CN102911762A - High-thermal conductivity lubricating oil and preparation method thereof - Google Patents
High-thermal conductivity lubricating oil and preparation method thereof Download PDFInfo
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- CN102911762A CN102911762A CN2012104348147A CN201210434814A CN102911762A CN 102911762 A CN102911762 A CN 102911762A CN 2012104348147 A CN2012104348147 A CN 2012104348147A CN 201210434814 A CN201210434814 A CN 201210434814A CN 102911762 A CN102911762 A CN 102911762A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 31
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Abstract
The invention relates to high-thermal conductivity lubricating oil and a preparation method thereof. The lubricating oil contains base oil and fluorinated graphene nanosheets, wherein the weight percent of content of the fluorinated graphene nanosheets is 0.01 to 10.0 %; and the preparation method comprises the steps as follows: firstly, preparing the fluorinated graphene nanosheets; and secondly, preparing the lubricating oil containing the fluorinated graphene nanosheets. The lubricating oil provided by the invention has the advantages of excellent antifriction effect, extremely high heat conduction capability and excellent stability and dispersibility.
Description
Technical field
The present invention relates to a kind of high thermal conduction characteristic lubricating oil and preparation method thereof that has, belong to the preparation field that machinery or aerospace are used the abrasion-proof lubricant oil medium.
Background technology
Lubricating oil or lubricating grease can be good at reducing the friction between the surface in contact (abbreviation friction pair) of two relative movement, can repair the effect of two friction pairs wearing and tearing simultaneously, and oilness and resistance to abrasion are the important symbols of lubricants performance.In a lot of mechanical movement occasions, the friction between surface in contact is a very violent motion, and larger pressure is arranged between friction pair, will produce high temperature in the friction process simultaneously.High Temperature High Pressure will produce larger impact to the physico-chemical property of lubricating oil.In order to remedy the defective of lubricating oil, usually adopt lubricity and the abrasion resistance of the method raising lubricating oil of slip additive, capable of reducing friction resistance, the work-ing life of prolongation element part.
Solid lubricant is joined in the lubricating oil, improve antiwear and antifriction and the extreme pressure property of lubricating oil, existing history for many years, wherein the most representative is the lubricating oil additive of stratiform class.Stratified material is owing to a little less than the combination between layers, just divide between parallel layers easily when being subject to External Force Acting and come, and namely between layers shear strength is lower, and friction resistance is less.The lubricating oil additive of stratiform class has mainly represented graphite, MoS
2, nanometer polytetrafluoroethylcomposite etc. [Jia Huadong, Liu Gang, Fan Ronghuan. nano material is as the Research Review of slip additive and present developments and prospect [J]. lubricated and sealing, 2006,175 (3): 181-18].The part but these interpolation materials come with some shortcomings is such as MoS
2May with surface in contact generation chemical action, cause oxidation and corrosion; Tetrafluoroethylene (PTFE) makes the thermal conductivity of lubricating oil and thermostability will become very poor; Because the density difference between graphite and the lubricating oil is larger, thus often need to add too much dispersion agent, so that stable system, and the too much adding of dispersion agent, easily make lubricating oil generation emulsification and rotten [Wang Xiaobo, graphite lubricating oil (GLO), Chinese patent application number: 01135108.X; Zhang Ruchun, graphite lubricating oil (GLO) and preparation method thereof, Chinese patent application number: 03139216.4], in addition, graphite is under vacuum or reducing atmosphere, and lubricity greatly reduces.
Along with the development of technology, mechanical industry is had higher requirement to lubricating oil.Lubricating oil not only will have preferably and to reduce friction and the effect that reduces wear, and more requires the life-time service that lubricating oil can be under extreme conditions.Lubricating oil must play the cooling thermal discharge effect, and the heat that lubricating oil produces when only having mechanical friction is taken away, and keeps certain thermal equilibrium state, could prevent effectively that Yin Wendu from constantly raising and the damage parts of generation.And existing lubricant base (mainly dividing mineral base oil, the oily three major types of synthetic base oil and vegetables oil basis) substantially all is made of organism, and thermal conductivity is low especially.This just causes the cooling thermal discharge effect of lubricating oil not obvious, so that the temperature of lubricating oil and friction pair is all very high.This can make friction pair more easy to wear on the one hand, and more so that lubricating oil is at high temperature perishable, the life-span reduces greatly.Exploitation has good antiwear and antifriction effect, and has quality, result of use and life-span that the lubricating oil of high thermal conductivity can improve lubricating oil undoubtedly greatly.
Summary of the invention
The objective of the invention is to overcome the defective of existing lubricating oil, a kind of lubricating oil with high thermal conductivity is provided.
For realizing purpose of the present invention, technical scheme of the present invention is:
A kind of high thermal conductivity lubricating oil, this lubricating oil comprises: base oil and fluorinated graphene nanometer sheet, wherein the weight percentage of fluorinated graphene nanometer sheet is 0.01%-10.0%.
In a preferred embodiment of the present invention, the weight percentage of described fluorinated graphene nanometer sheet is 0.01%-10.0%, and described lubricating oil comprises that also weight percentage is the dispersion agent of 0.01%-1.0%.
In a preferred embodiment of the present invention, described base oil is Witco 70 or HVI150SN lubricating oil.
In a preferred embodiment of the present invention, described dispersion agent is one or more the mixture in polyisobutylene-bis-succinimide, boronation polyisobutene succinimide, isopropyl titanate, sorbitan monooleate, polyoxyethylene glycol, polyvinylpyrrolidone, sodium polyacrylate, stearic acid or the oleic acid.
Another object of the present invention provides a kind of preparation method of high thermal conductivity lubricating oil, and the method may further comprise the steps:
(1) preparation fluorinated graphene nanometer sheet;
(2) lubricating oil of preparation fluorinated graphene nanometer sheet.
In a preferred embodiment of the present invention, described step (2) comprising:
1) the fluorinated graphene nanometer sheet is progressively joined in the base oil, stir;
2) mixture of step 1) gained homogenized and the gelatinizing processing, obtain uniform and stable lubricating oil.
In a preferred embodiment of the present invention, described step (2) comprising:
1) with after fluorinated graphene nanometer sheet and the dispersant, progressively joins in the base oil, stir;
2) mixture of step 1) gained homogenized and the gelatinizing processing, obtains uniform and stable lubricating oil,
In a preferred embodiment of the present invention, homogenizing in described is operating as the common implementing of a kind of in mechanical stirring or the sonic oscillation or two kinds.
In a preferred embodiment of the present invention, the gelatinizing in described is treated to glue mill technology.
In a preferred embodiment of the present invention, in the step (1), the described method for preparing the fluorinated graphene nanometer sheet is gaseous fluoridizing method or fluorographite stripping method.
The advantage of lubricating oil of the present invention is: 1) excellent antiwear and antifriction effect: compare with not additivated basic grease, can make the wear scar diameter decreased average more than 50%, rubbing factor reduces more than 60%, also has simultaneously preferably supporting capacity; This gives the credit to the unique texture of fluorinated graphene.As everyone knows, Graphene is the carbon simple substance of neatly being arranged and forming by hexagonal lattice by carbon atom, and structure is highly stable.Graphene and associated materials thereof be because its excellent electricity, calorifics and mechanical property, caused the extensive concern of community of physicists, material educational circles.The fluorinated graphene nanometer sheet has and the similar structure and characteristics of graphene nanometer sheet.The fluorinated graphene nanometer sheet is keeping the original laminate structure of graphite, but because fluorine enters between graphene layer, and electronics forms covalent linkage between graphene layer, and the bond energy between graphene layer significantly reduces, only be 8.4kJ/mol, low more than the interlayer energy 37.6kJ/mol of Graphene.In addition, because the upper and lower surface of the netted plane layer of Graphene hexagonal is gathered in conjunction with fluorine atom, and fluorine atom between layers has again repulsion each other, and they can offset the pressure from the outside, meanwhile, outside harsh atmosphere and temperature are difficult for making firmly F-C key disconnection.2) very high thermal conduction capability: the thermal conductivity ratio base oil is enhanced about more than once; The fluorinated graphene nanometer sheet has higher thermal conductivity, and less with the interface resistance of base oil.A small amount of fluorinated graphene nanometer sheet can increase substantially thermal conductivity and the thermal conduction capability of base oil; 3) excellent stability and dispersed: the fluorinated graphene nanometer sheet has very high specific surface area, and light weight, and apparent density can reach 0.002g/cm
3, and the density difference between base oil is little, can very easily be scattered in the base oil, even do not add tensio-active agent and dispersion agent, also can reach more than 6 months stationary phase.Add indivisible dispersion agent, can reach more than 2 years stationary phase, and the obvious emulsion of nothing under the high temperature lubricating situation, thoroughly solved the immiscible problem of lubricating oil additive and base oil.Therefore, the lubricating oil that contains the fluorinated graphene nanometer sheet of the present invention has higher thermal conductivity when having good antiwear and antifriction effect, the heat that produces in the friction process in time can be removed.
Description of drawings
Fig. 1 is the transmission electron microscope picture that gaseous fluoridizing method prepares the fluorinated graphene nanometer sheet.
Fig. 2 is the atomic force microscope figure that gaseous fluoridizing method prepares the fluorinated graphene nanometer sheet.
Fig. 3 is the transmission electron microscope picture that the fluorographite stripping method prepares the fluorinated graphene nanometer sheet.
Fig. 4 is the atomic force microscope figure that the fluorographite stripping method prepares the fluorinated graphene nanometer sheet.
Embodiment
Further specify the present invention below by embodiment.
Embodiment 1
A kind of high thermal conductivity lubricating oil comprises: weight percentage is that 98% Witco 70 and weight percentage are 2% fluorinated graphene nanometer sheet.
The preparation method of this lubricating oil is:
(1) gaseous fluoridizing method prepares the fluorinated graphene nanometer sheet: 1) preparation graphite oxide: in ice bath, 10g Graphite Powder 99 and 5g SODIUMNITRATE and the 230mL vitriol oil are mixed slow adding 30gKMn0 in the stirring
4Transfer them in 35 ° of C water-baths reaction 30 minutes, progressively add the 460mL deionized water again, continue reaction 40 minutes after temperature rises to 98 ℃, mixture becomes glassy yellow by brown, further thin up, and be 30% H with weight fraction
20
2Solution-treated; unreacted permanganic acid neutralizes; centrifuging and repetitive scrubbing filter cake; at last its vacuum-drying is namely obtained graphite oxide; 2) preparation Graphene: graphite oxide is ground; adopt high temperature thermal expansion (1000 ° of C of temperature; argon gas or nitrogen protection; reaction times 10-60 second) namely obtains Graphene; 3) preparation fluorinated graphene: (its weight fraction is respectively w (KF)=60% to utilize electrolytic tank electrolysis KF.2HF electrolytic solution; w (HF)=40%) can make fluorine gas, with the stainless steel tube introducing 500 ° of C of temperature of reaction are housed in the tube furnace reactor of Graphene after it is purified; react after 15 hours; stop to pass into and heating of fluorine gas, pass into nitrogen protection and cooling, can make fluorinated graphene.The fluorinated graphene that this kind method makes is thinner, between the 1-10 layer, thickness in 2nm, light weight, apparent density can reach 0.002g/cm
3, its transmission electron microscope and atomic force microscope figure are respectively as shown in Figures 1 and 2; (2) lubricating oil of preparation fluorinated graphene nanometer sheet: the fluorinated graphene nanometer sheet that 1) will adopt described method to obtain progressively adds in the whiteruss, its weight percentage is 2.0%, 2) to said mixture, under 60 ℃ of conditions, at first adopt mechanical stirring, stirred 2 hours, then adopt glue mill technology, glue mill 2 hours obtains uniform and stable lubricating oil.
Body series does not use dispersion agent, and the frictional wear experiment of this lubricating oil carries out at the MRS-10A type four-ball friction and wear test machine that trier factory in Jinan makes, and employed steel ball is the GCr15 bearing steel, and its diameter is 12.7mm, and hardness is 61-64HRC.Test result shows, under the test conditions of load 300N, time 30min and rotating speed 1450r/min, add 2% fluorinated graphene nanometer sheet after, its steel ball mill spot diameter decreased average 52%, rubbing factor reduces by 62%.Adopt a short silk thermal conductance instrument, recorded contain the 2.0%(weight percentage) the thermal conductivity of fluorinated graphene nanometer sheet whiteruss, improved 116% than neat liquid paraffin, thermal conduction capability improves greatly.
Embodiment 2
A kind of high thermal conductivity lubricating oil comprises: weight percentage is 94.95% HVI150SN lubricating oil, and weight percentage is that 5% fluorinated graphene nanometer sheet and weight percentage are 0.05% sorbitan monooleate tween 80.
The preparation method of this lubricating oil is:
(1) gaseous fluoridizing method prepares the fluorinated graphene nanometer sheet: its preparation process is identical with embodiment 1; (2) lubricating oil of preparation fluorinated graphene nanometer sheet: 1) progressively add in the HVI150SN lubricant base after will adopting fluorinated graphene nanometer sheet that described method obtains and oil-soluble dispersant sorbitan monooleate tween 80 mixing, wherein, fluorinated graphene nanometer sheet weight percentage is 5%, and the weight percentage of dispersion agent is 0.05%; 2) under 60 ℃ of conditions, to said mixture, at first high speed machine stirred 30 minutes, and ultrasonic 30 minutes again, then adopt glue mill technology, can obtain the lubricating oil of stable dispersion.
The frictional wear experiment condition embodiment 1 of this lubricating oil is identical.Test result shows, under the test conditions of load 300N, time 30min and rotating speed 1450r/min, add 5% fluorinated graphene nanometer sheet after, its steel ball mill spot diameter decreased average 65%, rubbing factor reduces by 79%.Adopt a short silk thermal conductance instrument, recorded contain the 5%(weight percentage) the fluorinated graphene nanometer sheet enters the thermal conductivity of HVI150SN base oil, improved 186% than neat liquid paraffin, thermal conduction capability improves greatly.
Embodiment 3
A kind of high thermal conductivity lubricating oil comprises: weight percentage is that 98.2% Witco 70 and weight percentage are 1.8% fluorinated graphene nanometer sheet.
The preparation method of this lubricating oil is:
(1) adopt the fluorographite stripping method to prepare the fluorinated graphene nanometer sheet: 1) to generate fluorographite by carbon and fluorine at 500 ℃ of lower direct reaction, 2) the solvent intercalation processing of fluorographite: the intercalation solvent is N, dinethylformamide (DMF), the 500mg fluorographite is dissolved among the 500ml DMF, reflux 2 hours, 3) suspension liquid that the ultrasonic procedure of fluorographite: with step 2) obtains is 200W at power, ultrasonic frequency is 40HZ, ultrasonic temperature is 25 ℃, ultrasonic time is 6 hours, 4) separation of fluorinated graphene nanometer sheet is dry: the method that adopts high speed centrifugation to separate obtains the fluorinated graphene wet powder, then adopt 60 ℃ of vacuum-dryings to obtain the fluorinated graphene nanometer sheet, the fluorinated graphene that this kind method makes is thicker, thickness 2-20nm with, matter is lighter, and apparent density is 0.05g/cm
3Its transmission electron microscope and atomic force microscope figure are respectively shown in accompanying drawing 3 and accompanying drawing 4; (2) lubricating oil of preparation fluorinated graphene nanometer sheet: the fluorinated graphene nanometer sheet that 1) adopts aforesaid method to obtain progressively adds in the whiteruss, its weight percentage is 1.8%, 2) to said mixture, under 60 ℃ of conditions, at first adopt mechanical stirring, stirred 2 hours, then adopt glue mill technology, glue mill 2 hours obtains uniform and stable lubricating oil.
Body series does not use dispersion agent, and the frictional wear experiment condition embodiment 1 of this lubricating oil is identical.Test result shows, adds the 1.8%(weight percentage) after the fluorinated graphene nanometer sheet, its steel ball mill spot diameter decreased average 51%, rubbing factor reduces by 53%.Recorded the thermal conductivity that contains 2% fluorinated graphene nanometer sheet whiteruss, improved 105% than neat liquid paraffin, thermal conduction capability improves greatly.
Embodiment 4
A kind of high thermal conductivity lubricating oil comprises: weight percentage is 89.7% HVI150SN lubricating oil, and weight percentage is that 10% fluorinated graphene nanometer sheet and weight percentage are 0.3% oleic acid.
The preparation method of this lubricating oil is:
(1) adopt the fluorographite stripping method to prepare the fluorinated graphene nanometer sheet: its preparation process is identical with embodiment 3; (2) lubricating oil of preparation fluorinated graphene nanometer sheet: 1) will adopt fluorinated graphene nanometer sheet that aforesaid method obtains and dispersion agent oleic acid will mix after, progressively add in the HVI150SN lubricant base, wherein, the weight percentage of fluorinated graphene nanometer sheet is 10%, and the weight percentage of dispersion agent is 0.3%.2) to said mixture, under 60 ℃ of conditions, at first high speed machine stirred 30 minutes, and the glue mill is 60 minutes again, can obtain the lubricating oil of stable dispersion.
The frictional wear experiment condition embodiment 1 of this lubricating oil is identical.Test result shows, adds the 10%(weight percentage) after the fluorinated graphene nanometer sheet, its steel ball mill spot diameter decreased average 76%, rubbing factor reduces by 83%.Silk thermal conductance instrument is lacked in employing, has recorded to contain the thermal conductivity that 10% fluorinated graphene nanometer sheet enters the HVI150SN base oil, has improved 223% than neat liquid paraffin, and thermal conduction capability improves greatly.
More than show and described ultimate principle of the present invention, principal character and advantage of the present invention.The technician of the industry should understand; the present invention is not restricted to the described embodiments; that describes in above-described embodiment and the specification sheets just illustrates principle of the present invention; the present invention also has various changes and modifications without departing from the spirit and scope of the present invention, and these changes and improvements all fall in the scope of protection of present invention.The scope of protection of present invention is defined by appending claims and equivalent thereof.
Claims (10)
1. a high thermal conductivity lubricating oil is characterized in that, described lubricating oil comprises: base oil and fluorinated graphene nanometer sheet, wherein the weight percentage of fluorinated graphene nanometer sheet is 0.01%-10.0%.
2. high thermal conductivity lubricating oil according to claim 1 is characterized in that, the weight percentage of described fluorinated graphene nanometer sheet is 0.01%-10.0%, and described lubricating oil comprises that also weight percentage is the dispersion agent of 0.01%-1.0%.
3. high thermal conductivity lubricating oil according to claim 1 and 2 is characterized in that, described base oil is Witco 70 or HVI150SN lubricating oil.
4. high thermal conductivity lubricating oil according to claim 1 and 2, it is characterized in that described dispersion agent is one or more the mixture in polyisobutylene-bis-succinimide, boronation polyisobutene succinimide, isopropyl titanate, sorbitan monooleate, polyoxyethylene glycol, polyvinylpyrrolidone, sodium polyacrylate, stearic acid or the oleic acid.
5. the preparation method of a high thermal conductivity lubricating oil claimed in claim 1 is characterized in that, the method may further comprise the steps:
(1) preparation fluorinated graphene nanometer sheet;
(2) lubricating oil of preparation fluorinated graphene nanometer sheet.
6. the preparation method of high thermal conductivity lubricating oil according to claim 5 is characterized in that, described step (2) comprising:
1) the fluorinated graphene nanometer sheet is progressively joined in the base oil, stir;
2) mixture of step 1) gained homogenized and the gelatinizing processing, obtain uniform and stable lubricating oil.
7. the preparation method of high thermal conductivity lubricating oil according to claim 5 is characterized in that, described step (2) comprising:
1) with after fluorinated graphene nanometer sheet and the dispersant, progressively joins in the base oil, stir;
2) mixture of step 1) gained homogenized and the gelatinizing processing, obtain uniform and stable lubricating oil.
8. according to claim 6 or the preparation method of 7 described high thermal conductivity lubricating oil, it is characterized in that homogenizing in described is operating as the common implementing of a kind of in mechanical stirring or the sonic oscillation or two kinds.
9. according to claim 6 or the preparation method of 7 described high thermal conductivity lubricating oil, it is characterized in that the gelatinizing in described is treated to glue mill technology.
10. the preparation method of high thermal conductivity lubricating oil according to claim 5 is characterized in that, in the step (1), the described method for preparing the fluorinated graphene nanometer sheet is gaseous fluoridizing method or fluorographite stripping method.
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