CN103073060B - 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
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.
Background technology
Magnesium-yttrium-transition metal sulfoselenide has various physical properties, as metallicity, semiconductor property, magnetic, supraconductivity etc., is with a wide range of applications.The preparation of this class material and character become recent research focus gradually.
Molybdenumdisulphide (MoS
2) be a kind of lubricant of excellent performance, in industry, be widely used.MoS
2have the laminate structure that is similar to graphite, in its structure, Mo-S faceted pebble specific surface area is large, combine, and interlayer combines by weak Van der Waals Er Sili, is easy between layers peel off in layer by very strong covalent linkage.Thereby the anti-shearing force of interlayer is very low, has good lubricity.As the MoS of lubricating oil additive
2, lubricant effect is also by MoS
2thin layer causes.
In the time that material size of particles enters nanometer scale, itself there is 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, by soluble in water to sodium sulphite and molybdenum acid ammonia, fully reacts two kinds of compounds, adds Aqueous Solutions of Polyethylene Glycol as dispersion agent simultaneously, with the above-mentioned solution of salt acidometric titration, obtains brown precipitate molybdenum trisulfide; By molybdenum trisulfide precipitation and centrifugal separation; after vacuum-drying, in quartz tube furnace under argon shield atmosphere, hydrogen desulfurization at 500～1000 DEG C of temperature; and be incubated 5～10 hours, obtain the inorganic spherical fullerene molybdenum disulfide nano particle with 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 He Liu source, molybdenum source, taking oxalic acid as reductive agent, at temperature 70 C～90 DEG C, stir 1～1.5h, sink to the bottom and obtain amorphous molybdenumdisulphide through chemistry, 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 above-mentioned patent.
Summary of the invention
The object of the present invention is to provide a kind of preparation method as six side's molybdenum disulfide nano sheets of antifriction additive of excellent property, to reduce the preparation cost of six side's molybdenum disulfide nano sheets, simplify preparation technology, and improve that to prepare productive rate high.
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), taking macromolecular compound as carbon source synthetic carbon ball;
Step (2), obtain solution: by Na
2mO
4, Na
2s, NH
2oHHCl is soluble in water, dissolves and obtains solution, then add homemade nano carbon microsphere, by centrifugal mixer, it is distributed in solution uniformly, is finally 6 ~ 8 by the pH value of acid-conditioning solution;
After step (3), solution stirring that step (2) is obtained, move into stainless steel cauldron, sealing, after isothermal reaction, is cooled to room temperature, obtains reaction product;
Step (4), separate above-mentioned reaction product, washing, dry, and by product under air conditions, 400～600 DEG C 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, preferably 1:3:2.
Described carbon ball and Na
2mO
4the ratio of amount of substance be 1:4 ~ 8, preferably 1:5.
Temperature of reaction in described step (3) is 160 DEG C～200 DEG C.
In described step (1), synthetic carbon ball 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 and dripped oleic acid in the base oil of tensio-active agent.The lubricating oil configuring 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 six side's molybdenum disulfide nano sheets simultaneously; 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 product rate is high, is applicable to large-scale industrial production.In preparation process, all reagent is commerical prod, does not need to prepare again.The six side's molybdenum disulfide nano sheets that make are due to its laminated structure, itself there is good lubricating property, in friction process, the nanometer sheet being dispersed in 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 " micro-bearing " effect, approx sliding friction is become to the compound motion of rolling and sliding friction, thereby reduction rubbing factor, improves lubricity; Nano level lubricating oil additive more easily deposits to play the effect of filling up for a long time in friction process on polishing scratch simultaneously, repairs in time damage location, improves the antifriction antiwear ability of surface of friction; While use as lubricating oil additive, there is peeling off of interlayer 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 engineering Application Areas.
Brief description of the 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 Fig. 2 under high resolving power field emission scanning electron microscope (SEM).
Embodiment
Embodiment 1
(a) 0.2 ml ammonia soln (25wt%) is added in the dehydrated alcohol of 16 ml and the distilled water mixing solutions of 40ml, add again 0.13 g F127, the formaldehyde solution of 0.4 g Resorcinol and 0.56 ml, is placed on 30 DEG C of waters bath with thermostatic control in constant-temperature heating magnetic stirring apparatus by this solution and is stirred to evenly; Then, above-mentioned mixing solutions is placed on to stainless steel cauldron hydrothermal reaction kettle and is placed in vacuum drying oven in 180 DEG C of insulation 24h, be cooled to room temperature.Reaction product, after centrifugation, is used respectively deionized water and dehydrated alcohol repetitive scrubbing, and finally under vacuum condition, 60 DEG C of dry 10h obtain resorcinol-formaldehyde resin nanometer polymerization ball.
(b) by 0.88g Na
2mO
4, 1.40g Na
2s, 0.7g NH
2oHHCl is dissolved in the distilled water of 70 ml, and before then adding, the resorcinol-formaldehyde resin nanometer polymerization ball 0.3g of preparation, stirs, then use salt acid for adjusting pH value to 7 left and right of 2mol/L.Mixed solution is transferred in stainless steel cauldron, is placed in vacuum drying oven in 180 DEG C of insulation 24h, be cooled to room temperature.Reaction product, after centrifugation, is used respectively deionized water and dehydrated alcohol repetitive scrubbing, and after the lower 80 DEG C of dry 10h of vacuum condition, under air atmosphere, 450 DEG C of annealing 2h obtain 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 photos under field emission scanning electron microscope and the high resolving power field emission scanning electron microscope of six prepared side's molybdenum disulfide nano sheets of embodiment 1, can obviously see 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
By 0.88g Na
2mO
4, 1.40g Na
2s, 0.7gNH
2oHHCl is dissolved in the distilled water of 70 ml, then adds 0.3g nano carbon microsphere of (a) middle preparation of embodiment 1 before, then uses salt acid for adjusting pH value to 7 left and right of 2mol/L.Stir after 30min, mixed solution is transferred in the stainless steel cauldron of 100ml, be placed in vacuum drying oven in 180 DEG C of insulation 24h, be cooled to room temperature.Reaction product, after centrifugation, is used respectively deionized water and dehydrated alcohol repetitive scrubbing, and after the lower 80 DEG C of dry 10h of vacuum condition, in tube furnace, under air atmosphere, 450 DEG C of annealing 2h obtain black powder, i.e. six side's molybdenum disulfide nano sheets.
The six side's molybdenum disulfide nano sheets that make are joined in heavy-duty gear oil CKD220, adopt the surface dispersant that oleic acid is nano material, configuration oil sample is placed under 60 DEG C of constant temperature and is disperseed 1 hour with ultrasonic disperser.(experiment condition is: 75 DEG C ± 2 DEG C 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 wear scar diameter (WSD), rubbing factor (f), the last non seizure load PB comparison of in base oil, adding six side's molybdenum disulfide nano sheets.
Table 1
| 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 |
From table 1, add the lubricating oil of six side's molybdenum disulfide nano sheets, obviously lower the friction factor in 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, fat, reduce the friction factor in friction process, improve fastness to wear, the work-ing life of elongated component.
It should be noted that; although technology contents of the present invention and technical characterictic have disclosed as above; but 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 present patent application claim.
Claims (4)
1. a preparation method who is used 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 taking macromolecular compound as carbon source;
(2) Na that is 0.5～1.5:2.5～3.5:1.5～2.5 by the ratio of amount of substance
2mO
4, Na
2s, NH
2oHHCl is soluble in water, dissolves and obtains solution, then add the prepared carbon ball of step (1), wherein carbon ball and Na
2mO
4the ratio of amount of substance be 1:4～8, after stirring, be 6～8 by the pH value of acid-conditioning solution;
(3) after solution stirring step (2) being obtained, move into after stainless steel cauldron reaction, temperature of reaction is 160 DEG C～200 DEG C, obtains reaction product;
(4) separate described reaction product, and reaction product annealing is obtained to six side's molybdenum disulfide nano sheets;
Wherein, described carbon ball is resorcinol-formaldehyde resin nanometer polymerization ball, and what the synthetic method of described carbon ball adopted is
method.
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 1:3:2.
3. method according to claim 1 and 2, is characterized in that, described carbon ball and Na
2mO
4the ratio of amount of substance be 1:5.
4. preparation method according to claim 1, is characterized in that, after reaction product described in described step (4) separates, through washing, dry, and annealing obtains six side's molybdenum disulfide nano sheets in the tube furnace of 400～600 DEG C of temperature.
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| CN103613137B (en) * | 2013-11-08 | 2015-07-29 | 电子科技大学 | A kind of hydrothermal synthesis method of molybdenum disulfide nano flower |
| 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 |
| CN107539964B (en) * | 2017-09-30 | 2019-11-26 | 江苏理工学院 | A kind of two selenizing molybdenum powder body material of hexagonal flake and preparation method thereof |
| CN108298508B (en) * | 2018-04-04 | 2019-09-10 | 西北大学 | Two sulphur oxygen molybdenums and its synthetic method and application |
| CN109943386B (en) * | 2019-03-22 | 2021-06-15 | 合肥学院 | Molybdenum disulfide/spent bleaching clay compound, preparation method and application |
| JP7131717B2 (en) * | 2019-12-09 | 2022-09-06 | Dic株式会社 | Lubricants and lubricating compositions |
| CN111704165B (en) * | 2020-08-04 | 2022-04-08 | 湘潭大学 | Hexagonal MoTe2Nanosheet and preparation method |
| WO2022202751A1 (en) * | 2021-03-24 | 2022-09-29 | Dic株式会社 | Particle-containing grease composition |
| WO2022201610A1 (en) * | 2021-03-24 | 2022-09-29 | Dic株式会社 | Molybdenum disulfide particles and lubricating composition |
| KR20230159414A (en) * | 2021-03-24 | 2023-11-21 | 디아이씨 가부시끼가이샤 | Molybdenum disulfide particles and lubricating compositions |
| CN113293400B (en) * | 2021-06-09 | 2023-06-20 | 济南大学 | Electrocatalytic nitrogen reduction catalyst MoS 2 -Mo 2 Process for the preparation 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 |