CN106147958B - 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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Abstract
The present invention relates to lubricating oil field, a kind of lubricant oil composite and preparation method thereof is specifically provided.The rubber particles with cross-linked structure prepared by cross-linking radiation method that the lubricant oil composite contains silicone oil base oil and is dispersed in the silicone oil base oil, the silicone oil base oil is continuous phase, the rubber particles are dispersed phase, and the silicone oil base oil relative to 100 parts by weight, the content of the rubber particles are 0.001-40 parts by weight.Lubricant oil composite provided by the invention can effectively adjust viscosity with the variation of temperature, compared with the lubricant oil composite containing the rubber particles by chemical crosslinking, viscosity is lower at low temperature, and viscosity is higher at high temperature, therefore, with good viscosity temperature characteristic.
Description
Technical field
It is prepared the present invention relates to a kind of lubricant oil composite, the preparation method of the lubricant oil composite and by this method
Obtained lubricant oil composite.
Background technique
The promotion each time of lubricating oil quality is nearly all the result that oil dope breaks through development.Nanoscale science and technology
As the new science and technology that phase late 1980s is born, the application in lubricating oil is more prominent, and nanometre metal powder is as new
Type solid lubricant reduces one of friction, the effective approach for reducing abrasion when having become lubrication.It is domestic at present that nanometer is added
The research of agent is still in the primary stage, this is primarily due to nano particle and is not easy or is difficult to be dissolved in oil, it is also difficult to steadily divide
It dissipates in lubricating oil.With people's deepening continuously to the research field of lubricating oil, discovery is and high with oleophylic by reducing partial size
After molecule modifies it, additive shows excellent performance in lubricating oil, hence it is evident that improves the friction of base oil
Performance is learned, there is good development and application prospect.
There is the report of the largely application about inorganic nano-particle in lubricating oil field in the prior art.For example,
CN1150958A discloses a kind of Low-density high temperature resistant wear-resistant self-lubricating nano particle filling enhancing polymer composite, by
Thermoplasticity heat-resistant polymer and nanoparticle composition, the nanoparticle includes nano-silicon nitride, nanometer silicon carbide and nanometer
Silica, the product have excellent self-lubricating property.CN1301319C discloses one kind and contains nano silicon dioxide particles
Lubricant oil composite, which is lubricating oil extreme pressure, the antiwear composite of a kind of function admirable, the technical solution
Use in a manner of base oil and nano silica and addition dispersing aid and synergist that realize nano silica micro-
The dispersion of grain.CN1180079A and CN1354056A individually discloses receiving through fatty acid modifying metallic oxide or hydroxide
The application of rice micro mist and warp containing the organic compound modified metal copper nano granules of thio phosphorus in lubricating oil field.
CN1827753A discloses a kind of fluorine-containing rare earth nano lubricating oil additive and preparation method thereof, the additive include base oil with
And the surface coated rare earth fluoride nanoparticle of itrogenous organic substance.CN101058760A disclose a kind of nano ceramic lubricating oil and
Preparation method, the ingredient containing traditional lubrication oil, and modified Nano ceramics are added on the basis of traditional lubrication oil
Grain belongs to the preparation field that mechanical movement lubricates oil medium, especially suitable for lubricating oil used in automobile industry and its
Preparation method.In the invention, the concentrate of the nano-ceramic particle of stable dispersion is successfully made by pre-dispersed method, in turn
Prepare the nano ceramics machine oil that nano-ceramic particle weight percentage is 0.00001%-5%.CN101235337B is disclosed
A kind of slipper or sliding component suitable for car combustion engine or power transmitting apparatus is to significantly reduce coefficient of friction
Lubricant oil composite, the lubricant oil composite contain lubricating oil base oil, oxygen-containing organic compound, diamond nano-particles and
Diamond nano-particles dispersing agent.CN101555430A discloses a kind of lubricant oil composite, containing oil base stock and receives
Rice carbon ball, the nano carbon microsphere surface grafting have alkyl, are scattered in it in oil base stock, and the nano carbon microsphere is hollow structure
Or it is filled with metal, metal alloy, metal oxide, metal carbides, metal sulfide, metal nitride or metal diboride
Object.
In addition, there are also the answering in lubricating oil field about organic fine particles gel other than inorganic nano-particle
Report.For example, Rhein Chemie Rheinau GmbH application patent CN1856527A, CN1840622A and
CN1861673A discloses the micro gel of a kind of micro gel in non-crosslinkable organic media and crosslinking for changing
The purposes of the temperature-independent performance of the non-crosslinked organic media of property.However, this several patents application is pointed out bar none, institute
State micro gel and be by the way of chemical crosslinking (for example, by with polyfunctional compound's crosslinking copolymerization or pass through peroxide
Compound crosslinking) micro gel that is prepared, rather than the micro gel being crosslinked with high-energy radiation.Above-mentioned patent application thinks high
The micro gel of energy crosslinking with radiation is actually unable in be prepared on an industrial scale, and the use of the high-energy radiation of radioactivity cobalt source is with tight
The safety problem of weight, the and when micro gel of crosslinking with radiation is used in plastic matrix, can be between matrix and dispersed phase
Tearing effect occurs, to compromise the mechanical performance of the plastics containing the micro gel, swelling behavior, stress corrosion cracking
Energy is equal.However, in patent CN1856527A, CN1840622A and CN1861673A of Rhein Chemie Rheinau GmbH's application
The viscosity temperature characteristic of disclosed lubricant oil composite is poor, and the viscosity of the lubricant oil composite can sharply increase with the reduction of temperature
Greatly, it can strongly reduce as the temperature rises, but viscosity is excessive at low temperature or viscosity is too small unfavorable at high temperature
With the application of lubricant oil composite, this will greatly limit the application of the lubricant oil composite.Therefore, it needs to develop
A kind of lubricant oil composite with preferable viscosity temperature characteristic.
Summary of the invention
The defect that the purpose of the invention is to overcome existing lubricant oil composite viscosity temperature characteristic poor, and one kind is provided
It the preparation method of lubricant oil composite, a kind of lubricant oil composite with excellent viscosity temperature characteristic and is prepared by this method
Lubricant oil composite.
The present inventor has found that Rhein Chemie Rheinau GmbH applies several above-mentioned after further investigation
Dispersed phase in lubricant oil composite disclosed in patent CN1856527A, CN1840622A and CN1861673A is using multifunctional
The micro gel that compound or peroxide are obtained by chemical crosslinking mode, although the lubricating oil composition containing the microgel particle
Object can reduce the coefficient of friction of organic media to a certain extent, but the viscosity of these lubricant oil composites is by the shadow of temperature
Sound is larger, and temperature too high (viscosity is too small) or too low (viscosity is too big) will limit the use of the lubricant oil composite, applicable for temperature
It is relatively narrow to spend range.And the rubber particles with cross-linked structure prepared by cross-linking radiation method with by using multiple functionalized
Closing the rubber particles with cross-linked structure that object or peroxide carry out chemical crosslinking preparation has entirely different microcosmic knot
Structure.When the dispersed phase in lubricant oil composite is the rubber particles with cross-linked structure prepared by cross-linking radiation method
When, corresponding lubricant oil composite has good viscosity temperature characteristic, viscosity very well can be adjusted with the variation of temperature,
It reduces low temperature viscosity and improves high temperature viscosity, therefore, can largely make up since the variation of temperature causes viscosity
Influence.In addition, high-energy radiation actually very cleaning, the safe and efficient energy, wide by many developed countries at present
It generally for fields such as health care, food processing, industrial productions, is existed using Chemical Crosslinking Methods (peroxide) instead
Some very important problems, such as the environmental pollution that production efficiency is not high, peroxide is remained and be may cause, these are all
It will limit its application.
Further, since the chemical structure of silicone oil base oil and rubber particles is almost the same, it is former according to structure similar compatibility
Reason, the two be it is fully compatible, rubber particles will significantly improve the boundary lubrication performance of silicone oil base oil, and further change
Kind viscosity temperature characteristic and antiwear and friction reduction property, this is for promoting the greasy property of silicone oil base oil, widening the application of silicone oil base oil
The equal important in inhibiting of range.
Based on above-mentioned discovery, the present inventor completes the present invention.
Specifically, the present invention provides a kind of lubricant oil composites, wherein the lubricant oil composite contains silicone oil basis
Oil and the rubber particles with cross-linked structure prepared by cross-linking radiation method being dispersed in the silicone oil base oil, institute
Stating silicone oil base oil is continuous phase, and the rubber particles are dispersed phase, and relative to the silicone oil of 100 parts by weight basis
Oil, the content of the rubber particles are 0.001-40 parts by weight.
The present invention also provides a kind of preparation method of lubricant oil composite, this method include by silicone oil basis fat liquor with
It successively mixed, be demulsified altogether and divided again by the rubber particles lotion with cross-linked structure prepared by cross-linking radiation method
It dissipates, and relative to the silicone oil base oil in the silicone oil basis fat liquor of 100 parts by weight, the rubber particles lotion is consolidated
The dosage of content is 0.001-40 parts by weight.
In addition, the present invention also provides lubricant oil composites prepared by the above method.
Lubricant oil composite provided by the invention can effectively adjust viscosity with the variation of temperature, with contain passing through
The lubricant oil composite for learning the rubber particles of crosslinking is compared, and viscosity is lower under low temperature (40 DEG C), and at high temperature (100 DEG C)
Lower viscosity is higher, can satisfy the requirement that temperature reaches 200 DEG C or more occasions, therefore, has significantly widened the lubricating oil group
Close the use temperature range of object.
In addition, lubricant oil composite provided by the invention can be used for blends engine oil, gear oil, hydraulic oil etc., other are high
Temperature industrial oil, be particularly applied to the field such as engine oil more demanding to viscosity temperature characteristic, be suitable for adjust viscosity temperature characteristic compared with
Difference using double ring arene, polycyclic aromatic hydrocarbon and non-hydrocarbons base oil as the viscosity temperature characteristic of the lubricating composition of main component, can be with
According to the demand in different operating place, easy adjustment provides the lubricating oil of different viscosity temperature characteristics.
Other features and advantages of the present invention will the following detailed description will be given in the detailed implementation section.
Specific embodiment
Detailed description of the preferred embodiments below.It should be understood that described herein specific
Embodiment is merely to illustrate and explain the present invention, and is not intended to restrict the invention.
Lubricant oil composite provided by the invention contains silicone oil base oil and is dispersed in passing through in the silicone oil base oil
The rubber particles with cross-linked structure of cross-linking radiation method preparation, the silicone oil base oil are continuous phase, the silicon rubber
Particle is dispersed phase, and the silicone oil base oil relative to 100 parts by weight, and the content of the rubber particles is 0.001-40
Parts by weight.Wherein, the rubber particles are in stable dispersion state in silicone oil base oil.
The lubricant oil composite provided according to the present invention, as discussed previously with respect to the silicone oil basis of 100 parts by weight
Oil, the content of the rubber particles are 0.001-40 parts by weight.But in order to enable silicone oil base oil and rubber particles play
Better coordinated effect, and so that the lubricant oil composite arrived has better viscosity temperature characteristic, it is preferable that relative to
The silicone oil base oil of 100 parts by weight, the content of the rubber particles are 0.001-10 parts by weight, more preferably 0.001-
5 parts by weight.
The lubricant oil composite provided according to the present invention, it is preferable that the average grain diameter of the rubber particles is 20-
2000nm, more preferably 50-1000nm, particularly preferably 70-500nm.It is controlled when by the average grain diameter of the rubber particles
When within the above range, the viscosity of lubricant oil composite can be more effectively adjusted, there is better temperature pumping and mobility
Can, be conducive to the cold start-up of mechanical equipment, and be also beneficial to form thicker oil film at high temperature, reduce mantle friction, that is, can
Adapt to broader use temperature range.
The lubricant oil composite provided according to the present invention, it is preferable that the gel content of the rubber particles is 60 weights
Measure % or more, more preferably 75 weight % or more, particularly preferably 80 weight % or more.When by the gel of the rubber particles
When content is controlled within the above range, the viscosity of lubricant oil composite can be more effectively adjusted with the variation of temperature, can be fitted
Answer broader use temperature range.In the present invention, the gel content is this field for characterizing the one of rubber cross degree
Kind Common Parameters, measure according to method disclosed in CN1402752A.
The present invention is not particularly limited the type of the rubber particles, for example, methyl silicone rubber grain can be selected from
Sub (including dimethyl silicone rubber particle), hydroxyl rubber particles, hydrogeneous methyl silicone rubber particle, contains ethyl rubber particles
Hydrogen hydroxyl rubber particles, methyl vinyl silicone rubber particle, methyl vinyl phenyl rubber particles, methyl ethylene trifluoro
Propyl rubber particles, phenylene silicone rubber particle, phenylene ether base rubber particles, nitrile silicone rubber particle, silicon boron rubber particles
At least one of with fluorine silicone rubber particle.
In addition, rubber particles provided by the invention preferably have equal phase structure.In the present invention, described " equal phase structure "
Refer to and observe under existing microtechnic do not have to find the not homogeneous phenomenons such as layering, split-phase in rubber particles.
The lubricant oil composite provided according to the present invention, high-energy ray source used in the cross-linking radiation can be specifically selected from
At least one of cobalt source, ultraviolet, high-energy electron accelerator, it is preferable that the wavelength in the high-energy ray source is less than 0.1 μm, example
For example cobalt source.In addition, under normal circumstances, the dosage of irradiation should make the gel of the rubber particles after rubber latex cross-linking radiation
Content reaches 60 weight % or more, preferably reaches 75 weight % or more, more preferably up to 80 weight % or more.Specifically, it irradiates
Dosage can be 0.1-30Mrad, preferably 0.5-20Mrad.
The present invention is not particularly limited the type of the silicone oil base oil, can be unmodified silicone oil, or
Unmodified silicone oil can also be the mixture of modified silicon oil and unmodified silicone oil.
Specifically, the example of the unmodified silicone oil includes but is not limited to: methyl-silicone oil, ethyl silicon oil, phenyl silicone oil, first
Base containing hydrogen silicone oil, methyl phenyl silicone oil, methylchlorophenyl silicone oil, MethylethoxylsiliconFluid Fluid, methyl trifluoro propyl silicone oil, methyl second
Alkenyl silicone oil, methylhydroxy silicone oil, ethyl containing hydrogen silicone oil, hydroxyl hydrogen silicone oil and at least one of containing nitrile silicone, preferably
Methyl-silicone oil.
The unmodified silicone oil refers to be changed using obtained from the part methyl group in certain modified groups substitution silicone oil
Property silicone oil, modified silicon oil are not only a kind of extraordinary silicone oil with common dimethicone speciality, and according to the difference of importing
Modified group, silicone oil are endowed a variety of new characteristics, such as water-soluble, compatibility or with the reactivity of various other materials, coating
Property etc..The example of the modified silicon oil includes but is 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-polyether block
Modification by copolymerization silicone oil, alkyl and polyether modified silicon oil, alkyl ether polyether silicone oil, epoxy group polyether modified silicon oil, amino-polyether are embedding
At least one of section silicone oil, glycerol ether silicone oil, the cruel base silicone oil of phosphoric acid, glycosyl polyethers silicone oil and beet base silicone oil.
In addition, lubricant oil composite provided by the invention can also contain common additive.The type of the additive
Including but not limited to: anti-aging agent, antiwear additive, antilubricant, antioxidant, anti-foaming agent, antirust agent, detersive, dispersing agent, pigment, pole
Press at least one of composition, friction protection composition, detersive, coupling agent etc..The dosage of the additive can be this
The conventional selection in field can know that therefore not to repeat here to this those skilled in the art.
The preparation method of lubricant oil composite provided by the invention includes by silicone oil basis fat liquor and passing through cross-linking radiation
The rubber particles lotion with cross-linked structure of method preparation successively mixed, is demulsified altogether and redisperse, and relative to 100
Silicone oil base oil in the silicone oil basis fat liquor of parts by weight, the dosage of the solid content of the rubber particles lotion are
0.001-40 parts by weight.
The preparation method of the lubricant oil composite provided according to the present invention, as discussed previously with respect to described in 100 parts by weight
Silicone oil base oil in the fat liquor of silicone oil basis, the dosage of the solid content of the rubber particles lotion are 0.001-40 weight
Part.But in order to enable silicone oil base oil and rubber particles play the role of better coordinated, and so that the lubrication arrived
Fluid composition has better viscosity temperature characteristic, it is preferable that relative to the silicone oil in the silicone oil basis fat liquor of 100 parts by weight
Base oil, the dosage of the solid content of the rubber particles lotion are 0.001-10 parts by weight, more preferably 0.001-5 weight
Part.
The preparation method of the lubricant oil composite provided according to the present invention, silicone oil base oil in the fat liquor of the silicone oil basis
Content and the solid content of rubber particles lotion can be each independently 10 weight % or more, be preferably each independently 20
Weight % or more is more preferably each independently 30 weight % or more.
The preparation method of the lubricant oil composite provided according to the present invention, it is preferable that silicon in the rubber particles lotion
The average grain diameter of rubber particles is 20-2000nm, more preferably 50-1000nm, particularly preferably 70-500nm.
The preparation method of the lubricant oil composite provided according to the present invention, it is preferable that silicon in the rubber particles lotion
The gel content of rubber particles is 60 weight % or more, more preferably 75 weight % or more, particularly preferably 80 weight % or more.
It, can be with temperature when by the gel content control of rubber particles in the rubber particles lotion within the above range
Variation more effectively adjusts the viscosity of lubricant oil composite, is suitable for broader use temperature range.
Rubber particles in the rubber particles lotion preferably have equal phase structure.In the present invention, described " homogeneous
Structure " refers to be observed under existing microtechnic, in the rubber particles in rubber particles lotion no without discovery layering, split-phase etc.
Homogeneous phenomenon.
Rubber particles lotion provided by the invention is prepared by silicon rubber lotion by cross-linking radiation.In the silicon rubber
In the preparation process of the sub- lotion of micelle, high-energy ray source used in cross-linking radiation can specifically be selected from cobalt source, ultraviolet, high energy electron
At least one of accelerator, it is preferable that the wavelength in the high-energy ray source is less than 0.1 μm, for example, cobalt source.In addition, general
In the case of, the dosage of irradiation should make the gel content of the rubber particles after rubber latex cross-linking radiation reach 60 weight % with
On, preferably reach 75 weight % or more, more preferably up to 80 weight % or more.Specifically, the dosage of irradiation can be 0.1-
30Mrad, preferably 0.5-20Mrad.
The rubber particles lotion can be commercially available, can also be according to various methods well known to art technology
It is prepared.For example, the rubber particles lotion can applicant according to the invention submitted on September 18th, 2000
International patent application WO01/40356 (priority date on December 3rd, 1999) and applicant of the present invention were June 15 in 2001
The international patent application WO01/98395 (priority date on June 15th, 2000) that day submits prepares selected when fully vulcanized powder rubber
Lotion carries out cross-linking radiation and obtains.In addition, the example of the rubber particles lotion includes but is not limited to: methyl silicone rubber
It is particle lotion (including dimethyl silicone rubber particle lotion), ethyl rubber particles lotion, hydroxyl rubber particles lotion, hydrogeneous
Methyl silicone rubber particle lotion, hydrogeneous hydroxyl rubber particles lotion, methyl vinyl silicone rubber particle lotion, methyl ethylene
Phenyl siloxane rubber particle lotion, methyl ethylene trifluoro propyl rubber particles lotion, phenylene silicone rubber particle lotion, sub- benzene
In ether rubber particles lotion, nitrile silicone rubber particle lotion, silicon boron rubber particles lotion and fluorine silicone rubber particle lotion extremely
Few one kind.The gel content of rubber particles is preferably 60 weight % or more in the rubber particles lotion, and more preferably 75
Weight % or more, particularly preferably 80 weight % or more.The average grain diameter of rubber particles is excellent in the rubber particles lotion
It is selected as 20-2000nm, more preferably 50-1000nm, particularly preferably 70-500nm.In addition, in the rubber particles lotion
Each rubber particle be it is homogeneous, i.e., under existing microscopy in particle without discovery layering, split-phase etc. no
Homogeneous phenomenon.
In addition, cross-linking aid can not be used in the cross-linking radiation preparation process of the rubber particles lotion, it can also
To use cross-linking aid.The cross-linking aid can be selected from simple function group cross-linking aid, two functional group's cross-linking aids, trifunctional
Any one in cross-linking aid, the above cross-linking aid of four-functional group cross-linking aid and five functional groups.The simple function group crosslinking
The example of auxiliary agent includes but is not limited to: (methyl) 2-ethyl hexyl acrylate, (methyl) Isooctyl acrylate monomer, (methyl) acrylic acid shrink sweet
At least one of grease；The example of two functional group cross-linking aid includes but is not limited to: 1,4- butanediol two (methyl) third
Olefin(e) acid ester, 1,6-hexylene glycols two (methyl) acrylate, diethylene glycol two (methyl) acrylate, triethylene glycol two (methyl) third
At least one of olefin(e) acid ester, neopentyl glycol two (methyl) acrylate, divinylbenzene；The trifunctional cross-linking aid
Example includes but is not limited to: trimethylolpropane tris (methyl) acrylate and/or pentaerythrite three (methyl) acrylate；Institute
The example for stating four-functional group cross-linking aid includes but is not limited to: pentaerythrite four (methyl) acrylate and/or ethoxyquin season penta
Tetrol four (methyl) acrylate；The example of the above cross-linking aid of five functional groups includes but is not limited to: dipentaerythritol five
(methyl) acrylate.Herein, described (methyl) acrylate refers to acrylate or methacrylate.These crosslinkings
Auxiliary agent can be applied in combination in any way, as long as they facilitate crosslinking under irradiation.In addition, the cross-linking aid
Additional amount is generally the 0.1-10 weight % of dry glue weight in latex, preferably 0.5-9 weight %, more preferably 0.7-7 weight
Measure %.
In addition, the preparation method of lubricant oil composite provided by the invention can also include by additive and silicone oil base oil
Lotion and rubber particles lotion are mixed together.
The type of silicone oil base oil and additive in the fat liquor of the silicone oil basis has been described herein above,
Therefore not to repeat here.
A kind of specific embodiment according to the present invention, silicone oil basis fat liquor into silicone oil base oil by being added
Then emulsifier is emulsified using emulsifying device and is obtained.Wherein, the type of the emulsifier can be the routine of this field
Selection, for example, existing various nonionic surfactants, cationic surfactant, anion surface active can be selected from
In agent, amphoteric surfactant, polyacrylamide amine emulsifier, esters non-ionic additive and the closed non-ionic additive of terminal hydroxy group
At least one is specifically known to the skilled person, and therefore not to repeat here.In addition, the emulsifying device can be selected from emulsification
At least one of blender, colloid mill and homogenizer.
The present invention is demulsified to the mixing, altogether and the mode of redisperse is not particularly limited, as long as enabling to silicon rubber
Micelle is effectively dispersed in silicone oil base oil, to obtain using silicone oil base oil as continuous phase and with rubber particles being
The lubricant oil composite of dispersed phase.A preferred embodiment of the invention, the mixing, altogether demulsification and redisperse
Mode include: (1) will the rubber particles lotion be added silicone oil basis fat liquor in and by mechanical stirring mixing,
So that the composition that the rubber particles emulsion dispersion in the fat liquor of the silicone oil basis, is tentatively dispersed；(2) by institute
It states the composition tentatively dispersed and carries out total demulsification, then remove moisture therein, obtain demulsification liquid；(3) by the demulsification liquid into
Row redisperse, until the average grain diameter of the rubber particles after dispersion reach 20-2000nm in the range of, preferably reach 50-
In the range of 1000nm, in the range of more preferably up to 70-500nm.Pass through this preferred mixing, altogether demulsification and redisperse
Mode enables to rubber particles to be dispersed in silicone oil base oil with initial size, the viscous warm nature of obtained lubricant oil composite
It can be more preferably.
The mixing of mechanical stirring described in step (1) can carry out in existing various mechanical mixing equipments, for example, can
To be carried out in the mechanical mixing equipments such as high-speed mixer, kneader.The present invention does not have the condition that the mechanical stirring mixes yet
Have and particularly limit, as long as making the rubber particles lotion and silicone oil with cross-linked structure prepared by cross-linking radiation method
Under the premise of the performance of basic fat liquor does not have any variation, make the silicon with cross-linked structure prepared by cross-linking radiation method
Rubber particles emulsion dispersion is suspended in the fat liquor of silicone oil basis, can be known to this those skilled in the art, herein
It does not repeat.
The present invention is not particularly limited the mode being demulsified altogether in step (2), for example, can using plus demulsifier, from
At least one of heart separation, heating stirring, freeze-drying and vacuum drying carry out total demulsification.
Redisperse described in step (3) can homogenizer, bead mill, three-roll grinder, single screw extrusion machine,
It carries out at least one of multi-screw extruder, kneader, dissolvers and ultrasonic disperser mixing apparatus, is preferably being homogenized
It is carried out in device, three-roll grinder and ultrasonic disperser, these three preferred mixing apparatus have processing output height, mixed effect
The fairly simple advantage of good, subsequent cleaning.Most preferably, it is redispersed in homogenizer and carries out described in step (3).Dispersing
In the process, it according to different dispersion quality requirements, needs cycles samples cooling, then iterate through mixing apparatus and repeatedly divided
It dissipates, until the average grain diameter for the rubber particles being dispersed in silicone oil base oil reaches within the scope of 20-2000nm, preferably reaches
Within the scope of 50-1000nm, within the scope of more preferably up to 70-500nm.In addition, the present invention is to the condition of the redisperse without spy
It does not limit, as long as destroying silicone oil base oil and the rubber particles performance in dispersion process not, and makes silicon rubber
The partial size of micelle reaches 20-2000nm, preferably reaches 50-1000nm, more preferably up to 70-500nm, to this this field
Technical staff can know that therefore not to repeat here.
The present invention also provides lubricant oil composites prepared by the above method.
The present invention will be described in detail by way of examples below.
(1) raw material used in embodiment and comparative example is as follows:
Simethicone emulsion, Beijing sea cowry think company's production, and dimethyl-silicon oil content is 35 weight %, and viscosity is
350cp (1cp=1mPa.s).
Simethicone emulsion, Beijing sea cowry think company's production, and dimethyl-silicon oil content is 35 weight %, and viscosity is
500cp。
Dimethyl silicone rubber lotion, Sinopec production, trade mark vp-661, solid content are 35 weight %, gel content
For 88 weight %, wherein the average grain diameter of silicon rubber is 100nm, is observed under the microscope, in the dimethyl silicone rubber lotion
Without discovery layering, noted phase separation phenomena in dimethyl silicone rubber particle.The dimethyl silicone rubber lotion is by past 1kg dimethyl-silicon
Rubber latex adds 15g trimethylolpropane trimethacrylate, stirs 1 hour and is uniformly mixed, irradiates to obtain by cobalt source later,
Irradiation dose 20Mrad.
Peroxide crosslinking dimethyl silicone rubber lotion is prepared according to method disclosed in patent CN1840622A,
Rubber latex be dimethyl silicone rubber latex (with prepare dimethyl silicone rubber glue used by dimethyl silicone rubber lotion vp-661
Cream is identical), the crosslinking agent used is cumyl peroxide (DCP), the peroxide crosslinking dimethyl silicone rubber finally obtained
The average grain diameter 100nm of dimethyl silicone rubber particle in particle lotion, solid content are 35 weight %, and gel content is 88 weights
Measure %.
(2) viscosity of the lubricant oil composite in following embodiment and comparative example: HAAKE RheoStress is used
RS300 rheometer (subsidiary TC501 temperature control device), C60/1 ° of Ti module are measured, test respectively 40 DEG C, 60 DEG C, 80 DEG C,
Viscosity at 100 DEG C.
Embodiment 1
The embodiment is for illustrating lubricant oil composite provided by the invention and preparation method thereof.
The simethicone emulsion of 100 parts by weight 350cp and 1 parts by weight dimethyl silicone rubber lotion vp-661 are mixed simultaneously
Progress mechanical stirring is uniform, then at oil bath high speed stirring (mixing speed 10000rpm/min, similarly hereinafter) 6 hours of 95 DEG C
Total demulsification is carried out, water therein is then removed, obtains demulsification liquid.Above-mentioned demulsification liquid is homogenized circulation three in high pressure homogenizer
Secondary, homogenization pressure is 100MPa, obtains lubricant oil composite, and viscosity is shown in Table 1.
Embodiment 2
The embodiment is for illustrating lubricant oil composite provided by the invention and preparation method thereof.
The simethicone emulsion of 100 parts by weight 350cp and 3 parts by weight dimethyl silicone rubber lotion vp-661 are mixed simultaneously
Progress mechanical stirring is uniform, and then the oil bath high speed stirring at 95 DEG C carries out total demulsification for 6 hours, then removes water therein,
Obtain demulsification liquid.Above-mentioned demulsification liquid is homogenized circulation three times in high pressure homogenizer, homogenization pressure is 100MPa, is lubricated
Fluid composition, viscosity are shown in Table 1.
Embodiment 3
The embodiment is for illustrating lubricant oil composite provided by the invention and preparation method thereof.
The simethicone emulsion of 100 parts by weight 350cp and 5 parts by weight dimethyl silicone rubber lotion vp-661 are mixed simultaneously
Progress mechanical stirring is uniform, and then the oil bath high speed stirring at 95 DEG C carries out total demulsification for 6 hours, then removes water therein,
Obtain demulsification liquid.Above-mentioned demulsification liquid is homogenized circulation three times in high pressure homogenizer, homogenization pressure is 100MPa, is lubricated
Fluid composition, viscosity are shown in Table 1.
Embodiment 4
The embodiment is for illustrating lubricant oil composite provided by the invention and preparation method thereof.
The simethicone emulsion of 100 parts by weight 350cp and 7.5 parts by weight dimethyl silicone rubber lotion vp-661 are mixed
And carry out that mechanical stirring is uniform, it is then stirred in 95 DEG C of oil bath high speed and carries out within 6 hours total demulsification, then removed therein
Water obtains demulsification liquid.Above-mentioned demulsification liquid is homogenized circulation three times in high pressure homogenizer, homogenization pressure is 100MPa, is obtained
Lubricant oil composite, viscosity are shown in Table 1.
Embodiment 5
The embodiment is for illustrating lubricant oil composite provided by the invention and preparation method thereof.
The simethicone emulsion of 100 parts by weight 350cp and 10 parts by weight dimethyl silicone rubber lotion vp-661 are mixed
And carry out that mechanical stirring is uniform, it is then stirred in 95 DEG C of oil bath high speed and carries out within 6 hours total demulsification, then removed therein
Water obtains demulsification liquid.Above-mentioned demulsification liquid is homogenized circulation three times in high pressure homogenizer, homogenization pressure is 100MPa, is obtained
Lubricant oil composite, viscosity are shown in Table 1.
Embodiment 6
The embodiment is for illustrating lubricant oil composite provided by the invention and preparation method thereof.
The simethicone emulsion of 100 parts by weight 500cp and 1 parts by weight dimethyl silicone rubber lotion vp-661 are mixed simultaneously
Progress mechanical stirring is uniform, and then the oil bath high speed stirring at 95 DEG C carries out total demulsification for 6 hours, then removes water therein,
Obtain demulsification liquid.Above-mentioned demulsification liquid is homogenized circulation three times in high pressure homogenizer, homogenization pressure is 100MPa, is lubricated
Fluid composition, viscosity are shown in Table 2.
Embodiment 7
The embodiment is for illustrating lubricant oil composite provided by the invention and preparation method thereof.
The simethicone emulsion of 100 parts by weight 500cp and 3 parts by weight dimethyl silicone rubber lotion vp-661 are mixed simultaneously
Progress mechanical stirring is uniform, and then the oil bath high speed stirring at 95 DEG C carries out total demulsification for 6 hours, then removes water therein,
Obtain demulsification liquid.Above-mentioned demulsification liquid is homogenized circulation three times in high pressure homogenizer, homogenization pressure is 100MPa, is lubricated
Fluid composition, viscosity are shown in Table 2.
Embodiment 8
The embodiment is for illustrating lubricant oil composite provided by the invention and preparation method thereof.
The simethicone emulsion of 100 parts by weight 500cp and 5 parts by weight dimethyl silicone rubber lotion vp-661 are mixed simultaneously
Progress mechanical stirring is uniform, and then the oil bath high speed stirring at 95 DEG C carries out total demulsification for 6 hours, then removes water therein,
Obtain demulsification liquid.Above-mentioned demulsification liquid is homogenized circulation three times in high pressure homogenizer, homogenization pressure is 100MPa, is lubricated
Fluid composition, viscosity are shown in Table 2.
Comparative example 1
The comparative example is for illustrating lubricant oil composite of reference and preparation method thereof.
Lubricant oil composite is prepared according to the method for embodiment 8, unlike, by 5 parts by weight dimethyl silicone rubber lotions
The peroxide crosslinking dimethyl silicone rubber lotion of 5 parts by weight of vp-661 substitutes, and obtains reference lube composition, viscosity
It is shown in Table 2.
Embodiment 9
The embodiment is for illustrating lubricant oil composite provided by the invention and preparation method thereof.
The simethicone emulsion of 100 parts by weight 500cp and 7.5 parts by weight dimethyl silicone rubber lotion vp-661 are mixed
And carry out that mechanical stirring is uniform, it is then stirred in 95 DEG C of oil bath high speed and carries out within 6 hours total demulsification, then removed therein
Water obtains demulsification liquid.Above-mentioned demulsification liquid is homogenized circulation three times in high pressure homogenizer, homogenization pressure is 100MPa, is obtained
Lubricant oil composite, viscosity are shown in Table 2.
Embodiment 10
The embodiment is for illustrating lubricant oil composite provided by the invention and preparation method thereof.
The simethicone emulsion of 100 parts by weight 500cp and 10 parts by weight dimethyl silicone rubber lotion vp-661 are mixed
And carry out that mechanical stirring is uniform, it is then stirred in 95 DEG C of oil bath high speed and carries out within 6 hours total demulsification, then removed therein
Water obtains demulsification liquid.Above-mentioned demulsification liquid is homogenized circulation three times in high pressure homogenizer, homogenization pressure is 100MPa, is obtained
Lubricant oil composite, viscosity are shown in Table 2.
Table 1
Table 2
It can be seen that from the comparison of embodiment 8 and comparative example 1 and contain the Si powder rubber obtained by peroxide crosslinking
The lubricant oil composite of micelle is compared, and the Si powder rubber granule with cross-linked structure obtained by cross-linking radiation method is contained
The lubricant oil composite of son in low temperature (40 DEG C) viscosity is lower, and (100 DEG C) viscosity is higher at high temperature, therefore, the present invention
The lubricant oil composite of offer has better viscosity temperature characteristic, to have better temperature pumping and mobile performance, is conducive to
The cold start-up of mechanical equipment, and be also beneficial to form thicker oil film at high temperature, mantle friction is reduced, lubricant effect is improved,
It is suitable for broader temperature use scope simultaneously, and friction can be reduced, energy-saving effect is more preferably.
The preferred embodiment of the present invention has been described above in detail, still, during present invention is not limited to the embodiments described above
Detail within the scope of the technical concept of the present invention can be with various simple variants of the technical solution of the present invention are made, this
A little simple variants all belong to the scope of protection of the present invention.
It is further to note that specific technical features described in the above specific embodiments, in not lance
In the case where shield, it can be combined in any appropriate way.In order to avoid unnecessary repetition, the present invention to it is various can
No further explanation will be given for the combination of energy.
In addition, various embodiments of the present invention can be combined randomly, as long as it is without prejudice to originally
The thought of invention, it should also be regarded as the disclosure of the present invention.
Claims (35)
1. a kind of lubricant oil composite, which is characterized in that the lubricant oil composite contains silicone oil base oil and is dispersed in described
The rubber particles with cross-linked structure prepared by cross-linking radiation method in silicone oil base oil, the silicone oil base oil are
Continuous phase, the rubber particles are dispersed phase, and the silicone oil base oil relative to 100 parts by weight, the silicon rubber grain
The content of son is 0.001-40 parts by weight, wherein the average grain diameter of the rubber particles is 20-2000nm, the silicon rubber
The gel content of particle is 60 weight % or more.
2. lubricant oil composite according to claim 1, wherein relative to the silicone oil base oil of 100 parts by weight, institute
The content for stating rubber particles is 0.001-10 parts by weight.
3. lubricant oil composite according to claim 2, wherein relative to the silicone oil base oil of 100 parts by weight, institute
The content for stating rubber particles is 0.001-5 parts by weight.
4. lubricant oil composite according to claim 1, wherein the average grain diameter of the rubber particles is 50-
1000nm。
5. lubricant oil composite according to claim 4, wherein the average grain diameter of the rubber particles is 70-
500nm。
6. lubricant oil composite according to claim 1, wherein the gel content of the rubber particles is 75 weight %
More than.
7. lubricant oil composite according to claim 6, wherein the gel content of the rubber particles is 80 weight %
More than.
8. lubricant oil composite described in any one of -3 according to claim 1, wherein the rubber particles have homogeneous
Structure.
9. lubricant oil composite described in any one of -3 according to claim 1, wherein the rubber particles are selected from methyl
Rubber particles, ethyl rubber particles, hydroxyl rubber particles, hydrogeneous methyl silicone rubber particle, hydrogeneous hydroxyl silicon rubber grain
Son, methyl vinyl silicone rubber particle, methyl vinyl phenyl rubber particles, methyl ethylene trifluoro propyl silicon rubber grain
Son, phenylene silicone rubber particle, phenylene ether base rubber particles, nitrile silicone rubber particle, silicon boron rubber particles and fluorine silicone rubber grain
At least one of son.
10. lubricant oil composite described in any one of -3 according to claim 1, wherein the silicone oil base oil is not change
Property silicone oil and/or modified silicon oil.
11. lubricant oil composite according to claim 10, wherein the unmodified silicone oil is selected from methyl-silicone oil, ethyl
Silicone oil, phenyl silicone oil, Methyl Hydrogen Polysiloxane Fluid, methyl phenyl silicone oil, methylchlorophenyl silicone oil, MethylethoxylsiliconFluid Fluid, methyl three
Fluoropropyl silicone oil, methyl vinyl silicon oil, methylhydroxy silicone oil, ethyl containing hydrogen silicone oil, hydroxyl hydrogen silicone oil and containing in nitrile silicone
At least one.
12. lubricant oil composite according to claim 10, wherein the modified silicon oil is selected from amino-modified silicone oil, ring
It is oxygroup modified silicon 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-polyether block modification by copolymerization silicone oil, alkyl and polyether modified silicon oil, alkyl ether polyether silicone oil, epoxy
Base polyether modified silicon oil, amino-polyether block silicone oil, glycerol ether silicone oil, the cruel base silicone oil of phosphoric acid, glycosyl polyethers silicone oil and beet
At least one of base silicone oil.
13. a kind of preparation method of lubricant oil composite, this method includes by silicone oil basis fat liquor and by cross-linking radiation side
The rubber particles lotion with cross-linked structure of method preparation successively mixed, is demulsified altogether and redisperse, and relative to 100 weights
The silicone oil base oil in the silicone oil basis fat liquor of part is measured, the dosage of the solid content of the rubber particles lotion is
0.001-40 parts by weight, wherein the average grain diameter of rubber particles is 20-2000nm in the rubber particles lotion, described
The gel content of rubber particles is 60 weight % or more in rubber particles lotion.
14. according to the method for claim 13, wherein the mixing, the mode of demulsification and redisperse includes: altogether
(1) the rubber particles lotion is added in the fat liquor of the silicone oil basis and is mixed by mechanical stirring, so that institute
Rubber particles emulsion dispersion is stated in the fat liquor of the silicone oil basis, the composition tentatively dispersed；
(2) composition tentatively dispersed is subjected to total demulsification, then removes moisture therein, obtain demulsification liquid；
(3) the demulsification liquid is subjected to redisperse, until the average grain diameter of the rubber particles after dispersion reaches 20-2000nm's
In range.
15. according to the method for claim 14, wherein the demulsification liquid is carried out redisperse, until the silicon rubber after dispersion
The average grain diameter of micelle reaches in the range of 50-1000nm.
16. according to the method for claim 15, wherein the demulsification liquid is carried out redisperse, until the silicon rubber after dispersion
The average grain diameter of micelle reaches in the range of 70-500nm.
17. according to the method for claim 14, wherein the mode being demulsified altogether includes adding demulsifier, centrifuge separation, adding
At least one of thermal agitation, freeze-drying and vacuum drying.
18. according to the method for claim 14, wherein described to be redispersed in homogenizer, bead mill, the grinding of three rollers
At least one of machine, single screw extrusion machine, multi-screw extruder, kneader, dissolvers and ultrasonic disperser mixing apparatus
Middle progress.
19. according to the method for claim 18, wherein described to be redispersed in homogenizer, three-roll grinder and ultrasonic wavelength-division
It dissipates and is carried out at least one of device mixing apparatus.
20. according to the method for claim 19, wherein described be redispersed in homogenizer carries out.
21. method described in any one of 3-20 according to claim 1, wherein the Silicon-oil-based relative to 100 parts by weight
Silicone oil base oil in plinth fat liquor, the dosage of the solid content of the rubber particles lotion are 0.001-10 parts by weight.
22. according to the method for claim 21, wherein relative in the silicone oil basis fat liquor of 100 parts by weight
Silicone oil base oil, the dosage of the solid content of the rubber particles lotion are 0.001-5 parts by weight.
23. method described in any one of 3-20 according to claim 1, wherein Silicon-oil-based in the fat liquor of the silicone oil basis
The content of plinth oil and the solid content of rubber particles lotion are each independently 10 weight % or more.
24. according to the method for claim 23, wherein the content and silicon of silicone oil base oil in the fat liquor of the silicone oil basis
The solid content of rubber particles lotion is each independently 20 weight % or more.
25. according to the method for claim 24, wherein the content and silicon of silicone oil base oil in the fat liquor of the silicone oil basis
The solid content of rubber particles lotion is each independently 30 weight % or more.
26. according to the method for claim 13, wherein the average grain diameter of rubber particles in the rubber particles lotion
For 50-1000nm.
27. according to the method for claim 26, wherein the average grain diameter of rubber particles in the rubber particles lotion
For 70-500nm.
28. according to the method for claim 13, wherein the gel content of rubber particles in the rubber particles lotion
For 75 weight % or more.
29. according to the method for claim 28, wherein the gel content of rubber particles in the rubber particles lotion
For 80 weight % or more.
30. method described in any one of 3-20 according to claim 1, wherein the silicon rubber in the rubber particles lotion
Micelle has equal phase structure.
31. method described in any one of 3-20 according to claim 1, wherein the rubber particles lotion is selected from methyl
Rubber particles lotion, ethyl rubber particles lotion, hydroxyl rubber particles lotion, hydrogeneous methyl silicone rubber particle lotion,
Hydrogeneous hydroxyl rubber particles lotion, methyl vinyl silicone rubber particle lotion, methyl vinyl phenyl rubber particles lotion,
Methyl ethylene trifluoro propyl rubber particles lotion, phenylene silicone rubber particle lotion, phenylene ether base rubber particles lotion,
At least one of nitrile silicone rubber particle lotion, silicon boron rubber particles lotion and fluorine silicone rubber particle lotion.
32. method described in any one of 3-20 according to claim 1, wherein the silicone oil in the fat liquor of the silicone oil basis
Base oil is unmodified silicone oil and/or modified silicon oil.
33. according to the method for claim 32, wherein the unmodified silicone oil is selected from methyl-silicone oil, ethyl silicon oil, phenyl
Silicone oil, Methyl Hydrogen Polysiloxane Fluid, methyl phenyl silicone oil, methylchlorophenyl silicone oil, MethylethoxylsiliconFluid Fluid, methyl trifluoro propyl silicon
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
Kind.
34. according to the method for claim 32, wherein the modified silicon oil is selected from amino-modified silicone oil, epoxy-modified
Silicone oil, Carboxyl Modified Polydimethylsiloxane, alcoholic extract hydroxyl group modified silicon oil, phenolic group modified silicone oil, sulfhydryl modified silicone oil, gathers polyether modified silicon oil
Organosiloxane-polyether block modification by copolymerization silicone oil, alkyl and polyether modified silicon oil, alkyl ether polyether silicone oil, epoxy group polyethers
Modified silicon oil, amino-polyether block silicone oil, glycerol ether silicone oil, the cruel base silicone oil of phosphoric acid, glycosyl polyethers silicone oil and beet base silicon
At least one of oil.
35. the lubricant oil composite that the method as described in any one of claim 13-34 is prepared.
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| CN1861673A (en) * | 2005-03-24 | 2006-11-15 | 莱茵化学莱茵瑙有限公司 | Microgels and thickening agents-containing compositions |
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| CN100528939C (en) * | 2003-09-27 | 2009-08-19 | 莱茵化学莱茵瑙有限公司 | Microgels in non-crosslinkable organic media |
| CN1861673A (en) * | 2005-03-24 | 2006-11-15 | 莱茵化学莱茵瑙有限公司 | Microgels and thickening agents-containing compositions |
| JP2013227438A (en) * | 2012-04-26 | 2013-11-07 | Mitsui Chemicals Inc | Lubricant composition |
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