CN101787321A - Micro-nano mineral grain lubricating additive with self-repairing function, lubricating oil and production method - Google Patents
Micro-nano mineral grain lubricating additive with self-repairing function, lubricating oil and production method Download PDFInfo
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Abstract
The invention discloses a micro-nano mineral grain lubricating additive with self-repairing function, lubricating oil and a production method. The method comprises the following steps: preparing nano MgO grains by adopting a sol-gel method respectively; modifying the grains by adopting oleic acid as surface modification agent; and mixing the grains and the base lubricating oil according to a certain proportion to form a lubricating agent which contains the micro-nano mineral grain lubricating additive and has the self-repairing function. When a mechanical metal part rubbing pair works, the additive material in the lubricating agent and the iron-based metal on the rubbing surface undergo physical and chemical reactions so as to continually generate compact iron-based silicate metal ceramic layers, partially or totally recover the size of the abraded part and finish self-repairing of the abraded part in the running dynamic process of the parts. Compared with the base lubricating oil, the lubricating agent can remarkably prolong the service life of the parts, improve the rubbing surface hardness and finishment, and greatly reduce the friction coefficient.
Description
Technical field
The present invention relates to a kind of lubricating oil additive and compounding process thereof, belong to the power lubrication technical field with antifriction antiwear and self-repair function.
Background technology
Recent study shows, in some nanometer particles or nanoparticle and dispersion stabilizer adding lubricating oil thereof of modifying, the extreme pressure property of lubricating oil is improved a lot.Russia utilizes Nano diamond to produce the trade mark as lubricating oil additive to be N-50A break-in lubricant, and Ukraine academy of sciences has also developed similar lubricant, and the trade mark is M5-20 and M5-21, is specifically designed to internal combustion engine running-in.Use these product that seating time is shortened, fuel economy prolongs engine life.If be used for the lubricated of precision finishing machine, then can reduce with oil 50%.The king of China shows that moral synthesized senior lubricant with Nano graphite powder as additive, and has applied for patent of invention.Yu Zhimin adopts Nano metal powder, oxidation inhibitor and solvent to make a kind of lubricating repairing agent of nanometer metal micropowder through certain processing condition.The Nano metal powder that uses comprises pure nickel and the fine copper micro mist of 10-100nm, and the lubricating repairing agent that makes has the lubricated and repair efficiency of maintenance to automobile engine cylinder.Xia Yanqiu etc. are added to 10-50nm copper powder, nickel powder, glass putty and bismuth meal respectively in the base oil, carry out the antiwear and friction reduction property test.Test shows that under equal conditions its frictional coefficient reduces, and the polishing scratch width diminishes, and improves the anti-extreme pressure energy of lubricating oil.Lubricating oil and conventional lubrication oil that additive is done with nano metal by Michigan, United States university have carried out the contrast experiment, the result shows, the lubricating oil that nano metal is done additive obviously reduces camshaft and wear of piston-rings, and reduced surface friction, thereby the reduction oil consumption has guaranteed the safe operation of gasoline, diesel machine.The lubricating oil research and development centre of CNPC and the Lanzhou Chemistry and Physics Institute of the Chinese Academy of Sciences have developed a kind of nanometer copper additives.Use shows, this additive is added in the automobile engine oil, can obviously reduce the starting current of engine and increase cylinder pressure.After for some time is used in this agent, can form layer protecting film at cylinder sleeve and piston ring surface.But above-mentioned materials does not all possess self-repair function.
On the other hand, for improving the work-ing life of mechanical component friction pair, propose a kind of galling self-repair technology by The former Russian scholar the seventies in 20th century.This self-repair technology is meant that adopting metal or nonmetal fine particle to add in oil product and the lubricating grease uses, and generates the selfreparing protective film under the frictional wear condition on machinery part surface.The self-repair material of current extensive concern is that main component is that serpentine (hydroxyl magnesium silicate) is the lubricating oil additive that main multiple complex component constitutes.In view of serpentine complicated component and uncertain, so the replacement(metathesis)reaction that causes mineral grain in the lubricant medium and metallic surface whether to have self-repair function depends on various procedures and condition in the friction process, therefore the stable inadequately phenomenon of actual effect of its application appears.
But so far about adopting nano-MgO one class fine inorganic material to prepare additive, make lubricant have above-mentioned two specific characters concurrently, the characteristics that promptly both had the wear resistant friction reducing of nanometer lubricating additive, the lubricating oil adding technique that has the mineralogical composition self-repair function does not again appear in the newspapers as yet.
Summary of the invention
The purpose of patent of the present invention is the characteristics of a kind of wear resistant friction reducing with nanometer lubricating additive of preparation, the lubricating oil additive that has the mineralogical composition self-repair function again, make the metal mechanical component be in operation to reduce frictional force, alleviate wearing and tearing, and can realize the wearing and tearing selfreparing, and actual effect is stable, with the work-ing life of significant prolongation part.
The invention provides a kind of micro-nano mineral grain lubricating additive with self-repair function, is that the lipophilic degree through finishing is 60.98%, and median size is 45-55nm, particle be shaped as spheric nano-MgO powder.
The also claimed a kind of lubricating oil that contains micro-nano mineral grain lubricating additive of the present invention with self-repair function; it comprises the nano-MgO powder of 0.1%-1.0%; described nano-MgO powder is through finishing; lipophilic degree is 60.98%; the MgO median size is 45-55nm, particle be shaped as sphere.
The also claimed a kind of preparation method with micro-nano mineral grain lubricating additive of self-repair function of the present invention may further comprise the steps:
1) the preparation median size is 45-55nm, particle be shaped as spheric nano-MgO powder;
2) finishing get contain oleic acid 0.5-1.5% 95% ethanolic soln as modifier, the modification condition stirs in the constant temperature 50-60 ℃ oil bath for the two is blended in, the back naturally cooling that reacts completely, again through suction filtration, be drying to obtain.
Described modifier concentration 1.0%; Modify 55 ℃ of temperature; During modification time 3h, modification effect the best.
The preparation median size is 45-55nm in the described step 1), and the prior art that the step that is shaped as spheric nano-MgO powder of particle can adopt any those skilled in the art to know prepares, example method as described in example 1 above.The method described in reference [1], [2], [3] for example again.
Beneficial effect of the present invention is:
1, compare with common nano particle slip additive, nano-MgO particulate lubricating oil additive not only possesses good antiwear and friction reduction property, and good self-repair function is arranged; Compare with the selfreparing slip additive based on hydroxyl magnesium silicate, it can play the nano lubricating effect that the latter does not have.
2, the MgO microparticle surfaces is modified, the nano-MgO particulate is added on prevents agglomeration in the lubricating oil; Strengthen the interface compatibility of nano-powder in medium, and dodge under the operating mode of temperature in certain surface contact and friction generation when nanoparticle, desired replacement(metathesis)reaction takes place in the ferrous metals that finishing does not influence on nano-MgO particulate and the surface of friction.
3, under the operating mode that the surface contacts and the generation sudden strain of a muscle that rubs is warm, make that ferrous metals generation thermochemistry and the power chemical replacement on nano-MgO particulate and the surface of friction reacted, formation is stablized and uniform ferrosilicate ceramic layer, plays self-repair function.
At the nano-MgO particle under high loading, because the nano-MgO surface of dissociating out exists a large amount of dangling bondss and defect structure, have high chemically reactive and high diffusibility, make the magnesium atom in the particulate crystal and the iron atom generation replacement(metathesis)reaction of metal surface, generate the new crystal of ferrosilicate at friction surface.In friction process, new crystal constantly increases at friction surface, has finally formed the protective layer that becomes the chemical bond combination with ferrous metals, and this layer nanometer layer filled surface concave and tiny crack, plays the repair to wear surface.The formation speed of protective layer is relevant with the energy that friction discharges with thickness, but self-regulating: when wearing and tearing took place, frictional energy increased, and the complex series of reactions that MgO and surface of friction pair take place begins to carry out, and protective film begins growth simultaneously; And when polishing scratch obtained to repair, the frictional energy that intermetallic discharges reduced, and the series reaction of MgO and surface of friction pair will stop, and protective film also just no longer thickens.Therefore, the position that renovation agent particulate generation chemical reaction generates protective layer is selectively, and it only takes place on the position of galling.This self-repair function is that other common metal or nonmetal nanometer additive are not available.
Figure of description
Fig. 1 is the pattern of 4012 marine lubricants following sample behind 500N load, friction 8h;
Fig. 2 is the 4012 marine lubricants pattern of sample down behind 500N load, friction 8h that contains 0.4% nanometer .MgO particulate.
Embodiment
Embodiment 1
1) preparation nano-MgO powder:
Get 9.4gMgCl
26H
2O, 35ml ethylene glycol and a small amount of polyvinylpyrrolidone (PVP) add in the beaker of 100mL, fully stir with magnetic force heater heats agitator, and just it forms polymers soln.In whipping process, slowly drip dense NH
3H
2O produces the oyster white colloid, continues to stir 10min, and it is fully reacted.Slurry is placed 5h, and centrifugation is also used absolute ethanol washing, in 80 ℃ of dryings, with 450 ℃ of calcination 3h, obtains pale powder in retort furnace.Prepared MgO powder is carried out scanning electron microscope analysis, and going out the MgO median size according to the particle diameter statistical computation of electromicroscopic photograph is 50nm.Particle be shaped as sphere.
2) finishing:
Get 450 ℃ of MgO powder 1g behind the calcination 3h in beaker, get and contain 1.0% oleic 95% ethanolic soln, the two is blended in 55 ℃ of oil baths of constant temperature and stirs, naturally cooling behind the reaction 3h, through suction filtration, cryodrying, just make micro-nano MgO powder through the oleic acid finishing.
Measure according to lipophilic degree: after testing, its lipophilic degree is 60.98%.
The test of finishing optimum reaction condition
When behind a small amount of oleic acid modified, its lipophilic degree value increases immediately, when oleic acid concentration is 1.0% left and right sides, and the rising that almost is in line, this moment, lipophilic degree reached maximum value 60.98%; Along with the modifier consumption continues to increase, the lipophilic degree value of particulate begins to descend, and almost maintains about 47%-48%.So the inventor thinks that for nano-MgO among the present invention its coating materials oleic acid concentration should select 1.0% for use.
Micro-nano mineral grain lubricating additive wear resistant friction reducing effect test
For the marine diesel of under declared working condition, working, be in the base oil with 4012 marine lubricants, the nano-MgO particulate when adding makes its content when 0.3%-0.5%, and it is best that anti-wear and wear-resistant performance reaches.
Adopt reciprocating type wear test machine, at 100N, 300N, the condition of loading of 500N be experiment 8h down to cast iron-spot contact bearing steel-steel pair, the frictional coefficient minimum of sample is respectively 0.035,0.45,0.53 when the nano-MgO fraction of particle is respectively 0.4%, 0.3%, 0.4%; The antifriction rate is respectively 41.936%, 41.975% and 48.544% relatively.The frictional coefficient minimum of sample is respectively 32mg, 42mg, 66mg when the nano-MgO fraction of particle is 0.4%, 0.3%, 0.5%; The anti-attrition rate is respectively 59.49%, 61.47%, 70.00% relatively.
Above-mentioned test-results shows 4012 marine lubricants that add behind the nano-MgO particulate, all shows significantly antifriction antiwear effect under various load, and especially than under the high-load, the antifriction antiwear effect is more remarkable.
By the observation of the pattern of the polishing scratch of sample being analyzed the antifriction antiwear effect of nano-MgO particulate
This experiment places the pattern of observing its polishing scratch under the inverted metallurgic microscope respectively with 4012 marine lubricants, the following sample that contains behind the oil lubrication effect 8h of 0.4% nano-MgO particulate, analyzes the relatively friction and wear behavior of nano-MgO particulate.4012 marine lubricants that Fig. 1, Fig. 2 are respectively 4012 marine lubricants and contain 0.4% nanometer .MgO particulate pattern of sample down behind 500N load, friction 8h.
The sample that does not add the nano-MgO particulate as seen from Figure 1, behind friction 8h under the load of 500N, polishing scratch ditch dug with a plow skewness, depth difference is big, grinding defect diameter is bigger, and the edge is clear and sharp, analyzes through OLYCIA easy image analysis software, its ditch dug with a plow degree of depth is the darkest reaches 0.382mm, and diameter all surpasses 0.415mn mostly.What have just can distinguish under naked eyes.And the sample (as Fig. 2) after having added the nano-MgO particulate, its mill spot ditch dug with a plow and polishing scratch seem obviously that evenly smoother is observed in the polishing scratch surface under naked eyes.Between 0.05mm-0.08mm, the polishing scratch width is mostly between 0.25mm-0.35mm mostly for its ditch dug with a plow degree of depth.This strong explanation nano-MgO particulate can reduce the polishing scratch ditch dug with a plow degree of depth, diameter, and the polishing scratch ditch dug with a plow has been played filling effect, has reduced the roughness of surface of friction pair, thereby has helped antifriction.
The self-repair function effect
Under the operating mode that the surface contacts and the generation sudden strain of a muscle that rubs is warm, make that ferrous metals generation thermochemistry and the power chemical replacement on nano-MgO particulate and the surface of friction reacted, formation is stablized and uniform ferrosilicate ceramic layer, plays self-repair function.
Lubricating oil additive of the present invention is with the comparison test of the lubricating oil additive of serpentine particulate preparation:
1) by the mechanical crushing method preparation, this method technology is simple basically for the lubricating oil additive of serpentine particulate preparation, is convenient to operation.Choose the 12mm steel ball as abrading-ball in our test, drum's speed of rotation is adjusted to 450rpm, ball milling 48 hours can obtain the particle of micro-meter scale, and is about 20% less than 1 micron particle, about 3 microns of critical particle diameters.As seen its production efficiency is on the low side, and particle diameter is bigger than normal, thereby influences serpentine additive suspension stability in lubricating oil.The present invention adopts sol-gel method (Sol-Gel) preparation nano-MgO, and the MgO median size is 50nm.Particle be shaped as sphere, the additive size is more small, than the former easier raising additive powder suspension stability and dispersiveness in mineral lubricating oils.
By above-mentioned test as can be known: the above additive material of comparing, the easier preparation of nano-MgO of the present invention, size is littler, and the purity of preparing product is higher.Thereby stability and dispersion effect are better in lubricating oil, find phenomenons such as tangible reunion in the prepared lubricating oil, more difficult filtering in the oiling system of filtration unit is arranged.
2) the effect comparison of reducing friction and wearing and tearing: be base oil all with 4012 marine lubricants, add serpentine (hydroxyl magnesium silicate) lubricating oil additive (1.0%) and nano-MgO (0.3%-0.5%) respectively, adopt reciprocating type wear test machine, to cast iron-spot contact bearing steel-steel pair at 100N, 300N tests 8h under the condition of loading of 500N.
Experimental result shows: contain the relative antifriction rate of serpentine (hydroxyl magnesium silicate) lubricating oil additive testing of lubricating oil and be respectively 46.8%, 45.1%, 64.3%; Contain the relative antifriction rate of nano-MgO testing of lubricating oil and be respectively 41.936%, 41.975% and 48.544%.Contain the relative anti-attrition rate of serpentine (hydroxyl magnesium silicate) lubricating oil additive testing of lubricating oil: 83.3%, 57.14%, 63.6%; Contain the relative anti-attrition rate of nano-MgO lubricating oil additive testing of lubricating oil: 59.49%, 61.47%, 70.00%.As can be seen from the results: contain serpentine (hydroxyl magnesium silicate) lubricating oil additive lubricating oil friction reducing effect and slightly be better than the nano-MgO additive-treated oil.MgO lubricating oil additive lubricating oil antifriction effect under underload less than serpentine (hydroxyl magnesium silicate) lubricating oil additive lubricating oil; Under heavy lift, be better than serpentine (hydroxyl magnesium silicate) lubricating oil additive lubricating oil.Consider in the test factors such as error, can reach a conclusion is that the comprehensive antifriction antiwear characteristics of nano-MgO lubricating oil additive is equivalent to serpentine (hydroxyl magnesium silicate) lubricating oil additive.But nano-MgO antifriction optimum addn concentration (0.3%-0.5%) is less than serpentine (about 1.0%) lubricating oil additive lubricating oil.
Reference
[1] Li Haijun, Qiao Xueliang, Chen Jianguo, Wang Wei. the preparation of different shape nano magnesia and applied research progress. the material Leader, May the 21st in 2007 was rolled up special edition VIII, 139-142
[2] Yang Hongping, Kong Jie, Wu Bo. nano magnesia Study of synthesis method progress. the 37th volume the 10th phase Liaoning chemical industry Vol.37, No.10.2008 L in October iaoning Chemical Industry October, 2008:692-694
[3] Cao Ying, kingdom wins. the progress of nano magnesia technology of preparing. and the 37th volume the 1st phase Liaoning chemical industry Vol.37, No.1.2008 L in January iaoning Chemical Industry January, 2008:40-43
Claims (4)
1. the micro-nano mineral grain lubricating additive with self-repair function is that lipophilic degree is 60.98%, and median size is 45-55nm, particle be shaped as spheric nano-MgO powder.
2. lubricating oil that contains micro-nano mineral grain lubricating additive with self-repair function, it is characterized in that: comprise the nano-MgO powder of 0.1%-1.0%, it is through finishing, and lipophilic degree is 60.98%, the MgO median size is 45-55nm, particle be shaped as sphere.
3. preparation method with micro-nano mineral grain lubricating additive of self-repair function may further comprise the steps:
1) the preparation median size is 45-55nm, particle be shaped as spheric nano-MgO powder;
2) finishing get contain oleic acid 0.5-1.5% 95% ethanolic soln as modifier, the modification condition stirs in the constant temperature 50-60 ℃ oil bath for the two is blended in, the back naturally cooling that reacts completely, again through suction filtration, be drying to obtain.
4. the preparation method with micro-nano mineral grain lubricating additive of self-repair function according to claim 3 is characterized in that: oleic acid concentration 1.0% in the described modifier; Modify 55 ℃ of temperature; Modification time 3h.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102533413A (en) * | 2011-12-30 | 2012-07-04 | 大连海事大学 | Four-stroke gasoline engine oil composition of SG motorcycle, and preparation method and use thereof |
| CN113430046A (en) * | 2021-06-08 | 2021-09-24 | 大连海事大学 | Preparation method of friction-induced metal wear-resistant layer |
| CN114369482A (en) * | 2021-12-29 | 2022-04-19 | 烟台大学 | Preparation and use method of nanoscale super-smooth powder antifriction additive |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1206737A (en) * | 1998-07-13 | 1999-02-03 | 褚炎明 | Nanometer metal micropowder wear-resistant lubricant |
| CN1765803A (en) * | 2005-09-06 | 2006-05-03 | 南京中盟科技新材料有限公司 | Metal/ ceramic nano composite additive of self-rehabilitation and its preparation method |
-
2010
- 2010-03-16 CN CN 201010128448 patent/CN101787321A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1206737A (en) * | 1998-07-13 | 1999-02-03 | 褚炎明 | Nanometer metal micropowder wear-resistant lubricant |
| CN1765803A (en) * | 2005-09-06 | 2006-05-03 | 南京中盟科技新材料有限公司 | Metal/ ceramic nano composite additive of self-rehabilitation and its preparation method |
Non-Patent Citations (1)
| Title |
|---|
| 《中国优秀硕士学位论文全文数据库工程科技I辑》 20090915 马珂 微纳米润滑添加剂的研究 , * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102533413A (en) * | 2011-12-30 | 2012-07-04 | 大连海事大学 | Four-stroke gasoline engine oil composition of SG motorcycle, and preparation method and use thereof |
| CN113430046A (en) * | 2021-06-08 | 2021-09-24 | 大连海事大学 | Preparation method of friction-induced metal wear-resistant layer |
| CN114369482A (en) * | 2021-12-29 | 2022-04-19 | 烟台大学 | Preparation and use method of nanoscale super-smooth powder antifriction additive |
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Application publication date: 20100728 |