CN104593130A - Method for preparing graphene water-based lubricating agent in situ - Google Patents
Method for preparing graphene water-based lubricating agent in situ Download PDFInfo
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Abstract
The invention discloses a method for preparing a graphene water-based lubricating agent in situ, belonging to the field of application of graphene serving as a nanometer lubricating additive. The lubricating agent consists of graphene nanoparticles, a surface modifier and purified water. The method comprises the following preparation steps: 1, dissolving a surfactant in deionized water according to a ratio, thereby obtaining a liquid; 2, uniformly dispersing graphene powder in the liquid; 3, performing ultrasonic cavitation treatment on the graphene dispersion liquid; 4, standing the liquid for a certain time, and taking the upper liquid; 5, performing centrifugal separation treatment on the obtained liquid; and 6, collecting the supernatant of the centrifuged liquid, thereby obtaining the water-based lubricating agent containing graphene prepared in situ. The method disclosed by the invention is simple in feasible, and the dispersion stability of the graphene is high. The friction test result proves that according to the extremely small addition amount (0.001-1 percent) of the graphene, the anti-wear and friction reduction properties of the lubricating agent can be greatly improved, and excellent characteristics such as good inherent cooling property, high machinability and environment friendliness of the water-based lubricating agent are not influenced.
Description
Technical field:
The present invention relates to a kind of method that original position prepares Graphene water base lubricant, specifically a kind ofly prepare Graphene at surface-modifying agent aqueous solution situ and be used as the technology of lubricant.Belong to Graphene be used as nanometer lubricating additive answer technical field.
Background technology:
At metal material processing industrial circle, for raising the efficiency and working accuracy, improving quality product, reduce wear, reduce friction, suitable lubricant be selected, be specifically divided into oil type and aq. type two kinds.Both compare, and water base lubricant is widely used because of advantages such as its cooling are good, be applicable to high speed processing conditions, processed surface smoothness is good, environment compatibility is good.But simultaneously due to himself oilness and resistance to abrasion poor, so the occasion of light machining load can only be applicable to.At present, the raising of water base lubricant lubrication and abrasion resistance depends on the content increasing wherein oil in water emulsion, forms emulsion, thus improves the intensity of composite lubricating film, and this will inevitably cause the reduction of the every advantage performance of water base lubricant.Therefore, be necessary to develop novel Water-based Lubricating Additives, allow to, while guarantee water base lubricant special performance, improve its lubrication and abrasion resistance, widen its range of application.
A kind of novel nano-material---Graphene, since being found, with its unique excellent performance such as electricity, calorifics, mechanics, received extensive concern in fields such as material, the energy and electron devices from 2004.It should be noted that Graphene is as conventional lubrication material---the component units of graphite, itself has outstanding lubricating property.The nano-grade size of Graphene in thickness orientation makes it easily in friction process between engaging friction pair, and the laminate structure of uniqueness makes it be easy to be deposited on surface of friction pair, therefore the direct contact on friction member surface is stoped, make friction then occur in be deposited between surperficial Graphene, thus reach the effect reducing friction, reduce wearing and tearing.At present, graphene oxide or redox graphene be a large amount of oxygen-containing functional group because surface exists, and makes it have easy modification and hydrophilic feature, is thus subject to the favor of researchist.Some scientific workers have been had successfully to carry out surface modification to Graphene prepared by oxidation reduction process, and add in lubricating base oil as nanometer additive, enhance antiwear and friction reduction property (J.Phys.D Appl.Phys., 2011 of lubricating oil to a certain extent, 44,205303).On the other hand, also there is researchist to be directly applied to (Carbon, 2013,59,167 – 175) in water base lubricant based on the hydrophilicity of graphene oxide, and achieve certain achievement in research.But graphene oxide and intrinsic Graphene are due to the difference of structure, and character quite has difference.As Water-based Lubricating Additives application aspect, graphene oxide is compared with intrinsic Graphene, have the following disadvantages: 1, surface of graphene oxide exists a large amount of oxygen-containing functional group and presents the pattern of fold, thus its smoothness of the surface is reduced greatly, add the frictional coefficient of interlayer.In contrast, intrinsic graphenic surface is substantially without functional group, and defect level is low, and smooth corrugationless, be beneficial to interformational sliding.Friction force microscope research shows, the frictional coefficient of surface of graphene oxide reaches 7 times more than (Tribol.Lett., 2013,50,137 – 144) of intrinsic Graphene.2, graphene oxide is water-soluble can form colloidal solution, makes the viscosity of lubricant significantly increase, thus can reduce its operability in application scenarios such as mist lubrications (J.Phys.Chem., 2011,115,3410 – 3415).And intrinsic Graphene can obtain excellent lubricant effect with few addition, substantially do not affect the viscosity of water base lubricant.3, preparation technology's relative complex of graphene oxide or redox graphene, the large multipair environment of higher, the used chemical reagent of preparation cost have harm, are difficult to the needs meeting low cost Green synthesis and application.By contrast; intrinsic Graphene can utilize the direct stripping means of liquid phase to carry out preparation in macroscopic quantity now; have the advantage of high-level efficiency, low cost, simple and easy green, easily mass-producing concurrently, this is that intrinsic Graphene provides strong technical support in the application of lubricating area simultaneously.In view of above discussion, necessaryly carrying out the applied research that intrinsic Graphene makes an addition to water base lubricant, is the nanometer lubricating additive of a kind of simple and efficient, environmental protection.
Summary of the invention:
1, object: the object of the present invention is to provide a kind of original position to prepare the method for Graphene water base lubricant, the Graphene that described lubricant is prepared using original position is as slip additive, and dispersion stabilization is good, there is good antiwear and friction reduction property, and preparation method is simple, environmental friendliness, pollution-free.
2, technical scheme: foregoing invention object is achieved by the following technical solutions:
Original position prepares a method for Graphene water base lubricant, and described lubricant is made up of Graphene, surface-modifying agent and pure water, and wherein, Graphene accounts for 0.001% ~ 1% of lubricant total mass.
A kind of original position of the present invention prepares the method for Graphene water base lubricant, and concrete steps are as follows:
Step one: be added in deionized water with predetermined proportion by surface-modifying agent, and strong stirring 2-24 hour, make surface-modifying agent fully soluble in water, obtain the solution for the preparation of water base lubricant;
Step 2: Graphite Powder 99 is added in solution prepared by step one with predetermined proportion, is stirred to it and is uniformly dispersed, obtain graphite dispersing solution;
Step 3: the graphite dispersing solution obtained in step 2 is processed 2-48 hour in ultrasonic cavitation generating unit;
Step 4: by the solution left standstill 12-48 hour after ultrasonic cavitation process in step 3, get upper solution afterwards;
Step 5: be distributed in centrifuge tube by the upper solution obtained in step 4, carries out centrifuging treatment, and centrifugal rotational speed is 500 revs/min to 5000 revs/min (centrifugal acceleration 35g to 3555g); The centrifugal treating time is 30 minutes to 180 minutes.
Step 6: to the solution after centrifugal treating in step 5, gets its supernatant liquid, namely obtains the water base lubricant of graphene-containing.
Wherein, surface-modifying agent described in step one refers to the one in following listed properties-correcting agent: Triton X-100 (polyoxyethylene octyl phenyl ether), sodium lauryl sulphate, Sodium dodecylbenzene sulfonate, lithium dodecyl sulfate, Sodium cholic acid, sodium taurodeoxycholate, cetyl trimethylammonium bromide, polyoxyethylenes (40) nonylplenyl ether, Tween 80 (sorbitan monooleate Soxylat A 25-7) etc., in solution, the best in quality ratio of surface-modifying agent is 0.01%-1%.
Wherein, in step one, deionized water used also can be common pure water, distilled water etc.
Wherein, the Graphite Powder 99 described in step 2 is that granularity is less than 325 object natural flake graphites.
Wherein, the mass ratio adding Graphite Powder 99 and solution described in step 2 is 0.1%-10%.
Wherein, ultrasonic cavitation process described in step 3 is that graphite dispersing solution is loaded Erlenmeyer flask (but being not limited to Erlenmeyer flask), then be bathed in the container (filling water in advance in container) of ultrasonic cavitation generating unit and carried out ultrasonic cavitation process, treatment time is 2-48 hour, and period keeps water temperature in container lower than 40 DEG C by hydronic mode.
3, beneficial effect
(1) prepare the preparation technology of Graphene water base lubricant and method is very simple at surface-modifying agent aqueous solution situ, be easy to laboratory and suitability for industrialized production realizes.
(2), in the water base lubricant that prepared by the method, the dispersion stabilization of Graphene is fine.This is because in ultrasonic cavitation process, surface modification agent molecule carries out effectively coated to peeling off the graphene sheet layer produced, thus prevents it to reunite and sedimentation.
(3) water base lubricant of graphene-containing has splendid antiwear and friction reduction property, and compared with the lubricant adding Graphene with nothing, frictional coefficient sharply reduces, and abrasion loss significantly reduces.This is due in friction process; the laminated structure of Graphene and the nano-grade size of thickness direction make it easily enter between friction pair and are deposited on friction member surface to form protective membrane; and then the direct contact avoided between friction member; friction is mainly occurred between graphene sheet layer; thus improve the supporting capacity of friction pair, simultaneously also make frictional coefficient obviously reduce and more stable.
(4) in the water base lubricant prepared of the method, the content of Graphene is little, therefore while raising lubricant antiwear and friction reduction property, also maintains the intrinsic advantage of water base lubricant, as good in cooling, good processability, pollution-free etc.
Accompanying drawing explanation
The standing sedimentation curve of Fig. 1 graphene-containing water base lubricant prepared by embodiment 1 ~ 3, left side ordinate zou is the absorbance measurement of lubricant, and right side ordinate zou is corresponding Graphene concentration, and X-coordinate is time of repose.
Fig. 2 is for graphene-containing water base lubricant described in embodiment 1 ~ 3 and without the friction coefficient curve figure adding Graphene lubricant (only moisture and surface-modifying agent); Wherein, 0.000%-is without adding Graphene lubricant, 0.002%-embodiment 1,0.007%-embodiment 2,0.011%-embodiment 3; 2N and 15N refers to different experiment loads.
Fig. 3 is for graphene-containing water base lubricant described in embodiment 1 ~ 3 and without the steel ball mill spot diameter histogram adding Graphene lubricant (only moisture and surface-modifying agent); Wherein, 0.000%-is without adding Graphene lubricant, 0.002%-embodiment 1,0.007%-embodiment 2,0.011%-embodiment 3; 2N and 15N refers to different experiment loads.
Fig. 4 a is experiment load 2N, when in lubricant, Graphene content is 0.000%, and steel ball mill spot optical microscope picture after frictional experiment;
Fig. 4 b is experiment load 2N, when in lubricant, Graphene content is 0.000%, and steel disk cut optical microscope picture after frictional experiment;
Fig. 4 c is experiment load 2N, when in lubricant, Graphene content is 0.000%, and the scanning electron microscopic picture of steel disk cut after frictional experiment;
Fig. 4 d is experiment load 2N, when in lubricant, Graphene content is 0.000%, and the 3D skeleton diagram of steel disk cut after frictional experiment;
Fig. 4 e is experiment load 2N, when in lubricant, Graphene content is 0.000%, and the cross section profile figure of steel disk cut after frictional experiment.
Fig. 5 a is when in experiment load 2N lubricant, Graphene content is 0.011% (embodiment 3), steel ball mill spot optical microscope picture after frictional experiment;
Fig. 5 b is when in experiment load 2N lubricant, Graphene content is 0.011% (embodiment 3), steel disk cut optical microscope picture after frictional experiment;
Fig. 5 c is when in experiment load 2N lubricant, Graphene content is 0.011% (embodiment 3), the scanning electron microscopic picture of steel disk cut after frictional experiment;
Fig. 5 d is when in experiment load 2N lubricant, Graphene content is 0.011% (embodiment 3), the scanning electron microscopic picture of steel disk cut after frictional experiment;
Fig. 5 e is when in experiment load 2N lubricant, Graphene content is 0.011% (embodiment 3), the cross section profile figure of steel disk cut after frictional experiment.
Fig. 6 is FB(flow block) of the present invention.
Embodiment:
Below in conjunction with the drawings and specific embodiments in detail the present invention is described in detail, but is not limited thereto.
See Fig. 6, the present invention, a kind of original position prepares the method for Graphene water base lubricant, and the method concrete steps are as follows:
Embodiment 1
Step one: take 0.3g surface-modifying agent Triton X-100, add in 300mL deionized water, strong stirring 12 hours, makes surface-modifying agent fully soluble in water, obtains the solution (Triton X-100 mass ratio is 0.1%) for the preparation of water base lubricant;
Step 2: take 1.5g Graphite Powder 99 (granularity is less than 325 orders) and add in the solution of preparation, be stirred to it and be uniformly dispersed, obtain graphite dispersing solution (Graphite Powder 99 mass ratio 0.5%), and loaded in the Erlenmeyer flask with lid;
Step 3: be bathed in by the Erlenmeyer flask that graphite dispersing solution is housed in the container (filling water in advance) of ultrasonic cavitation generating unit, carries out ultrasonic cavitation process 8 hours, and period keeps water temperature in container lower than 40 DEG C by hydronic mode; Ultrasonic cavitation generating unit power is 120W, frequency 40KHz;
Step 4: after supersound process, leaves standstill 12 hours by the Erlenmeyer flask filling graphite dispersing solution, takes out upper solution afterwards;
Step 5: be distributed in centrifuge tube by the upper solution of taking-up, puts into whizzer and carries out centrifuging treatment; Centrifugal rotational speed is 1500rpm (317g), and centrifugation time is 1 hour;
Step 6: after centrifugal treating, collects the supernatant liquid of solution, namely obtains the water base lubricant of graphene-containing; By measuring its absorbancy (being directly proportional to the concentration of Graphene), determine that the content of Graphene is 23.8 μ g/mL (~ 0.002%).
Embodiment 2
Step one: take 0.3g surface-modifying agent Triton X-100, add in 300mL deionized water, strong stirring 12 hours, makes surface-modifying agent fully soluble in water, obtains the solution (Triton X-100 mass ratio is 0.1%) for the preparation of water base lubricant;
Step 2: take 3g Graphite Powder 99 (granularity is less than 325 orders) and add in the solution of preparation, be stirred to it and be uniformly dispersed, obtain graphite dispersing solution (Graphite Powder 99 mass ratio 1%), and loaded in the Erlenmeyer flask with lid;
Step 3: be bathed in by the Erlenmeyer flask that graphite dispersing solution is housed in the container (filling water in advance) of ultrasonic cavitation generating unit, carries out ultrasonic cavitation process 8 hours, and period keeps water temperature in container lower than 40 DEG C by hydronic mode; Ultrasonic cavitation generating unit power is 120W, frequency 40KHz;
Step 4: after supersound process, leaves standstill 12 hours by the Erlenmeyer flask filling graphite dispersing solution, takes out upper solution afterwards;
Step 5: be distributed in centrifuge tube by the upper solution of taking-up, puts into whizzer and carries out centrifuging treatment; Centrifugal rotational speed is 1500rpm (317g), and centrifugation time is 1 hour;
Step 6: after centrifugal treating, collects the supernatant liquid of solution, namely obtains the water base lubricant of graphene-containing; By measuring its absorbancy (being directly proportional to the concentration of Graphene), determine that the content of Graphene is 69.9 μ g/mL (~ 0.007%).
Embodiment 3
Step one: take 0.3g surface-modifying agent Triton X-100, add in 300mL deionized water, strong stirring 12 hours, makes surface-modifying agent fully soluble in water, obtains the solution (Triton X-100 mass ratio is 0.1%) for the preparation of water base lubricant;
Step 2: take 6g Graphite Powder 99 (granularity is less than 325 orders) and add in the solution of preparation, be stirred to it and be uniformly dispersed, obtain graphite dispersing solution (Graphite Powder 99 mass ratio 2%), and loaded in the Erlenmeyer flask with lid;
Step 3: be bathed in by the Erlenmeyer flask that graphite dispersing solution is housed in the container (filling water in advance) of ultrasonic cavitation generating unit, carries out ultrasonic cavitation process 8 hours, and period keeps water temperature in container lower than 40 DEG C by hydronic mode; Ultrasonic cavitation generating unit power is 120W, frequency 40KHz;
Step 4: after supersound process, leaves standstill 12 hours by the Erlenmeyer flask filling graphite dispersing solution, takes out upper solution afterwards;
Step 5: be distributed in centrifuge tube by the upper solution of taking-up, puts into whizzer and carries out centrifuging treatment; Centrifugal rotational speed is 1500rpm (317g), and centrifugation time is 1 hour;
Step 6: after centrifugal treating, collects the supernatant liquid of solution, namely obtains the water base lubricant of graphene-containing; By measuring its absorbancy (being directly proportional to the concentration of Graphene), determine that the content of Graphene is 110 μ g/mL (~ 0.011%).
In embodiment 1 ~ 3, prepared frictional characteristics of lubricant adopts UMT-3 type tester for friction between to detect, friction type is that (material of ball, dish is GCr15 to steel ball-steel disk, steel ball size is 9.53mm) rotary friction, experimental result is as shown in Figure 2-5.Frictional experiment condition is: rotation radius 5mm, rotating speed 120r/m, experiment load 2N/15N, rub cycle number of times are 2000 times.The standing sedimentation curve of Fig. 1 graphene-containing water base lubricant prepared by embodiment 1 ~ 3.
Fig. 2 shows the friction coefficient curve figure of water base lubricant under different experiments load that in each embodiment, Graphene content is different.Compared with the lubricant (0.000%) adding Graphene with nothing, the lubricant of graphene-containing makes frictional coefficient all significantly reduce.When low year (2N), the highest reduction by 76.6% (0.449 → 0.105, embodiment 3) of average friction coefficient; When height carries (15N), average friction coefficient reducing amount is 50% (0.366 → 0.183, embodiment 3).This illustrates under height condition of loading, and the interpolation of Graphene all effectively can improve the lubricity of lubricant.
Fig. 3 shows water base lubricant steel ball mill spot diameter histogram under different experiments load that in each embodiment, Graphene content is different.Compared with the lubricant (0.000%) adding Graphene with nothing, the lubricant of graphene-containing makes abrasion loss obviously reduce.When low year (2N), the highest reduction by 61.7% (511.3 → 196 μm, embodiment 3) of steel ball mill spot diameter; When height carries (15N), steel ball mill spot diameter reducing amount is 18.4% (682.1 → 556.3 μm, embodiment 3).This illustrates under height condition of loading, and the interpolation of Graphene all effectively can improve the wear resistance of lubricant.
When Fig. 4 a-e and Fig. 5 a-e is respectively experiment load 2N, under being 0.011% (embodiment 3) lubricant condition without interpolation Graphene (0.000%) and Graphene content, the microscopic sdIBM-2+2q.p.approach of surface of friction pair after frictional experiment.(a, b), can intuitively find out, under graphene-containing lubricant lubricating condition, the abrasion loss of ball-dish friction pair significantly reduces contrast optical microscope picture; As can be seen from electron microscopic picture (c) and surperficial 3D (d) and 1D (e) skeleton diagram, under graphene-containing lubricant lubricating condition, surface of friction pair is more smooth, and ditch dug with a plow obviously shoals.Reach a conclusion thus, the interpolation of Graphene effectively can improve friction pair wearing and tearing and surfaceness situation thereof.
Obviously, above-mentioned case study on implementation of the present invention is only used to clearly demonstrate example of the present invention, and the restriction not to embodiments of the present invention.For the those of ordinary skill in described field, other multi-form change or variations can also be made on the basis of the above description.Here cannot give exhaustive to all embodiments, every belong to technical scheme of the present invention the apparent change of amplifying out or variation be still in the row of protection scope of the present invention.
Claims (6)
1. original position prepares a method for Graphene water base lubricant, it is characterized in that: described lubricant is made up of Graphene, surface-modifying agent and pure water, and Graphene accounts for 0.001% ~ 1% of lubricant total mass; The method concrete steps are as follows:
Step one: be added in deionized water with predetermined proportion by surface-modifying agent, and strong stirring 2-24 hour, make surface-modifying agent fully soluble in water, obtain the solution for the preparation of water base lubricant;
Step 2: Graphite Powder 99 is added in solution prepared by step one with predetermined proportion, is stirred to it and is uniformly dispersed, obtain graphite dispersing solution;
Step 3: the graphite dispersing solution obtained in step 2 is processed 2-48 hour in ultrasonic cavitation generating unit;
Step 4: by the solution left standstill 12-48 hour after ultrasonic cavitation process in step 3, get upper solution afterwards;
Step 5: be distributed in centrifuge tube by the upper solution obtained in step 4, carries out centrifuging treatment, and centrifugal rotational speed is 500 revs/min to 5000 revs/min, centrifugal acceleration 35g to 3555g; The centrifugal treating time is 30 minutes to 180 minutes;
Step 6: to the solution after centrifugal treating in step 5, gets its supernatant liquid, namely obtains the water base lubricant of graphene-containing.
2. a kind of original position according to claim prepares the method for Graphene water base lubricant, it is characterized in that: the surface-modifying agent described in step one refers to the one in following listed properties-correcting agent: polyoxyethylene octyl phenyl ether Triton X-100, sodium lauryl sulphate, Sodium dodecylbenzene sulfonate, lithium dodecyl sulfate, Sodium cholic acid, sodium taurodeoxycholate, cetyl trimethylammonium bromide, polyoxyethylenes (40) nonylplenyl ether, sorbitan monooleate Soxylat A 25-7 Tween 80, in solution, the best in quality ratio of surface-modifying agent is 0.01%-1%.
3. a kind of original position according to claim prepares the method for Graphene water base lubricant, it is characterized in that: in step one, deionized water used also can be common pure water, distilled water.
4. a kind of original position according to claim prepares the method for Graphene water base lubricant, it is characterized in that: the Graphite Powder 99 described in step 2 is that granularity is less than 325 object natural flake graphites.
5. a kind of original position according to claim prepares the method for Graphene water base lubricant, it is characterized in that: the mass ratio adding Graphite Powder 99 and solution described in step 2 is 0.1%-10%.
6. a kind of original position according to claim prepares the method for Graphene water base lubricant, it is characterized in that: the ultrasonic cavitation process described in step 3 is that graphite dispersing solution is loaded Erlenmeyer flask, then be bathed in ultrasonic cavitation generating unit to fill in advance in the container of water and carry out ultrasonic cavitation process, treatment time is 2-48 hour, and period keeps water temperature in container lower than 40 DEG C by hydronic mode.
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