CN106147952B - A kind of lubricant composition and preparation method thereof - Google Patents
A kind of lubricant composition and preparation method thereof Download PDFInfo
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- CN106147952B CN106147952B CN201510188843.3A CN201510188843A CN106147952B CN 106147952 B CN106147952 B CN 106147952B CN 201510188843 A CN201510188843 A CN 201510188843A CN 106147952 B CN106147952 B CN 106147952B
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Abstract
The present invention relates to lubricating grease field, a kind of lubricant composition and preparation method thereof is specifically provided.The rubber particles with cross-linked structure prepared by cross-linking radiation method that the lubricant composition 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 10-180 parts by weight.Lubricant composition provided by the invention can effectively adjust viscosity with the variation of temperature, temperature limit is wide, compared with the lubricant composition containing the rubber particles obtained by peroxide crosslinking, at 40 DEG C, kinematic viscosity is lower, and kinematic viscosity is higher at 100 DEG C.In addition, lubricant composition provided by the invention also has excellent antiwear and friction reduction property.
Description
Technical field
It is prepared the present invention relates to a kind of lubricant composition, the preparation method of the lubricant composition and by this method
Obtained lubricant composition.
Background technique
Lubricating grease is usually that thickening agent is dispersed in one or more of lube base oils, and obtains by saponification
Semisolid, the solid lubricant arrived.Common grease thickener is divided into soap base, non-soap base and hydrocarbyl type, soap base thickening agent
Mostly fatty acid salt, such as stearic acid calcium salt, 12- hydroxy stearic acid calcium salt, non-soap base thickening agent then includes organic polyureas, inorganization
Object etc. is closed, alkyl thickening agent is usually paraffin class.It generally can satisfy using lubricating grease prepared by above-mentioned thickening agent commonly used
Demand, but as modern industry rapidly develops, the high-grade, precision and advanced mechanical equipment continued to bring out is higher and higher to PERFORMANCE OF GREASES requirement,
Need to meet broader use temperature range, more high shear rates, more big load condition etc..Novel lubricating grease thickening agent as a result,
Or the exploitation of compound additive is in widespread attention.
Nano material refers to the solid material that the ultrafine dust by size less than 100 nanometers forms.Since it has than table
The features such as area is big, good dispersion, easy-sintering, big hardness, and there is good antifriction compressive property and nanoparticle opposite grinding
There is certain repair on damage surface, and therefore, it can be improved the service life of lubricating system.In addition, just because of using nanometer material
Lubricating oil, the lubricating grease of feed additives preparation reflect good tribological property, prepare high property using nano material additive
Energy lubricating grease has good prospect.
There is the report of the largely application about inorganic nano-particle in lubricating grease field in the prior art.For example,
CN104046407A discloses a kind of lubricating oil (rouge) antiwear and antifriction compound additive, consisting of oxide nano rare earth coats
Ultra-fine muscovite is added in base oil or lubricating grease with the ratio of 0.5-3%, it can is significantly reduced coefficient of friction, is reduced mill
Spot diameter.CN104031717A discloses a kind of aluminium nitride and copper mixing nanometer lubricating grease additive, this compound additive grain
Degree range is 50-200nm.Lubricating grease using the preparation of this additive has good antiwear and friction reduction property, and coefficient of friction can reduce
23.6-15.8%, friction durability can extend 6-7 times.CN103525513A discloses a kind of high temperature lubricating oil/fat composition and preparation
Method, wherein using boron nitride micro mist as thickening agent, using graphite microparticles and MCA (melamine cyanurate) as extreme-pressure anti-wear
The lubricating grease of agent, preparation has excellent high-temperature behavior, extreme pressure and antiwear behavior and oxidation stability.Although by adding inorganic receive
The lubricant composition that rice material obtains has excellent high temperature resistant, pressure resistance, wear-resisting property, but it is residual that easy sintering is used for a long time
Friction surface is stayed in, lubricant effect is influenced.In addition, most inorganic nano additives need to be used cooperatively with conventional thickening agent, this
The PERFORMANCE OF GREASES that sample is prepared can be improved, therefore increase manufacturing cost and use cost.
In addition, there are also the answering in lubricating grease 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 composition is poor, and the viscosity of the lubricant composition 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 composition, this will greatly limit the application of the lubricant composition.Therefore, it needs to develop
A kind of lubricant composition with preferable viscosity temperature characteristic.
Summary of the invention
The defect that the purpose of the invention is to overcome existing lubricant composition viscosity temperature characteristic poor, and one kind is provided
It the preparation method of lubricant composition, a kind of lubricant composition with excellent viscosity temperature characteristic and is prepared by this method
Lubricant composition.
The present inventor has found that Rhein Chemie Rheinau GmbH applies several above-mentioned after further investigation
Dispersed phase in lubricant composition 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 grease 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 compositions 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 composition, applicable for temperature
It is relatively narrow to spend range.And the rubber particles with cross-linked structure that are prepared by cross-linking radiation method and by using multifunctional chemical combination
The rubber particles with cross-linked structure that object or peroxide carry out chemical crosslinking preparation have entirely different microstructure.When
It is corresponding when dispersed phase in lubricant composition is the rubber particles with cross-linked structure prepared by cross-linking radiation method
Lubricant composition have good viscosity temperature characteristic, very well can adjust viscosity with the variation of temperature, reduce it is low
Warm viscosity simultaneously improves high temperature viscosity, therefore, can largely make up variation influence caused by viscosity as temperature.
In addition, high-energy radiation actually very cleaning, the safe and efficient energy, is widely used for by many developed countries at present
The fields such as health care, food processing, industrial production, instead be using Chemical Crosslinking Methods (peroxide) there are it is some can not
The problem of ignorance, such as the environmental pollution that production efficiency is not high, peroxide is remained and be may cause, these can all limit it
Using.
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 compositions, wherein the lubricant composition 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 10-180 parts by weight.
The present invention also provides a kind of preparation method of lubricant composition, this method is by silicone oil base oil and passes through irradiation
The rubber particles to be dispersed with cross-linked structure of cross-linking method preparation are mixed and are dispersed, and relative to 100 parts by weight
The silicone oil base oil, the dosages of the rubber particles to be dispersed is 10-180 parts by weight.
The present invention also provides lubricant compositions prepared by the above method.
Lubricant composition provided by the invention can effectively adjust viscosity with the variation of temperature, and viscosity temperature characteristic is excellent
Different, rubber particles therein make silicone oil base oil that stabilization be kept to not easily run off up to nano-dispersion, therefore, the profit
The temperature limit of grease composition is wide, and viscosity higher can still be maintained under high temperature high shear, can satisfy 100 DEG C with
On using temperature occasion lubricating requirement, be suitble to that the field of all grease applications, especially temperature be higher, antiwear and antifriction requirement
High field, as heavy load is mechanical, the lubrication occasion of running equipment steady in a long-term, and can also be multiple with other lubricating additives
With use, special lubricant composition is prepared.In addition, the antiwear and friction reduction property of lubricant composition provided by the invention is excellent
Different, the wearability of lubricant composition had not only can be improved in the rubber particles of nano-dispersion, but also can play similar micro- bearing
Effect, to increase rolling friction and reduce interface friction force.
Since cross-linking radiation makes special construction possessed by rubber particles, lubricant composition provided by the invention it is resistance to old
Change is had excellent performance, not easy to change, therefore this lubricant composition can be used as the lubricating grease haveing excellent performance and use, and especially answer
For the field more demanding to the viscosity temperature characteristic, ageing properties and frictional behaviour that lubricate oil systems.
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 composition 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 10-180 weight
Measure part.Wherein, the rubber particles are in stable dispersion state in silicone oil base oil.
The lubricant composition provided according to the present invention, as discussed previously with respect to the silicone oil basis of 100 parts by weight
The content of oil, the rubber particles is 10-180 parts by weight, but in order to enable silicone oil base oil and rubber particles play more
Good coordinated effect, and so that the lubricant composition 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 10-160 parts by weight, more preferably 10-120 weight
Measure part.
The lubricant composition 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 preferred 70-500nm.Exist when by the average grain diameter control of the rubber particles
When in above range, the viscosity of lubricant composition can be more effectively adjusted, broader use temperature range is suitable for.
The lubricant composition 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 composition 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
Son, ethyl rubber particles, hydroxyl rubber particles, hydrogeneous methyl silicone rubber particle, methyl vinyl silicone rubber particle, methyl
Ethenylphenyl rubber particles, methyl ethylene trifluoro propyl rubber particles, phenylene silicone rubber particle, phenylene ether base silicon
At least one of rubber particles, nitrile silicone rubber particle, silicon boron rubber particles and fluorine silicone rubber particle.
In addition, rubber particles provided by the invention are preferably equal phase structure.In the present invention, described " equal phase structure " is
Finger is observed under existing microtechnic, does not have to find the not homogeneous phenomenons such as layering, split-phase in rubber particles.
The lubricant composition 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 composition 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 composition provided by the invention includes by silicone oil base oil and passing through cross-linking radiation method
The rubber particles to be dispersed with cross-linked structure of preparation are mixed and are dispersed, and the silicon relative to 100 parts by weight
Oil base oil, the dosage of the rubber particles to be dispersed are 10-180 parts by weight.
The preparation method of the lubricant composition provided according to the present invention, as discussed previously with respect to described in 100 parts by weight
Silicone oil base oil, the dosages of the rubber particles to be dispersed are 10-180 parts by weight, but in order to enable silicone oil base oil and to
Dispersion rubber particles play the role of better coordinated, and so that the lubricant composition arrived has preferably viscous temperature
Performance, it is preferable that relative to the silicone oil base oil of 100 parts by weight, the dosage of the rubber particles to be dispersed is 10-
160 parts by weight, particularly preferably 10-120 parts by weight.
The preparation method of the lubricant composition provided according to the present invention, it is preferable that the rubber particles to be dispersed are
By average grain diameter be 20-2000nm, more preferably 50-1000nm, particularly preferably 70-500nm rubber particles reunite and
The rubber particles group of formation.After the rubber particles to be dispersed are dispersed in silicone oil base oil, the silicon rubber of reunion
Particle can be dispersed well, thus with 20-2000nm, preferably with 50-1000nm, more preferable being averaged with 70-500nm
Particle diameter distribution is in silicone oil base oil.In addition, the average grain diameter of the rubber particles to be dispersed is preferably 20-2000nm, more
Preferably 50-1000nm, particularly preferably 70-500nm.
The preparation method of the lubricant composition provided according to the present invention, it is preferable that the rubber particles to be dispersed
Gel content is 60 weight % or more, more preferably 75 weight % or more, particularly preferably 80 weight % or more.When will it is described to
When dispersing the gel content control of rubber particles within the above range, lubrication can be more effectively adjusted with the variation of temperature
The viscosity of oil/fat composition is suitable for broader use temperature range.
The rubber particles to be dispersed preferably have equal phase structure.In the present invention, described " equal phase structure " refers to
It is observed under existing microtechnic, wait disperse in rubber particles not having to find the not homogeneous phenomenons such as layering, split-phase.
The rubber particles to be dispersed can be selected from methyl silicone rubber particle, ethyl rubber particles, hydroxyl silicon rubber
Particle, hydrogeneous methyl silicone rubber particle, methyl vinyl silicone rubber particle, methyl vinyl phenyl rubber particles, methyl second
Alkenyl trifluoro propyl rubber particles, phenylene silicone rubber particle, phenylene ether base rubber particles, nitrile silicone rubber particle, silicon boron
At least one of rubber particles and fluorine silicone rubber particle.
In the preparation process of the rubber particles to be dispersed, high-energy ray source used in cross-linking radiation can specifically be 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 less than 0.1 μm,
For example, cobalt source.In addition, under normal circumstances, the dosage of irradiation should make the solidifying of the rubber particles after rubber latex cross-linking radiation
Glue content reaches 60 weight % or more, preferably reaches 75 weight % or more, more preferably up to 80 weight % or more.Specifically, spoke
According to dosage can be 0.1-30Mrad, preferably 0.5-20Mrad.
The rubber particles to be dispersed can be commercially available, can also be according to various sides well known to art technology
Method is prepared.For example, the rubber particles to be dispersed can be passed for applicant according to the invention on September 18th, 2000
The international patent application WO01/40356 (priority date on December 3rd, 1999) of friendship and applicant of the present invention were in 2001 6
What the method that the international patent application WO01/98395 (priority date on June 15th, 2000) that the moon is submitted on the 15th is provided was prepared
Silicon rubber powder particle.By above method preparation without adding interleaving agent can be free after dispersing rubber particles and being drying
The rubber micro mist of flowing, wherein each rubber particle is homogeneous, i.e., single particle is all homogeneous in composition, existing
Having under the observation of microtechnic does not have to find the not homogeneous phenomenons such as layering, split-phase in particle.The powdered rubber is by by phase
The rubber latex cross-linking radiation answered and the partial size of rubber particles is able to fixed.
In addition, cross-linking aid can not be used in the cross-linking radiation preparation process of the rubber particles to be dispersed,
Cross-linking aid can be used.The cross-linking aid can be selected from simple function group cross-linking aid, two functional group's cross-linking aids, trifunctional
Group's cross-linking aid, any one in the above cross-linking aid of four-functional group cross-linking aid and five functional groups.The simple function group is handed over
The example of connection auxiliary agent includes but is not limited to: (methyl) 2-ethyl hexyl acrylate, (methyl) Isooctyl acrylate monomer, (methyl) acrylic acid shrink
At least one of glyceride；The example of two functional group cross-linking aid includes but is not limited to: 1,4- butanediol two (methyl)
Acrylate, 1,6-hexylene glycols two (methyl) acrylate, diethylene glycol two (methyl) acrylate, triethylene glycol two (methyl)
At least one of acrylate, neopentyl glycol two (methyl) acrylate, divinylbenzene；The trifunctional cross-linking aid
Example include but is not limited to: trimethylolpropane tris (methyl) acrylate and/or pentaerythrite three (methyl) acrylate；
The example of the 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 are handed over
Connection 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 be 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 composition provided by the invention can also include by additive and silicone oil base oil
It is mixed and is dispersed together with rubber particles to be dispersed.
The type of the silicone oil base oil and additive has been described herein above, and therefore not to repeat here.
The present invention is not particularly limited the mode of the mixing and redisperse, as long as enabling to described to dispersed silicon
Rubber particles are effectively dispersed in silicone oil base oil, to obtain using silicone oil base oil as continuous phase and with rubber particles
For the lubricant composition of dispersed phase.A preferred embodiment of the invention, the mixing and the mode dispersed
Include:
(1) rubber particles to be dispersed are added in the silicone oil base oil and are mixed by mechanical stirring, so that
The rubber particles dispersion to be dispersed is suspended in the silicone oil base oil, the composition tentatively dispersed；
(2) composition tentatively dispersed is subjected to redisperse, until the average grain diameter of the rubber particles after dispersion
In the range of reaching 20-2000nm, in the range of preferably reaching 50-1000nm, in the range of more preferably up to 70-500nm.It is logical
It crosses this preferred mixing and the mode dispersed enables to rubber particles to be dispersed in silicone oil base oil with initial size, obtain
The viscosity temperature characteristic of the lubricant composition arrived is more preferably.
According to another preferred method of implementation of the present invention, the preparation method of the lubricant composition further includes step
(3), product step (2) obtained not less than 80 DEG C at a temperature of, preferably not less than 100 DEG C at a temperature of, more preferably
It places at least 1 hour, preferably places at least 2 hours at 100-200 DEG C, more preferably place at least 4 hours, most preferably placement 4-
Obtained product is subjected to secondary redisperse after 10 hours, enables to the rubber particles and silicone oil base oil of crosslinking in this way
Sufficiently infiltrate and be swollen, and rubber particles with smaller particle size dispersion in silicone oil base oil, to obtain viscosity temperature characteristic
Better lubricant composition.In addition, in step (3), by the product of step (2) not less than 80 DEG C at a temperature of place at least
During 1 hour, it can cooperate and accomplished continuously or intermittently stir, so that stirring material is heated more evenly.
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 and silicon to be dispersed with cross-linked structure prepared by cross-linking radiation method
Under the premise of the performance of oil base oil does not have any variation, make to prepare by cross-linking radiation method with cross-linked structure to point
It dissipates rubber particles dispersion or is suspended in silicone oil base oil, this those skilled in the art can be known, do not made herein
It repeats.
The preparation method of the lubricant composition provided according to the present invention, redisperse and step described in step (2)
(3) the secondary redisperse described in can be squeezed out in homogenizer, bead mill, three-roll grinder, single screw rod each independently
It carries out at least one of machine, multi-screw extruder, kneader, dissolvers and ultrasonic disperser mixing apparatus, preferably exists
It is carried out in homogenizer, three-roll grinder and ultrasonic disperser, these three preferred mixing apparatus have processing output height, mixing
The advantage that effect is good, subsequent cleaning is fairly simple.Most preferably, secondary in the redisperse and step (3) in step (2) divides again
It is dispersed in homogenizer and carries out.In dispersion process, according to different dispersion quality requirements, need by cycles samples cooling, then instead
Repeatedly dispersed by mixing apparatus again, until the average grain diameter for the rubber particles being dispersed in silicone oil base oil reaches
It 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, of the invention
The condition of the redisperse and secondary redisperse is not particularly limited, as long as silicone oil base oil and rubber particles is made to exist
Performance is not destroyed in dispersion process, and the partial size of rubber particles is made to reach 20-2000nm, preferably reach 50-
1000nm, more preferably up to 70-500nm, can know this those skilled in the art, therefore not to repeat here.
It, specifically can be in addition, placement described in step (3) preferably carries out in existing various airtight heating equipment
It is carried out in high temperature oven, vacuum high-temperature baking oven, heating kettle or similar airtight heating container, heat treatment efficiency can be improved in this way,
It is energy saving, while the contact of silicone oil base oil and rubber particles with air (oxygen) can also be reduced, reduce thermal oxide journey
Degree makes properties of product keep stablizing.
The present invention also provides lubricant compositions 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:
Methyl-silicone oil A, Japan XINYUE's production, trade mark 201-50, (25 DEG C) of viscosity are 50cp (1cp=1mPa
s)。
Methyl-silicone oil B, Japan XINYUE's production, trade mark 201-350, (25 DEG C) of viscosity are 350cp.
Rubber particles to be dispersed, Sinopec production, trade mark VP601, average grain diameter 100nm, 88 weight of gel content
% is measured, is observed under the microscope, it should be wait disperse without discovery layering, noted phase separation phenomena in rubber particles, by methyl ethylene
Silicon rubber lotion carries out cross-linking radiation method preparation using cobalt source and is dried to obtain by spray drying process.
Peroxide crosslinking rubber particles prepare and using spraying according to method disclosed in patent CN1840622A
Drying means obtains, rubber latex be respectively methyl vinyl silicone rubber lotion (with prepare rubber particles VP601 institute to be dispersed
The composition of the rubber latex of use is identical), the crosslinking agent used is cumyl peroxide (DCP), the peroxidating finally obtained
The average grain diameter of object cross-linked silicone rubber particle is 100nm, and gel content is 88 weight %.
(2) the following instrument and equipment of the experimental data in embodiment and comparative example and measuring method measurement:
(1) dynamic viscosity: the lubricating grease group at 40 DEG C and 100 DEG C is tested respectively using NDJ-5S type number rotational viscometer
Close the dynamic viscosity of object, wherein heat using oil bath temperature control.
(2) divide oil mass: being tested according to SH/T 0324-92 " lubricating grease Stencil oil-dividing measuring method (static method) " standard method,
Specifically, sample is placed on 100 mesh copper mesh, stands 24 hours in 100 DEG C of baking ovens and further takes out measurement point oil mass.
(3) coefficient of friction: the interface friction performance of measuring lubricating grease composition, load are on electronic tension tester
0.2kg compares the confficient of static friction μ of aluminium-steel (unlubricated) and aluminium-steel (having lubrication)sWith dynamic friction coefficient μk, wherein it is unlubricated
It indicates uncoated any lubricant composition in aluminium-steel material surface, there is lubrication to indicate to have been coated in aluminium-steel surface accordingly
Lubricant composition.
Embodiment 1
The embodiment is for illustrating lubricant composition provided by the invention and preparation method thereof.
By 100 parts by weight methyl-silicone oil A and 10 parts by weight rubber particles VP601 to be dispersed is mixed and mechanical stirring is equal
Even, then homogenizing circulation five times in three-roll grinder, roller revolving speed is 280 revs/min when homogenizing, and clearance between roll is minimum when dispersion
To 10 μm, mixed material is obtained.Said mixture material is kept for 4 hours in 150 DEG C of high temperature ovens, is ground again by three rollers
Machine homogenizing circulation five times, roller revolving speed is 280 revs/min when homogenizing, and clearance between roll is minimal to 5 μm when dispersion, obtains lubricating grease group
Object is closed, dynamic viscosity, point oil mass and greasy property are shown in Tables 1 and 2 respectively.
Comparative example 1
The comparative example is for illustrating lubricant composition of reference and preparation method thereof.
Lubricant composition is prepared according to the method for embodiment 1, unlike, rubber particles VP601 to be dispersed is used
The peroxide crosslinking rubber particles of identical weight part substitute, and obtain reference lubricant composition, dynamic viscosity divides oil mass
And greasy property is shown in Tables 1 and 2 respectively.
Embodiment 2
The embodiment is for illustrating lubricant composition provided by the invention and preparation method thereof.
By 100 parts by weight methyl-silicone oil A and 30 parts by weight rubber particles VP601 to be dispersed is mixed and mechanical stirring is equal
Even, then homogenizing circulation five times in three-roll grinder, roller revolving speed is 280 revs/min when homogenizing, and clearance between roll is minimum when dispersion
To 10 μm, mixed material is obtained.Said mixture material is kept for 4 hours in 150 DEG C of high temperature ovens, is ground again by three rollers
Machine homogenizing circulation five times, roller revolving speed is 280 revs/min when homogenizing, and clearance between roll is minimal to 5 μm when dispersion, obtains lubricating grease group
Object is closed, dynamic viscosity, point oil mass and greasy property are shown in Tables 1 and 2 respectively.
Embodiment 3
The embodiment is for illustrating lubricant composition provided by the invention and preparation method thereof.
By 100 parts by weight methyl-silicone oil A and 50 parts by weight rubber particles VP601 to be dispersed is mixed and mechanical stirring is equal
Even, then homogenizing circulation five times in three-roll grinder, roller revolving speed is 100 revs/min when homogenizing, and clearance between roll is minimum when dispersion
To 10 μm, mixed material is obtained.Said mixture material is kept for 4 hours in 150 DEG C of high temperature ovens, is ground again by three rollers
Machine homogenizing circulation five times, roller revolving speed is 100 revs/min when homogenizing, and clearance between roll is minimal to 5 μm when dispersion, obtains lubricating grease group
Object is closed, dynamic viscosity, point oil mass and greasy property are shown in Tables 1 and 2 respectively.
Embodiment 4
The embodiment is for illustrating lubricant oil composite provided by the invention and preparation method thereof.
By 100 parts by weight methyl-silicone oil A and 100 parts by weight rubber particles VP601 to be dispersed is mixed and mechanical stirring is equal
Even, then the homogenizing circulation five times, homogenization pressure 100MPa in high pressure homogenizer, every circulation primary all by water-bath cooling will
The temperature control of material is being no more than 70 DEG C, obtains mixed material.Said mixture material is kept 4 in 150 DEG C of high temperature ovens
Hour, then circulation is homogenized five times by second of high pressure homogenizer, homogenization pressures 100MPa obtains lubricant oil composite,
Dynamic viscosity, point oil mass and greasy property are shown in Tables 1 and 2 respectively.
Embodiment 5
The embodiment is for illustrating lubricant composition provided by the invention and preparation method thereof.
By 100 parts by weight methyl-silicone oil B and 10 parts by weight rubber particles VP601 to be dispersed is mixed and mechanical stirring is equal
Even, then homogenizing circulation five times in three-roll grinder, roller revolving speed is 280 revs/min when homogenizing, and clearance between roll is minimum when dispersion
To 10 μm, mixed material is obtained.Said mixture material is kept for 4 hours in 150 DEG C of high temperature ovens, is ground again by three rollers
Machine homogenizing circulation five times, roller revolving speed is 280 revs/min when homogenizing, and clearance between roll is minimal to 5 μm when dispersion, obtains lubricating grease group
Object is closed, dynamic viscosity, point oil mass and greasy property are shown in Tables 1 and 2 respectively.
Embodiment 6
The embodiment is for illustrating lubricant composition provided by the invention and preparation method thereof.
By 100 parts by weight methyl-silicone oil B and 50 parts by weight rubber particles VP601 to be dispersed is mixed and mechanical stirring is equal
Even, then homogenizing circulation five times in three-roll grinder, roller revolving speed is 100 revs/min when homogenizing, and clearance between roll is minimum when dispersion
To 10 μm, mixed material is obtained.Said mixture material is kept for 4 hours in 150 DEG C of high temperature ovens, is ground again by three rollers
Machine homogenizing circulation five times, roller revolving speed is 100 revs/min when homogenizing, and clearance between roll is minimal to 5 μm when dispersion, obtains lubricating grease group
Object is closed, dynamic viscosity, point oil mass and greasy property are shown in Tables 1 and 2 respectively.
Embodiment 7
The embodiment is for illustrating lubricant composition provided by the invention and preparation method thereof.
By 100 parts by weight methyl-silicone oil B and 100 parts by weight rubber particles VP601 to be dispersed is mixed and mechanical stirring is equal
Even, then homogenizing circulation five times in three-roll grinder, roller revolving speed is 100 revs/min when homogenizing, and clearance between roll is minimum when dispersion
To 10 μm, mixed material is obtained.Said mixture material is kept for 4 hours in 150 DEG C of high temperature ovens, is ground again by three rollers
Machine homogenizing circulation five times, roller revolving speed is 100 revs/min when homogenizing, and clearance between roll is minimal to 5 μm when dispersion, obtains lubricating grease group
Object is closed, dynamic viscosity, point oil mass and greasy property are shown in Tables 1 and 2 respectively.
The dynamic viscosity of 1 lubricant composition of table and divide oil mass
The greasy property of 2 lubricant composition of table
From the results shown in Table 1, with contain the lubricating grease group of rubber particles obtained by peroxide crosslinking
It closes object to compare, the lubricant composition containing the rubber particles with cross-linked structure obtained by cross-linking radiation method is low
When warm (40 DEG C) viscosity is lower, and (100 DEG C) viscosity is higher at high temperature, therefore, lubricant composition tool provided by the invention
There is better viscosity temperature characteristic, temperature limit is wide.
In addition, from the results shown in Table 2, the antiwear and friction reduction property of lubricant composition provided by the invention is very excellent
It is different.
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 composition, which is characterized in that the lubricant composition contains base oil and is dispersed in the basis
The rubber particles with cross-linked structure prepared by cross-linking radiation method in 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 content of the rubber particles
For 10-180 parts by weight；The average grain diameter of the rubber particles is 20-2000nm；The gel content of the rubber particles is
60 weight % or more.
2. lubricant composition 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 10-160 parts by weight.
3. lubricant composition 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 10-120 parts by weight.
4. lubricant composition according to claim 1, wherein the average grain diameter of the rubber particles is 50-
1000nm。
5. lubricant composition according to claim 4, wherein the average grain diameter of the rubber particles is 70-
500nm。
6. lubricant composition according to claim 1, wherein the gel content of the rubber particles is 75 weight %
More than.
7. lubricant composition according to claim 6, wherein the gel content of the rubber particles is 80 weight %
More than.
8. lubricant composition described in any one of -3 according to claim 1, wherein the rubber particles have homogeneous
Structure.
9. lubricant composition 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, methyl vinyl silicone rubber
Particle, methyl vinyl phenyl rubber particles, methyl ethylene trifluoro propyl rubber particles, phenylene silicone rubber particle,
At least one of phenylene ether base rubber particles, nitrile silicone rubber particle, silicon boron rubber particles and fluorine silicone rubber particle.
10. lubricant composition 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 composition 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 composition 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 composition, this method includes by silicone oil base oil and by cross-linking radiation method system
The standby rubber particles to be dispersed with cross-linked structure are mixed and are dispersed, and the silicone oil relative to 100 parts by weight
Base oil, the dosage of the rubber particles to be dispersed are 10-180 parts by weight；The rubber particles to be dispersed are by average
The rubber particles that partial size is 20-2000nm are reunited and the rubber particles group of formation；The gel of the rubber particles to be dispersed
Content is 60 weight % or more.
14. according to the method for claim 13, wherein the mixing and mode dispersed includes:
(1) rubber particles to be dispersed are added in the silicone oil base oil and are mixed by mechanical stirring, so that described
Rubber particles dispersion to be dispersed is suspended in the silicone oil base oil, the composition tentatively dispersed；
(2) composition tentatively dispersed is subjected to redisperse, until the average grain diameter of the rubber particles after dispersion reaches
In the range of 20-2000nm.
15. according to the method for claim 14, wherein the composition tentatively dispersed is subjected to redisperse, until point
The average grain diameter of rubber particles after dissipating reaches in the range of 50-1000nm.
16. according to the method for claim 15, wherein the composition tentatively dispersed is subjected to redisperse, until point
The average grain diameter of rubber particles after dissipating reaches in the range of 70-500nm.
17. according to the method for claim 14, wherein this method further includes step (3), the product that step (2) is obtained
Not less than 80 DEG C at a temperature of place at least 1 hour, obtained product is subjected to secondary redisperse later.
18. according to the method for claim 17, wherein this method further includes step (3), the product that step (2) is obtained
Not less than 100 DEG C at a temperature of place at least 2 hours, obtained product is subjected to secondary redisperse later.
19. according to the method for claim 18, wherein this method further includes step (3), the product that step (2) is obtained
Not less than 100 DEG C at a temperature of place at least 4 hours, obtained product is subjected to secondary redisperse later.
20. according to the method for claim 17, wherein described in redisperse described in step (2) and step (3) it is secondary again
Dispersion is each independently in homogenizer, bead mill, three-roll grinder, single screw extrusion machine, multi-screw extruder, kneading
It is carried out at least one of machine, dissolvers and ultrasonic disperser mixing apparatus.
21. according to the method for claim 20, wherein described in redisperse described in step (2) and step (3) it is secondary again
Dispersion carries out at least one of homogenizer, three-roll grinder and ultrasonic disperser mixing apparatus each independently.
22. according to the method for claim 21, wherein described in redisperse described in step (2) and step (3) it is secondary again
Dispersion carries out in homogenizer each independently.
23. according to the method for claim 17, wherein be placed in airtight heating equipment and carry out described in step (3).
24. according to the method for claim 13, wherein described wait divide relative to the silicone oil base oil of 100 parts by weight
The dosage for dissipating rubber particles is 10-160 parts by weight.
25. according to the method for claim 24, wherein described wait divide relative to the silicone oil base oil of 100 parts by weight
The dosage for dissipating rubber particles is 10-120 parts by weight.
26. according to the method for claim 13, wherein it is 50- that the rubber particles to be dispersed, which are by average grain diameter,
1000nm rubber particles are reunited and the rubber particles group of formation.
27. according to the method for claim 26, wherein it is 70- that the rubber particles to be dispersed, which are by average grain diameter,
500nm rubber particles are reunited and the rubber particles group of formation.
28. according to the method for claim 13, wherein the gel content of the rubber particles to be dispersed is 75 weight %
More than.
29. according to the method for claim 28, wherein the gel content of the rubber particles to be dispersed is 80 weight %
More than.
30. method described in any one of 3-25 according to claim 1, wherein the rubber particles to be dispersed have equal
Phase structure.
31. method described in any one of 3-25 according to claim 1, wherein the rubber particles to be dispersed are selected from first
Base rubber particles, ethyl rubber particles, hydroxyl rubber particles, hydrogeneous methyl silicone rubber particle, methyl ethylene silicon rubber
Micelle, methyl vinyl phenyl rubber particles, methyl ethylene trifluoro propyl rubber particles, phenylene silicone rubber grain
At least one of son, phenylene ether base rubber particles, nitrile silicone rubber particle, silicon boron rubber particles and fluorine silicone rubber particle.
32. method described in any one of 3-25 according to claim 1, wherein the silicone oil 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 composition that the method as described in any one of claim 13-34 is prepared.
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| JPH06330071A (en) * | 1993-05-24 | 1994-11-29 | Nippon Seiko Kk | Lubricant composition |
| US6015777A (en) * | 1997-04-16 | 2000-01-18 | University Of Connecticut | Silicone greases and methods for their production |
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| US4401781A (en) * | 1981-04-06 | 1983-08-30 | Nippon Cable System Inc. | Lubricative, oily, cross-linked resin composition |
| JPH06330071A (en) * | 1993-05-24 | 1994-11-29 | Nippon Seiko Kk | Lubricant composition |
| US6015777A (en) * | 1997-04-16 | 2000-01-18 | University Of Connecticut | Silicone greases and methods for their production |
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