimethyl silicone rubber emulsions of 100 weight portion 500cp
Vp-661 mixes and carries out mechanical agitation uniformly, and then the oil bath high speed at 95 DEG C stirs to enter for 6 hours
Row breakdown of emulsion altogether, then removes water therein, obtains breakdown of emulsion liquid.By above-mentioned breakdown of emulsion liquid in high pressure homogenizer
Homogenizing circulates three times, and homogenization pressure is 100MPa, obtains lubricant oil composite, and its viscosity is shown in Table 2.
Embodiment 8
Lubricant oil composite that this embodiment provides for the present invention is described and preparation method thereof.
By simethicone emulsion and the 5 weight portion dimethyl silicone rubber emulsions of 100 weight portion 500cp
Vp-661 mixes and carries out mechanical agitation uniformly, and then the oil bath high speed at 95 DEG C stirs to enter for 6 hours
Row breakdown of emulsion altogether, then removes water therein, obtains breakdown of emulsion liquid.By above-mentioned breakdown of emulsion liquid in high pressure homogenizer
Homogenizing circulates three times, and homogenization pressure is 100MPa, obtains lubricant oil composite, and its viscosity is shown in Table 2.
Comparative example 1
This comparative example is for lubricant oil composite that reference is described and preparation method thereof.
Lubricant oil composite is prepared, except for the difference that, by 5 weight portion dimethyl according to the method for embodiment 8
The silicone rubber emulsion vp-661 peroxide crosslinking dimethyl silicone rubber emulsion of 5 weight portions substitutes,
To reference lube compositions, its viscosity is shown in Table 2.
Embodiment 9
Lubricant oil composite that this embodiment provides for the present invention is described and preparation method thereof.
By simethicone emulsion and the 7.5 weight portion dimethyl silicone rubber emulsions of 100 weight portion 500cp
Vp-661 mixes and carries out mechanical agitation uniformly, and then the oil bath high speed at 95 DEG C stirs to enter for 6 hours
Row breakdown of emulsion altogether, then removes water therein, obtains breakdown of emulsion liquid.By above-mentioned breakdown of emulsion liquid in high pressure homogenizer
Homogenizing circulates three times, and homogenization pressure is 100MPa, obtains lubricant oil composite, and its viscosity is shown in Table 2.
Embodiment 10
Lubricant oil composite that this embodiment provides for the present invention is described and preparation method thereof.
By simethicone emulsion and the 10 weight portion dimethyl silicone rubber emulsions of 100 weight portion 500cp
Vp-661 mixes and carries out mechanical agitation uniformly, and then the oil bath high speed at 95 DEG C stirs to enter for 6 hours
Row breakdown of emulsion altogether, then removes water therein, obtains breakdown of emulsion liquid.By above-mentioned breakdown of emulsion liquid in high pressure homogenizer
Homogenizing circulates three times, and homogenization pressure is 100MPa, obtains lubricant oil composite, and its viscosity is shown in Table 2.
Table 1
Table 2
From the contrast of embodiment 8 and comparative example 1 it can be seen that with containing being obtained by peroxide crosslinking
The lubricant oil composite of Si powder rubber particles compare, containing by having that cross-linking radiation method obtains
The lubricant oil composite of the Si powder rubber particles of cross-linked structure (40 DEG C) viscosity when low temperature is lower, and
When high temperature, (100 DEG C) viscosity is higher, and therefore, the lubricant oil composite that the present invention provides has more preferably
Viscosity temperature characteristic, thus there is the cold of more preferable temperature pumping and mobile performance, beneficially plant equipment and open
Dynamic, and at high temperature it is also beneficial to be formed thicker oil film, reduce mantle friction, improve lubricant effect,
Being suitable for broader temperature range simultaneously, and can reduce friction, energy-saving effect is more preferably.
The preferred embodiment of the present invention described in detail above, but, the present invention is not limited to above-mentioned reality
Execute the detail in mode, in the technology concept of the present invention, can be to the technical side of the present invention
Case carries out multiple simple variant, and these simple variant belong to protection scope of the present invention.
It is further to note that each the concrete technology described in above-mentioned detailed description of the invention is special
Levy, in the case of reconcilable, can be combined by any suitable means.In order to avoid need not
The repetition wanted, various possible compound modes are illustrated by the present invention the most separately.
Additionally, combination in any can also be carried out between the various different embodiment of the present invention, as long as its
Without prejudice to the thought of the present invention, it should be considered as content disclosed in this invention equally.
Claims (19)
1. a lubricant oil composite, it is characterised in that described lubricant oil composite contains silicone oil basis
Oil and be dispersed in described silicone oil base oil by prepared by cross-linking radiation method, there is cross-linked structure
Rubber particles, described silicone oil base oil is continuous phase, and described rubber particles is dispersion phase, and relatively
In the described silicone oil base oil of 100 weight portions, the content of described rubber particles is 0.001-40 weight portion.
Lubricant oil composite the most according to claim 1, wherein, relative to 100 weight portions
Described silicone oil base oil, the content of described rubber particles is 0.001-10 weight portion, preferably 0.001-5
Weight portion.
Lubricant oil composite the most according to claim 1 and 2, wherein, described rubber particles
Mean diameter be 20-2000nm, preferably 50-1000nm, more preferably 70-500nm.
Lubricant oil composite the most according to claim 1 and 2, wherein, described rubber particles
Gel content be more than 60 weight %, more than preferably 75 weight %, more preferably 80 weight % with
On.
Lubricant oil composite the most according to claim 1 and 2, wherein, described rubber particles
There is equal phase structure.
Lubricant oil composite the most according to claim 1 and 2, wherein, described rubber particles
Selected from methyl silicone rubber particle, ethyl rubber particles, hydroxyl rubber particles, hydrogeneous methyl silicone rubber
Particle, hydrogeneous hydroxyl rubber particles, methyl vinyl silicone rubber particle, methyl vinyl phenyl silicon rubber
Micelle, methyl ethylene trifluoro propyl rubber particles, phenylene silicone rubber particle, phenylene ether base silicon
At least one in rubber particles, nitrile silicone rubber particle, silicon boron rubber particles and fluorosioloxane rubber particle.
Lubricant oil composite the most according to claim 1 and 2, wherein, described silicone oil base oil
For unmodified silicone oil and/or modified silicon oil；
Preferably, described unmodified silicone oil contains selected from methyl-silicone oil, ethyl silicon oil, phenyl silicone oil, methyl
Hydrogen silicone oil, methyl phenyl silicone oil, methylchlorophenyl silicone oil, MethylethoxylsiliconFluid Fluid, methyl trifluoro propyl
Silicone oil, methyl vinyl silicon oil, methylhydroxy silicone oil, ethyl containing hydrogen silicone oil, hydroxyl hydrogen silicone oil and contain
At least one in nitrile silicone；
Preferably, described modified silicon oil is selected from amino-modified silicone oil, epoxy-modified silicone oil, polyether-modified
Silicone oil, Carboxyl Modified Polydimethylsiloxane, alcoholic extract hydroxyl group modified silicon oil, phenolic group modified silicone oil, sulfhydryl modified silicone oil,
Polysiloxane-polyether block modification by copolymerization silicone oil, alkyl and polyether modified silicon oil, alkyl ether polyethers
Silicone oil, epoxy radicals polyether modified silicon oil, amino-polyether block silicone oil, glycerol ether silicone oil, the cruel base of phosphoric acid
At least one in silicone oil, glycosyl polyethers silicone oil and Radix Betae base silicone oil.
8. a preparation method for lubricant oil composite, the method includes silicone oil basis fat liquor with logical
Cross the rubber particles emulsion with cross-linked structure prepared by cross-linking radiation method carry out successively mixing, the most broken
Breast and redispersion, and relative to the silicone oil base oil in the described silicone oil basis fat liquor of 100 weight portions,
The consumption of the solid content of described rubber particles emulsion is 0.001-40 weight portion.
Method the most according to claim 8, wherein, described mixing, common breakdown of emulsion and redispersion
Mode includes:
(1) described rubber particles emulsion added in the fat liquor of described silicone oil basis and stirred by machinery
Mix mixing so that described rubber particles emulsion dispersion, in the fat liquor of described silicone oil basis, obtains preliminary
Scattered compositions；
(2) described preliminary scattered compositions is carried out common breakdown of emulsion, then remove moisture therein,
To breakdown of emulsion liquid；
(3) described breakdown of emulsion liquid is carried out redispersion, until the mean diameter of the rubber particles after Fen San
Reach in the range of 20-2000nm, preferably reach in the range of 50-1000nm, be more preferably up to
In the range of 70-500nm.
Method the most according to claim 9, wherein, the mode of described breakdown of emulsion altogether includes adding breakdown of emulsion
At least one in agent, centrifugation, heated and stirred, lyophilization and vacuum drying.
11. methods according to claim 9, wherein, described in be redispersed in homogenizer, bead grinds
Grinding machine, three-roll grinder, single screw extrusion machine, multi-screw extruder, kneader, dissolvers and ultrasonic
At least one mixing apparatus in ripple disperser is carried out, preferably at homogenizer, three-roll grinder and ultrasonic
At least one mixing apparatus in ripple disperser is carried out, more preferably carries out in homogenizer.
12. methods described in any one in-11 according to Claim 8, wherein, relative to 100 weights
Silicone oil base oil in the described silicone oil basis fat liquor of amount part, the solid content of described rubber particles emulsion
Consumption be 0.001-10 weight portion, preferably 0.001-5 weight portion.
13. methods described in any one in-11 according to Claim 8, wherein, described silicone oil basis
In fat liquor, the content of silicone oil base oil and the solid content of rubber particles emulsion are each independently 10 weights
Amount more than %, is preferably each independently more than 20 weight %, is more preferably each independently 30 weight
More than %.
14. methods described in any one in-11 according to Claim 8, wherein, described silicone rubber grain
In sub-emulsion, the mean diameter of rubber particles is 20-2000nm, preferably 50-1000nm, more preferably
For 70-500nm.
15. methods described in any one in-11 according to Claim 8, wherein, described silicone rubber grain
In sub-emulsion, the gel content of rubber particles is more than 60 weight %, more than preferably 75 weight %,
More than more preferably 80 weight %.
16. methods described in any one in-11 according to Claim 8, wherein, described silicone rubber grain
Rubber particles in sub-emulsion has equal phase structure.
17. methods described in any one in-11 according to Claim 8, wherein, described silicone rubber grain
Sub-emulsion is selected from selected from methyl silicone rubber particle emulsion, ethyl rubber particles emulsion, hydroxyl silicone rubber grain
Sub-emulsion, hydrogeneous methyl silicone rubber particle emulsion, hydrogeneous hydroxyl rubber particles emulsion, methyl ethylene
Rubber particles emulsion, methyl vinyl phenyl rubber particles emulsion, methyl ethylene trifluoro propyl silicon
Rubber particles emulsion, phenylene silicone rubber particle emulsion, phenylene ether base rubber particles emulsion, nitrile silicon rubber
At least one in the sub-emulsion of micelle, silicon boron rubber particles emulsion and fluorosioloxane rubber particle emulsion.
18. methods described in any one in-11 according to Claim 8, wherein, described silicone oil basis
Silicone oil base oil in fat liquor is unmodified silicone oil and/or modified silicon oil；
Preferably, described unmodified silicone oil contains selected from methyl-silicone oil, ethyl silicon oil, phenyl silicone oil, methyl
Hydrogen silicone oil, methyl phenyl silicone oil, methylchlorophenyl silicone oil, MethylethoxylsiliconFluid Fluid, methyl trifluoro propyl
Silicone oil, methyl vinyl silicon oil, methylhydroxy silicone oil, ethyl containing hydrogen silicone oil, hydroxyl hydrogen silicone oil and contain
At least one in nitrile silicone；
Preferably, described modified silicon oil is selected from amino-modified silicone oil, epoxy-modified silicone oil, polyether-modified
Silicone oil, Carboxyl Modified Polydimethylsiloxane, alcoholic extract hydroxyl group modified silicon oil, phenolic group modified silicone oil, sulfhydryl modified silicone oil,
Polysiloxane-polyether block modification by copolymerization silicone oil, alkyl and polyether modified silicon oil, alkyl ether polyethers
Silicone oil, epoxy radicals polyether modified silicon oil, amino-polyether block silicone oil, glycerol ether silicone oil, the cruel base of phosphoric acid
At least one in silicone oil, glycosyl polyethers silicone oil and Radix Betae base silicone oil.
19. lubricant oil composites prepared by the method described in any one in claim 8-18.
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