CN104591286B - A kind of preparation method of mos2 microsphere - Google Patents
A kind of preparation method of mos2 microsphere Download PDFInfo
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- CN104591286B CN104591286B CN201410816287.5A CN201410816287A CN104591286B CN 104591286 B CN104591286 B CN 104591286B CN 201410816287 A CN201410816287 A CN 201410816287A CN 104591286 B CN104591286 B CN 104591286B
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- ammonium molybdate
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- molybdate tetrahydrate
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G39/00—Compounds of molybdenum
- C01G39/06—Sulfides
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
Abstract
The invention discloses the preparation method of a kind of mos2 microsphere, comprise the steps: to dissolve in deionized water Ammonium Molybdate Tetrahydrate, it is made into the solution of 0.02～0.05mol/L, then in solution, add thiourea and polyvinylpyrrolidone, utilize magnetic stirrer 20～30min, make solution mix homogeneously, wherein Ammonium Molybdate Tetrahydrate is 1:10～1:20 with the mol ratio of thiourea, Ammonium Molybdate Tetrahydrate is 5:1 ~ 1:1 with the mass ratio of polyvinylpyrrolidone, then this solution is transferred in hydrothermal reaction kettle, hydro-thermal reaction 18～24h is carried out under the conditions of 220～250 DEG C, then natural cooling, by centrifugation, mos2 microsphere it is dried to obtain again after deionized water and washing with alcohol.The cost of the inventive method is inexpensive, and production technology is simple and easy to control, and the microsphere pattern of preparation is more homogeneous, and product output capacity is high, is suitable for large-scale commercial production.
Description
Technical field
The present invention relates to molybdenum bisuphide, particularly to the preparation method of a kind of mos2 microsphere.
Background technology
Friction and wear is the natural phenomena generally existed, according to estimates, more than the 1/3 of the disposable energy in the world because of friction loss produced by mechanical movement, abrasion is then one of material 3 kinds of principal modes with damage of facilities and inefficacy, lubricant then can help to reduce friction, reduce or avoid abrasion.Lubricant can be divided three classes: kollag, fluid lubricant and gas lubricant, modal lubricant is fluid lubricant, being made up of lubricating base oils and additive, additive has been largely fixed the serviceability of lubricant, including corrosion resistance, abrasion resistance and non-oxidizability；Antiwear and friction reduction property is one of main performance of lubricant, generally to pay the utmost attention to when research or exploitation lube product, and the research of lubrication oil antiwear antifriction additive is a popular domain；Recent two decades comes, and along with the continuous appearance of various nano materials, the research to lubricating oil antifriction additive nano material have also been obtained the development deepened continuously；Up to now, the nanoparticle being used as lube oil additive mainly has following a few class: the first kind is simple substance nano-metal particle, such as Nanometer Copper, stannum, bismuth, lead, nickel etc.；Equations of The Second Kind is nano-oxide, such as TiO2、ZnO、ZrO2、Y2O3Deng；3rd class is nano metal sulfoselenide, such as MoS2、WS2、NbS2、NbSe2、WSe2Deng.
Owing to the molybdenum bisuphide of body phase is the well known kollag with good friction reducing effect, the research that nano molybdenum disulfide is used as lube oil additive the most in recent years is the most；Such as Israel scientist Tenne
R team is to fullerene MoS2The tribological property of nano-particle has carried out extensive research, and they study discovery either by fullerene MoS2Nano-particle adds in structural material as kollag or adds to as lube oil additive and all can substantially reduce coefficient of friction and wear rate in base oil, improves the bearing capacity of friction pair simultaneously；Nearest research also finds MoS2Microsphere has good antiwear and friction reduction property as lube oil additive.
Summary of the invention
It is an object of the invention to provide the preparation method preparing mos2 microsphere that a kind of technique is simple, efficiency is high.
To achieve these goals, the present invention is by the following technical solutions: the preparation method of a kind of mos2 microsphere, comprise the steps: to dissolve in deionized water Ammonium Molybdate Tetrahydrate, it is made into the solution of 0.02～0.05mol/L, then in solution, add thiourea and polyvinylpyrrolidone, stirring makes solution mix homogeneously, then this solution is transferred in hydrothermal reaction kettle, carry out hydro-thermal reaction, then natural cooling, by centrifugation, is dried to obtain mos2 microsphere after deionized water and washing with alcohol again.
Described stirring is magnetic agitation, and the time is 20～30min.
Described Ammonium Molybdate Tetrahydrate is 1:10 ~ 1:20 with the mol ratio of thiourea.
Described Ammonium Molybdate Tetrahydrate is 5:1 ~ 1:1 with the mass ratio of polyvinylpyrrolidone.
Described hydrothermal temperature is 220～250 DEG C.
The described hydro-thermal reaction time is 18～24h.
Obtaining mos2 microsphere of the present invention, the control of its microsphere pattern is mainly reflected in:
1, the selection of raw material, molybdenum source should select Ammonium Molybdate Tetrahydrate, and concentration should control, 0.02～0.05mol/L, should add polyvinylpyrrolidone.
2, adding the control of the ratio of material, described Ammonium Molybdate Tetrahydrate is 1:10 ~ 1:20 with the mol ratio of thiourea；Described Ammonium Molybdate Tetrahydrate is 5:1 ~ 1:1 with the mass ratio of polyvinylpyrrolidone.
3, hydrothermal temperature should control at 220～250 DEG C, and Tai Gaotai is low the most not all right.
In preparation process of the present invention, all reagent are commercial product, it is not necessary to prepare again.
The cost of the inventive method is inexpensive, and production technology is simple and easy to control, and the microsphere pattern of preparation is more homogeneous, and product output capacity is high, is suitable for large-scale commercial production.
Accompanying drawing explanation
Fig. 1 is the XRD figure spectrum of the mos2 microsphere obtained by the embodiment of the present invention 1.
Fig. 2 is the EDS collection of illustrative plates of the mos2 microsphere that the embodiment of the present invention 1 prepares.
Fig. 3 is field emission scanning electron microscope (SEM) photo of the mos2 microsphere that the embodiment of the present invention 1 prepares.
Fig. 4 is the oil HVI750 additive friction curve to improving oil product tribological property based on mos2 microsphere prepared by example 1.
Fig. 5 is for containing MoS prepared by 1wt% example 12The change curve of the friction coefficient rotating speed of the lubricating oil of micro-sphere material.
Fig. 6 is field emission scanning electron microscope (SEM) photo of the mos2 microsphere that comparative example 1 of the present invention prepares.
Fig. 7 is field emission scanning electron microscope (SEM) photo of the mos2 microsphere that comparative example 3 of the present invention prepares.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is described further.
Embodiment
1
1.24g Ammonium Molybdate Tetrahydrate is dissolved in 36mL deionized water, it is configured to the solution of 0.03mol/L, add 0.76g thiourea and 0.5g polyvinylpyrrolidone, utilize magnetic stirrer 20min, the solution after stirring is transferred in the hydrothermal reaction kettle that volume is 50mL；Under the conditions of 220 DEG C, carry out hydro-thermal reaction 24h, then natural cooling, by centrifugation, be dried to obtain mos2 microsphere again after deionized water and washing with alcohol.
By obtained MoS2Microsphere is with addition 0.5wt%, 1 wt%, 3wt%, 5wt% adds in base oil HVI750, with ball-dish friction mode, upper sample is the stainless steel ball of material trademark 440C diameter 4mm, lower sample is the 45# steel disk of Φ 25mm × 6mm, during experiment, upper sample maintains static, lower sample rotates, with friction radius 7mm, relative rotational 400rpm, loading force 5N, 10N, 20N, 40N, 80N, the frictional experiment time, 30min carried out tribological property test to prepared oil product, result display quality proportioning 1wt% is with friction radius 7mm, speed of experiment 400rpm, properties of antifriction and wear resistance during loading force 20N is optimal, see Fig. 4.
In order to illustrate further containing 1.0wt% MoS2The tribological property of the oil product of additive, carries out speed change experiment to this oil product, will contain 1.0wt%
MoS2Oil sample and pure base oil HVI750 in load 20N, friction rotary speed 100rpm, 200rpm, 300rpm, 400rpm and 500rpm, friction radius 7mm, carry out during experimental period 30min contrasting frictional experiment, antifriction performance when seeking out rotating speed 400rpm is optimal, sees Fig. 5.
Embodiment
2
2.22g Ammonium Molybdate Tetrahydrate is dissolved in 36mL deionized water, it is configured to the solution of 0.05mol/L, add 2.72g thiourea and 1.5g polyvinylpyrrolidone, utilize magnetic stirrer 30min, the solution after stirring is transferred in the hydrothermal reaction kettle that volume is 50mL；Under the conditions of 240 DEG C, carry out hydro-thermal reaction 18h, then natural cooling, by centrifugation, be dried to obtain mos2 microsphere again after deionized water and washing with alcohol；SEM photograph is with embodiment 1.
Embodiment
3
1.65g Ammonium Molybdate Tetrahydrate is dissolved in 36mL deionized water, it is configured to the solution of 0.04mol/L, add 1.52g thiourea and 1g polyvinylpyrrolidone, utilize magnetic stirrer 20min, the solution after stirring is transferred in the hydrothermal reaction kettle that volume is 50mL；Under the conditions of 250 DEG C, carry out hydro-thermal reaction 24h, then natural cooling, by centrifugation, be dried to obtain mos2 microsphere again after deionized water and washing with alcohol；SEM photograph is with embodiment 1.
Fig. 1 is the XRD figure spectrum of the product prepared by embodiment 1, and product is pure MoS2Hexagonal；Fig. 2 is the EDS collection of illustrative plates of product prepared by embodiment 1, only exists S and Mo element in the drawings, and the atomic ratio of two elements is 1.98:1, and the product prepared by explanation is pure MoS2；Fig. 3 is the SEM photograph of the product prepared by embodiment 1, it can clearly be seen that sample is made up of substantial amounts of micron ball from SEM photograph Fig. 3, and microsphere diameter about 1 μm.
Comparative example 1
Change the addition of Ammonium Molybdate Tetrahydrate so that the mol ratio of Ammonium Molybdate Tetrahydrate and thiourea is 1:9, other preparation processes with embodiment 1, SEM photograph such as Fig. 6, it is impossible to prepared mos2 microsphere.
Comparative example 2
Change the addition of Ammonium Molybdate Tetrahydrate so that Ammonium Molybdate Tetrahydrate is 1:21 with the mol ratio of thiourea, and other preparation processes are with embodiment 1, and SEM photograph is similar with Fig. 6, it is impossible to prepare mos2 microsphere.
Comparative example 3
Change hydrothermal temperature so that hydrothermal temperature is 200 DEG C, other preparation processes with embodiment 1, SEM photograph such as Fig. 7, it is impossible to prepared mos2 microsphere.
Comparative example 4
Change hydrothermal temperature so that hydrothermal temperature is 260 DEG C, and other preparation processes are with embodiment 1, and SEM photograph is similar with Fig. 7, it is impossible to prepare mos2 microsphere.
Comparative example 5
Being added without polyvinylpyrrolidone, other preparation processes are with embodiment 1, and SEM photograph is similar with Fig. 6, it is impossible to prepare mos2 microsphere.
Comparative example 6
The concentration changing Ammonium Molybdate Tetrahydrate aqueous solution is 0.06mol/L, and other preparation processes are with embodiment 1, and SEM photograph is similar with Fig. 7, it is impossible to prepare mos2 microsphere.
Comparative example 7
The concentration changing Ammonium Molybdate Tetrahydrate aqueous solution is 0.01mol/L, and other preparation processes are with embodiment 1, and SEM photograph is similar with Fig. 7, it is impossible to prepare mos2 microsphere.
Claims (2)
1. the preparation method of a mos2 microsphere, it is characterised in that comprise the steps: to be dissolved in Ammonium Molybdate Tetrahydrate from
In sub-water, being made into the solution of 0.02～0.05mol/L, then add thiourea and polyvinylpyrrolidone in solution, stirring makes
Solution mix homogeneously, is then transferred to this solution in hydrothermal reaction kettle, carries out hydro-thermal reaction, then natural cooling, by centrifugation,
Mos2 microsphere it is dried to obtain again after washing；Described Ammonium Molybdate Tetrahydrate is 1:10～1:20 with the mol ratio of thiourea；Described four
AMMONIUM MOLYBDATE(VI) is 5:1～1:1 with the mass ratio of polyvinylpyrrolidone；Described hydrothermal temperature is 220～250 DEG C；Described
The hydro-thermal reaction time is 18～24h.
The preparation method of a kind of mos2 microsphere the most according to claim 1, it is characterised in that: described stirring is that magnetic force stirs
Mixing, the time is 20～30min.
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| CN105226277A (en) * | 2015-09-10 | 2016-01-06 | 中国科学院上海硅酸盐研究所 | A kind of high-performance transition metal dichalcogenide nanometer sheet radial direction assembling micro-sphere material and preparation method thereof |
| CN106807406B (en) * | 2015-11-27 | 2019-09-06 | 中国石油天然气股份有限公司 | The preparation method and catalyst of a kind of molybdenum disulfide nano catalyst and its application |
| CN105753053A (en) * | 2016-04-07 | 2016-07-13 | 福州大学 | Preparation method of nano-micro structure MoS2 spheres |
| CN106186158A (en) * | 2016-08-01 | 2016-12-07 | 镇江市高等专科学校 | Two selenizing molybdenums/ferroferric oxide magnetic nano composite, Preparation Method And The Use |
| CN106824230A (en) * | 2017-03-10 | 2017-06-13 | 哈尔滨工业大学 | The method that quantum dot aids in synthesis of carbon/molybdenum disulfide |
| CN107098390B (en) * | 2017-04-20 | 2018-10-16 | 合肥学院 | One kind simply preparing the adjustable sheet self assembly MoS of grain size2The method of bobbles shape powder |
| CN107579248A (en) * | 2017-08-23 | 2018-01-12 | 江汉大学 | The preparation method and applications of negative electrode of lithium ion battery molybdenum disulfide |
| CN108314084B (en) * | 2018-02-09 | 2019-12-20 | 西北工业大学 | Preparation method of metal phase molybdenum disulfide nanospheres |
| CN108535342B (en) * | 2018-03-14 | 2020-01-14 | 山东理工大学 | Preparation method and application of electrochemical immunosensor based on palladium-doped molybdenum disulfide nanospheres |
| CN108889315B (en) * | 2018-06-11 | 2021-01-15 | 合肥学院 | MoS2/TiO2Preparation method of heterostructure thin film photocatalyst |
| CN108658128B (en) * | 2018-08-02 | 2020-05-05 | 合肥中航纳米技术发展有限公司 | Preparation method of MoS2 micro nanospheres with hierarchical structure |
| CN109734132B (en) * | 2019-03-12 | 2020-10-16 | 中国矿业大学 | Method for controlling synthesis of molybdenum disulfide particles in mixed solvent system |
| WO2021117666A1 (en) * | 2019-12-09 | 2021-06-17 | Dic株式会社 | Lubricant and lubrication composition |
| CN112111730A (en) * | 2020-09-28 | 2020-12-22 | 长安大学 | Micro-arc oxidation layer with spherical molybdenum disulfide and preparation method thereof |
| CN115531539B (en) * | 2022-09-19 | 2023-09-15 | 海南大学 | Near-infrared SERS signal enhanced nano probe, preparation method thereof and application thereof in integrated diagnosis and treatment of infectious bacteria |
| CN116334689B (en) * | 2023-03-24 | 2024-02-23 | 安徽大学 | PVP modified NiMoS electrocatalyst and preparation method thereof |
| CN116593557B (en) * | 2023-05-17 | 2024-01-23 | 海南师范大学 | Electrochemical sensor prepared from molybdenum disulfide @ black phosphazene composite material and application thereof |
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