CN103073060A - Method for preparing hexagonal molybdenum disulfide nanosheet as anti-friction additive - Google Patents
Method for preparing hexagonal molybdenum disulfide nanosheet as anti-friction additive Download PDFInfo
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Abstract
The invention discloses a method for preparing a hexagonal molybdenum disulfide nanosheet as an anti-friction additive. An additive-assistant hydrothermal synthesis method is adopted. The preparation method comprises the following steps: synthesizing a carbon ball from a high molecular compound as a carbon source by a Stober method; dissolving Na2MO4, Na2S and NH2OH.HCl in water to obtain a solution; adding the prepared nano carbon ball and uniformly dispersing the nano carbon ball in the solution by centrifugal stirring; adjusting the pH value of the solution to 6 to 8 with acid, and stirring the obtained solution and then moving the solution to a stainless steel reaction kettle for thermostatic reaction to obtain a reaction product; and separating the reaction product and annealing the product in a tube furnace of 400 to 600 DEG C to obtain the hexagonal molybdenum disulfide nanosheet. The preparation method is simple in process, and the prepared product is high in purity and yield, and excellent in antifriction and anti-wearing and lubricating property, and can serve as the anti-friction additive of lubricating oil and fat.
Description
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Technical field
The present invention relates to a kind of preparation method of antifriction additive, be specifically related to the preparation method as six side's molybdenum disulfide nano sheets of antifriction additive.
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Background technology
The magnesium-yttrium-transition metal sulfoselenide has various physical properties, such as metallicity, semiconductor property, magnetic, supraconductivity etc., is with a wide range of applications.The preparation of this class material and character become the recent research focus gradually.
Molybdenumdisulphide (MoS
2) be a kind of lubricant of excellent performance, in industry, be widely used.MoS
2The laminate structure that is similar to graphite is arranged, and Mo-S faceted pebble specific surface area is large in its structure, combine by very strong covalent linkage in the layer, and interlayer combines by weak Van der Waals Er Sili, is easy between layers peel off.Thereby the anti-shearing force of interlayer is very low, has good lubricity.MoS as lubricating oil additive
2, lubricant effect also is by MoS
2Thin layer causes.
When the material size of particles enters nanometer scale, itself have quantum size effect, small-size effect, surface effects, quantum tunneling effect.Nano level MoS
2Performance further promoted, be embodied in specific surface area very big, adsorptive power is stronger, reactive behavior is high, the catalytic performance especially performance of catalytic hydrogenation desulfurization is stronger, can be used to prepare special catalytic material and air storage material; Along with MoS
2Particle diameter diminish, it all obviously improves in the tack of friction material surface and level of coverage, wear-resistant, antifriction performance is also significantly improved.At present, the main method of preparation has gas-solid reaction, laser splash and arc-over, thermal decomposition method and solvent-thermal method etc.
Chinese patent CN200510050405.7 has announced a kind of preparation method of inorganic fullerene molybdenum disulfide.The method is soluble in water with sodium sulphite and molybdenum acid ammonia, and two kinds of compounds are fully reacted, and adds simultaneously Aqueous Solutions of Polyethylene Glycol as dispersion agent, with salt acidometric titration mentioned solution, obtains the brown precipitate molybdenum trisulfide; With the molybdenum trisulfide precipitation and centrifugal separation; after the vacuum-drying, in quartz tube furnace under the argon shield atmosphere, hydrogen desulfurization under 500～1000 ℃ of temperature; and be incubated 5～10 hours, obtain to have the inorganic spherical fullerene molybdenum disulfide nano particle of nested stratiform enclosed construction.
Chinese patent CN201010185621.3 has announced a kind of preparation method of nanoscale flaky molybdenum disulfide.Its concrete synthetic method is as follows: four thio ammonium molybdate is molybdenum source and sulphur source, take oxalic acid as reductive agent, the lower 1～1.5h that stirs in temperature 70 C～90 ℃ sinks to the bottom through chemistry and to obtain amorphous molybdenumdisulphide, then the high temperature anneal under nitrogen atmosphere obtains nanoscale flaky molybdenum disulfide.And disclosed preparation method needs to carry out pyroprocessing or reaction in the above-mentioned patent.
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Summary of the invention
The object of the present invention is to provide a kind of preparation method of the six side's molybdenum disulfide nano sheets that are used as antifriction additive of excellent property, to reduce the preparation cost of six side's molybdenum disulfide nano sheets, simplify preparation technology, and it is high to improve the preparation productive rate.
To achieve the above object of the invention, the preparation method of six side's molybdenum disulfide nano sheets that the present invention proposes, its step is as follows:
Step (1), take macromolecular compound as carbon source synthetic carbon ball;
Step (2), obtain solution: with Na
2MO
4, Na
2S, NH
2OHHCl is soluble in water, and dissolving obtains solution, adds homemade nano carbon microsphere again, by centrifugal mixer it is distributed in the solution uniformly, and the pH value with acid-conditioning solution is 6 ~ 8 at last;
After step (3), the solution stirring that step (2) is obtained, move into stainless steel cauldron, sealing after the isothermal reaction, is cooled to room temperature, obtains reaction product;
Step (4), separate above-mentioned reaction product, washing, drying, and with product under air conditions, 400～600 ℃ of tube annealing of temperature obtain six side's molybdenum disulfide nano sheets.
Wherein, described Na
2MO
4, Na
2S, NH
2The ratio of the amount of substance of OHHCl is 0.5 ~ 1.5:2.5 ~ 3.5:1.5 ~ 2.5, preferred 1:3:2.
Described carbon ball and Na
2MO
4The ratio of amount of substance be 1:4 ~ 8, preferred 1:5.
Temperature of reaction in the described step (3) is 160 ℃～200 ℃.
Carbon ball synthetic in the described step (1) is resorcinol-formaldehyde resin nanometer polymerization ball.What the synthetic method of described carbon ball adopted is St ber method.
The six side's molybdenum disulfide nano sheets that make are joined dripped in the base oil of oleic acid as tensio-active agent.The lubricating oil that configures is in friction process; because contained additive six side's molybdenum disulfide nano sheets can form the protective membrane with certain supporting capacity, lubrication in friction process; provide effectively lubricated; the mill spot of all right filling and repairing working-surface of while six side's molybdenum disulfide nano sheets; play the repair of wear surface; can improve wear resistance, antifriction quality and the extreme pressure property of lubricating base oils, the work-ing life of prolonged mechanical part.
The present invention adopts additive auxiliary water thermal synthesis method to prepare six side's molybdenum disulfide nano sheets, and preparation cost is lower, and production technique is simple and easy to control, and the product rate is high, is fit to large-scale industrial production.In the preparation process, all reagent are commerical prod, do not need to prepare again.The six side's molybdenum disulfide nano sheets that make are because its laminated structure, itself has good lubricating property, in the friction process, the nanometer sheet that is dispersed in the lubricating oil can be along with the mobile ditch dug with a plow place that is brought to polishing scratch of oil, when nano particle is extruded between friction pair, squeeze broken nanoparticle and play " little bearing " effect, approx sliding friction is become the compound motion of rolling and sliding friction, thereby the reduction rubbing factor improves lubricity; Nano level lubricating oil additive is easier in friction process simultaneously deposits to play the effect of filling up on polishing scratch for a long time, in time repairs damage location, improves the antifriction antiwear ability of surface of friction; When using as lubricating oil additive, peeling off of interlayer occurs in six side's molybdenum disulfide nano sheets under high pressure, high temperature between friction pair, hindered the intermetallic direct contact of friction pair, also reduced the possibility of adhesive wear simultaneously.Six side's molybdenum disulfide nano sheets of nanostructure both can be used as solid lubricant, also can be used as the antifriction additive of lubricating oil, fat, had vast potential for future development in the engineering Application Areas.
Description of drawings
Fig. 1 is the X-ray spectrogram (XRD) of solid lubrication oil additive six side's molybdenum disulfide nano sheets of making of the present invention.
Fig. 2 is the microscopic appearance picture under solid lubrication oil additive six side's molybdenum disulfide nano sheet field emission scanning electron microscopes (SEM) of making of the present invention.
Fig. 3 is the microscopic appearance pictures of six side's molybdenum disulfide nano sheets shown in Figure 2 under high resolving power field emission scanning electron microscope (SEM).
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Embodiment
Embodiment 1
(a) 0.2 ml ammonia soln (25wt%) is added in the distilled water mixing solutions of the dehydrated alcohol of 16 ml and 40ml, add again 0.13 g F127,0.4 the formaldehyde solution of g Resorcinol and 0.56 ml is placed on this solution that 30 ℃ of waters bath with thermostatic control are stirred to evenly in the constant-temperature heating magnetic stirring apparatus; Then, above-mentioned mixing solutions is placed on the stainless steel cauldron hydrothermal reaction kettle places vacuum drying oven in 180 ℃ of insulation 24h, be cooled to room temperature.Reaction product is used respectively deionized water and dehydrated alcohol repetitive scrubbing after centrifugation, 60 ℃ of dry 10h obtain resorcinol-formaldehyde resin nanometer polymerization ball under vacuum condition at last.
(b) with 0.88g Na
2MO
4, 1.40g Na
2S, 0.7g NH
2OHHCl is dissolved in the distilled water of 70 ml, and the resorcinol-formaldehyde resin nanometer polymerization ball 0.3g of preparation stirs before then adding, and uses about the salt acid for adjusting pH value to 7 of 2mol/L again.Mixed solution is transferred in the stainless steel cauldron, places vacuum drying oven in 180 ℃ of insulation 24h, be cooled to room temperature.Reaction product is used respectively deionized water and dehydrated alcohol repetitive scrubbing after centrifugation, behind the lower 80 ℃ of dry 10h of vacuum condition, under air atmosphere, 450 ℃ of annealing 2h get black powder, i.e. six side's molybdenum disulfide nano sheets.
Fig. 1 is the XRD figure spectrum of the prepared product of embodiment 1, and product is pure MoS
2Hexagonal.Fig. 2 and Fig. 3 are the field emission scanning electron microscope of six prepared side's molybdenum disulfide nano sheets of embodiment 1 and the photo under the high resolving power field emission scanning electron microscope, can see obviously that the nanometer sheet of a large amount of homogeneous generates, without agglomeration.Its diameter is about 500～800nm, and thickness is six side's molybdenum disulfide nano sheets of 50～100 nm.
Embodiment 2
With 0.88g Na
2MO
4, 1.40g Na
2S, 0.7gNH
2OHHCl is dissolved in the distilled water of 70 ml, then adds before nano carbon microsphere of (a) middle preparation of embodiment 1 of 0.3g, uses about the salt acid for adjusting pH value to 7 of 2mol/L again.After stirring 30min, mixed solution is transferred in the stainless steel cauldron of 100ml, places vacuum drying oven in 180 ℃ of insulation 24h, be cooled to room temperature.Reaction product is used respectively deionized water and dehydrated alcohol repetitive scrubbing after centrifugation, behind the lower 80 ℃ of dry 10h of vacuum condition, under tube furnace Air atmosphere, 450 ℃ of annealing 2h get black powder, i.e. six side's molybdenum disulfide nano sheets.
The six side's molybdenum disulfide nano sheets that make are joined among the heavy-duty gear oil CKD220, and adopting oleic acid is the surface dispersant of nano material, will configure oil sample and place under 60 ℃ of constant temperature with ultrasonic disperser dispersion 1 hour.(experiment condition is: 75 ℃ ± 2 ℃ of temperature to investigate its tribological property at MR-S10B type four ball frictional testing machiness; Rotating speed 1200r/min ± 60r/min; Load 392N ± 4N; Time 60min ± 1min).Table 1 shows the wear scar diameter (WSD), rubbing factor (f), the last non seizure load PB that add six side's molybdenum disulfide nano sheets in base oil and compares.
Table 1
| The oil product title | Base oil | Add six side's molybdenum disulfide nano sheets (1.0%) |
| Wear scar diameter (WSD)/mm | 0.7733 | 0.3898 |
| Rubbing factor (f) | 0.0547 | 0.0478 |
| Last non seizure load (PB)/N | 726 | 1063 |
By as seen from Table 1, add the lubricating oil of six side's molybdenum disulfide nano sheets, obviously lower the friction factor in the friction process, improve fastness to wear and the extreme pressure property of lubricating oil.
Six side's molybdenum disulfide nano sheets as antifriction additive of the present invention can make an addition in lubricating oil, the fat, reduce the friction factor in the friction process, improve fastness to wear, the work-ing life of elongated component.
Need to prove; although technology contents of the present invention and technical characterictic have disclosed as above; yet those of ordinary skill in the art still may be based on teaching of the present invention and announcements and are done all replacement and modifications that does not deviate from spirit of the present invention; therefore; protection domain of the present invention should be not limited to the content that embodiment discloses; and should comprise various do not deviate from replacement of the present invention and modifications, and contained by the present patent application claim.
Claims (7)
1. preparation method as six side's molybdenum disulfide nano sheets of antifriction additive is characterized in that: comprise that step is as follows:
(1) the synthetic carbon ball take macromolecular compound as carbon source;
(2) with Na
2MO
4, Na
2S, NH
2OHHCl is soluble in water, and dissolving obtains solution, adds the prepared carbon ball of step (1) again, and the rear pH value with acid-conditioning solution that stirs is 6 ~ 8;
(3) after the solution stirring that step (2) is obtained, after the reaction of immigration stainless steel cauldron, obtain reaction product;
(4) separate described reaction product, and reaction product annealing is obtained six side's molybdenum disulfide nano sheets.
2. preparation method according to claim 1 is characterized in that, described Na
2MO
4, Na
2S, NH
2The ratio of the amount of substance of OHHCl is 0.5 ~ 1.5:2.5 ~ 3.5:1.5 ~ 2.5, preferred 1:3:2.
3. according to claim 1 or 2 described methods, it is characterized in that described carbon ball and Na
2MO
4The ratio of amount of substance be 1:4 ~ 8, preferred 1:5.
4. preparation method according to claim 1 is characterized in that, the temperature of reaction in the described step (3) is 160 ℃～200 ℃.
5. preparation method according to claim 1 is characterized in that, described carbon ball is resorcinol-formaldehyde resin nanometer polymerization ball.
6. preparation method according to claim 1 or 5 is characterized in that, what the synthetic method of described carbon ball adopted is St ber method.
7. preparation method according to claim 1 is characterized in that, after reaction product described in the described step (4) was separated, through washing, drying, and annealing obtained six side's molybdenum disulfide nano sheets in the tube furnace of 400～600 ℃ of temperature.
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| CN103613137A (en) * | 2013-11-08 | 2014-03-05 | 电子科技大学 | Hydrothermal synthesis method of molybdenum disulfide nano flowers |
| CN105923655A (en) * | 2016-04-22 | 2016-09-07 | 合肥工业大学 | Method for preparing molybdenum disulfide nanotube by calcining nanofiber-like sodium ammonium polymolybdate and carrying out sulfuration |
| CN107539964A (en) * | 2017-09-30 | 2018-01-05 | 江苏理工学院 | A kind of selenizing molybdenum powder body material of hexagonal flake two and preparation method thereof |
| CN108298508A (en) * | 2018-04-04 | 2018-07-20 | 西北大学 | Two sulphur oxygen molybdenums and its synthetic method and application |
| CN109943386A (en) * | 2019-03-22 | 2019-06-28 | 合肥学院 | A kind of molybdenum disulfide/spent bleaching clay compound, preparation method and application |
| CN111704165A (en) * | 2020-08-04 | 2020-09-25 | 湘潭大学 | Hexagonal MoTe2Nanosheet and preparation method |
| WO2021117666A1 (en) * | 2019-12-09 | 2021-06-17 | Dic株式会社 | Lubricant and lubrication composition |
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| CN105923655B (en) * | 2016-04-22 | 2017-06-06 | 合肥工业大学 | It is a kind of by calcining the method that nanometer fibrous poly- molybdic acid ammonium sodium and vulcanization prepare molybdenum disulfide nano tube |
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| CN113293400A (en) * | 2021-06-09 | 2021-08-24 | 济南大学 | Electro-catalytic nitrogen reduction catalyst MoS2-Mo2Preparation method of C |
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Effective date of registration: 20160104 Address after: 215500, Suzhou, Jiangsu Province, Changshou City Tong Town, Ho City Development Zone No. 19 Patentee after: Suzhou Huifeng lubricating material Co., Ltd. Address before: 215500, Suzhou, Jiangsu City, Changshou City province Ho Ho Town Industrial Park Patentee before: The plump sliding material of Jiangsu favour limited-liability company |