CN102911762B - 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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- CN102911762B CN102911762B CN201210434814.7A CN201210434814A CN102911762B CN 102911762 B CN102911762 B CN 102911762B CN 201210434814 A CN201210434814 A CN 201210434814A CN 102911762 B CN102911762 B CN 102911762B
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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 one and there is high thermal conduction characteristic lubricating oil and preparation method thereof, belong to the preparation field of machinery or aerospace 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, has larger pressure between friction pair, will produce high temperature in friction process simultaneously.High Temperature High Pressure produces larger impact by the physico-chemical property on lubricating oil.In order to make up the defect of lubricating oil, conventionally 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 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 due to combination between layers a little less than, when being subject to External Force Acting, just easily between parallel layers, dividing and come, namely shear strength is between layers lower, 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 current developments and prospect [J]. lubricated and sealing, 2006,175 (3): 181-18].The part but these interpolation materials come with some shortcomings, 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 lubricating oil is larger, thus often need to add too much dispersion agent, so that stable system; and too much the adding of dispersion agent; easily make lubricating oil generation emulsification and rotten [Wang Xiaobo, graphite lubricating oil (GLO), Chinese Patent Application No.: 01135108.X; Zhang Ruchun, graphite lubricating oil (GLO) and preparation method thereof, Chinese Patent Application No.: 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 good reduction friction and the effect that reduces wear, more requires the life-time service that lubricating oil can be under extreme conditions.Lubricating oil must play cooling thermal discharge effect, and the heat that lubricating oil produces while only having mechanical friction is taken away, and keeps certain thermal equilibrium state, could effectively prevent 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 consists of organism, thermal conductivity is low especially.This just causes the cooling thermal discharge effect of lubricating oil not obvious, makes the temperature of lubricating oil and friction pair all very high.This on the one hand, can make friction pair more easy to wear, more makes lubricating oil at high temperature perishable, and 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 object of the invention is to overcome the defect of existing lubricating oil, a kind of lubricating oil with high thermal conductivity is provided.
For realizing object 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 also comprises that 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 oleic acid.
Another object of the present invention is to provide a kind of preparation method of high thermal conductivity lubricating oil, and the method comprises the following steps:
(1) prepare fluorinated graphene nanometer sheet;
(2) prepare the lubricating oil of fluorinated graphene nanometer sheet.
In a preferred embodiment of the present invention, described step (2) comprising:
1) fluorinated graphene nanometer sheet is progressively joined in base oil, stir;
2) mixture of step 1) gained is homogenized and gelatinizing processing, obtain uniform and stable lubricating oil.
In a preferred embodiment of the present invention, described step (2) comprising:
1) by after fluorinated graphene nanometer sheet and dispersant, progressively join in base oil, stir;
2) mixture of step 1) gained is homogenized and 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 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 step (1), the described method of preparing 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: compared with not additivated basic grease, can make wear scar diameter decreased average more than 50%, rubbing factor reduces more than 60%, also has good supporting capacity simultaneously; This gives the credit to the unique texture of fluorinated graphene.As everyone knows, Graphene be by carbon atom by the hexagonal lattice carbon simple substance forming of neatly arranging, structure is highly stable.Graphene and associated materials thereof be due to its excellent electricity, calorifics and mechanical property, caused the extensive concern of community of physicists, material educational circles.Fluorinated graphene nanometer sheet has and the similar structure and characteristics of graphene nanometer sheet.Fluorinated graphene nanometer sheet is keeping the original laminate structure of graphite, but because fluorine enters between graphene layer, and between graphene layer, electronics forms covalent linkage, and the bond energy between graphene layer significantly reduces, be only 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 be offset from outside pressure, meanwhile, outside harsh atmosphere and temperature are difficult for making firmly F-C key to disconnect.2) very high thermal conduction capability: thermal conductivity ratio base oil is enhanced about more than once; 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 dispersiveness: 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 base oil, even if 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 significantly emulsion of nothing under high temperature lubricating situation, thoroughly solved the immiscible problem of lubricating oil additive and base oil.Therefore, the lubricating oil that contains fluorinated graphene nanometer sheet of the present invention, when having good antiwear and antifriction effect, has higher thermal conductivity, the heat producing can be removed in time in friction process.
Accompanying drawing explanation
Fig. 1 is the transmission electron microscope picture that gaseous fluoridizing method is prepared fluorinated graphene nanometer sheet.
Fig. 2 is the atomic force microscope figure that gaseous fluoridizing method is prepared fluorinated graphene nanometer sheet.
Fig. 3 is the transmission electron microscope picture that fluorographite stripping method is prepared fluorinated graphene nanometer sheet.
Fig. 4 is the atomic force microscope figure that fluorographite stripping method is prepared fluorinated graphene nanometer sheet.
Embodiment
Below by embodiment, further illustrate the present invention.
Embodiment 1
A kind of high thermal conductivity lubricating oil, comprising: the fluorinated graphene nanometer sheet that the Witco 70 that weight percentage is 98% and weight percentage are 2%.
The preparation method of this lubricating oil is:
(1) gaseous fluoridizing method is prepared fluorinated graphene nanometer sheet: 1) prepare graphite oxide: in ice bath, 10g Graphite Powder 99 and 5g SODIUMNITRATE are mixed with the 230mL vitriol oil, slowly add 30gKMn0 in stirring
4, transfer them in 35 ° of C water-baths and react 30 minutes, more progressively add 460mL deionized water, continue reaction 40 minutes after temperature rises to 98 ℃, mixture becomes glassy yellow by brown, further thin up, and the H that is 30% with weight fraction
20
2solution-treated, neutralize unreacted permanganic acid, centrifuging repetitive scrubbing filter cake, finally its vacuum-drying obtained to graphite oxide, 2) prepare 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) obtain Graphene, 3) prepare 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, after being purified, with stainless steel tube, introduce and be equipped with in the tube furnace reactor of Graphene, 500 ° of C of temperature of reaction, react after 15 hours, stop passing into and heating of fluorine gas, pass into nitrogen protection and cooling, can make fluorinated graphene.The fluorinated graphene that this kind of method makes is thinner, between 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) prepare the lubricating oil of fluorinated graphene nanometer sheet: 1) the fluorinated graphene nanometer sheet that adopts described method to obtain is progressively added in whiteruss, its weight percentage is 2.0%, 2) to said mixture, under 60 ℃ of conditions, first adopt mechanical stirring, stir 2 hours, then adopt glue mill technology, glue mill 2 hours, obtains uniform and stable lubricating oil.
Body series is not used dispersion agent, on the MRS-10A type four-ball friction and wear test machine that the frictional wear experiment of this lubricating oil is manufactured in Jinan trier factory, carries out, and the steel ball using is 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, adds after 2% fluorinated graphene nanometer sheet, and its steel ball mill spot diameter decreased average 52%, rubbing factor reduces by 62%.Adopt short silk thermal conductance instrument, recorded containing 2.0%(weight percentage) the thermal conductivity of fluorinated graphene nanometer sheet whiteruss, than neat liquid paraffin, improved 116%, thermal conduction capability improves greatly.
Embodiment 2
A kind of high thermal conductivity lubricating oil, comprising: the HVI150SN lubricating oil that weight percentage is 94.95%, the sorbitan monooleate tween 80 that the fluorinated graphene nanometer sheet that weight percentage is 5% and weight percentage are 0.05%.
The preparation method of this lubricating oil is:
(1) gaseous fluoridizing method is prepared fluorinated graphene nanometer sheet: its preparation process is identical with embodiment 1; (2) prepare the lubricating oil of fluorinated graphene nanometer sheet: after 1) the fluorinated graphene nanometer sheet that adopts described method to obtain being mixed with oil-soluble dispersant sorbitan monooleate tween 80, progressively add in HVI150SN lubricant base, 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, first high speed machine stirs 30 minutes, more ultrasonic 30 minutes, 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, adds after 5% fluorinated graphene nanometer sheet, and its steel ball mill spot diameter decreased average 65%, rubbing factor reduces by 79%.Adopting short silk thermal conductance instrument, recorded containing 5%(weight percentage) fluorinated graphene nanometer sheet enters the thermal conductivity of HVI150SN base oil, than neat liquid paraffin, improved 186%, and thermal conduction capability improves greatly.
Embodiment 3
A kind of high thermal conductivity lubricating oil, comprising: the fluorinated graphene nanometer sheet that the Witco 70 that weight percentage is 98.2% and weight percentage are 1.8%.
The preparation method of this lubricating oil is:
(1) adopt fluorographite stripping method to prepare fluorinated graphene nanometer sheet: 1) direct reaction at 500 ℃ generates fluorographite by carbon and fluorine, 2) the solvent intercalation processing of fluorographite: intercalation solvent is N, dinethylformamide (DMF), 500mg fluorographite is dissolved in 500ml DMF, reflux 2 hours, 3) ultrasonic procedure of fluorographite: by step 2) suspension liquid that 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: adopt the method that high speed centrifugation separates to obtain fluorinated graphene wet powder, then adopt 60 ℃ of vacuum-dryings to obtain fluorinated graphene nanometer sheet, the fluorinated graphene that this kind of method makes is thicker, thickness 2-20nm with, matter is lighter, apparent density is 0.05g/cm
3.Its transmission electron microscope and atomic force microscope figure are respectively as shown in accompanying drawing 3 and accompanying drawing 4; (2) prepare the lubricating oil of fluorinated graphene nanometer sheet: the fluorinated graphene nanometer sheet that 1) adopts aforesaid method to obtain progressively adds in whiteruss, its weight percentage is 1.8%, 2) to said mixture, under 60 ℃ of conditions, first adopt mechanical stirring, stir 2 hours, then adopt glue mill technology, glue mill 2 hours, obtains uniform and stable lubricating oil.
Body series is not used dispersion agent, and the frictional wear experiment condition embodiment 1 of this lubricating oil is identical.Test result shows, adds 1.8%(weight percentage) after fluorinated graphene nanometer sheet, its steel ball mill spot diameter decreased average 51%, rubbing factor reduces by 53%.Recorded the thermal conductivity containing 2% fluorinated graphene nanometer sheet whiteruss, than neat liquid paraffin, improved 105%, thermal conduction capability improves greatly.
Embodiment 4
A kind of high thermal conductivity lubricating oil, comprising: the HVI150SN lubricating oil that weight percentage is 89.7%, the oleic acid that the fluorinated graphene nanometer sheet that weight percentage is 10% and weight percentage are 0.3%.
The preparation method of this lubricating oil is:
(1) adopt fluorographite stripping method to prepare fluorinated graphene nanometer sheet: its preparation process is identical with embodiment 3; (2) prepare the lubricating oil of fluorinated graphene nanometer sheet: after 1) the fluorinated graphene nanometer sheet that adopts aforesaid method to obtain being mixed with dispersion agent oleic acid, progressively add in 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, first high speed machine stirring 30 minutes, then glue is ground 60 minutes, 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 10%(weight percentage) after fluorinated graphene nanometer sheet, its steel ball mill spot diameter decreased average 76%, rubbing factor reduces by 83%.Adopt short silk thermal conductance instrument, recorded the thermal conductivity that enters HVI150SN base oil containing 10% fluorinated graphene nanometer sheet, than neat liquid paraffin, improved 223%, 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 in above-described embodiment and specification sheets, describes 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 (1)
1. a high thermal conductivity lubricating oil, is characterized in that, comprising: the HVI150SN lubricating oil that weight percentage is 89.7%, the oleic acid that the fluorinated graphene nanometer sheet that weight percentage is 10% and weight percentage are 0.3%;
The preparation method of this lubricating oil is:
1) adopt fluorographite stripping method to prepare fluorinated graphene nanometer sheet:
1.1) by carbon and fluorine, direct reaction at 500 ℃ generates fluorographite;
1.2) the solvent intercalation processing of fluorographite: intercalation solvent DMF (DMF), is dissolved in 500mg fluorographite in 500ml DMF reflux 2 hours;
1.3) ultrasonic procedure of fluorographite: by step 1.2) suspension liquid that obtains is 200W at power, and ultrasonic frequency is 40Hz, and ultrasonic temperature is 25 ℃, and ultrasonic time is 6 hours;
1.4) separation of fluorinated graphene nanometer sheet is dry: adopt the method that high speed centrifugation separates to obtain fluorinated graphene wet powder, then adopt 60 ℃ of vacuum-dryings to obtain fluorinated graphene nanometer sheet; The fluorinated graphene thickness making is at 2-20nm, and apparent density is 0.05g/cm
3;
2) prepare the lubricating oil of fluorinated graphene nanometer sheet:
2.1) after the fluorinated graphene nanometer sheet that adopts aforesaid method to obtain is mixed with oleic acid, progressively add in HVI150SN lubricant base;
2.2), to said mixture, under 60 ℃ of conditions, first high speed machine stirring 30 minutes, then glue is ground 60 minutes, can obtain the lubricating oil of stable dispersion.
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