CN103602362A - Preparation method of ferrous disulfide-graphene composite nano lubricant - Google Patents
Preparation method of ferrous disulfide-graphene composite nano lubricant Download PDFInfo
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- CN103602362A CN103602362A CN201310588955.9A CN201310588955A CN103602362A CN 103602362 A CN103602362 A CN 103602362A CN 201310588955 A CN201310588955 A CN 201310588955A CN 103602362 A CN103602362 A CN 103602362A
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Abstract
The invention discloses a preparation method of a ferrous disulfide-graphene composite nano lubricant. The preparation method is characterized by comprising the following steps: (1), adding matrix graphene, an iron source ferrous chloride and a dispersing agent into water to prepare liquor, regulating pH value to be alkaline, adding a vulcanizing agent thiourea, and uniformly mixing the liquor for future use; and (2), transferring the liquor into a stainless steel reaction kettle, sealing, cooling to the room temperature after carrying out hydrothermal reaction for 16 hours at 140 DEG C-240 DEG C, cleaning products by using deionized water, repeatedly cleaning by using absolute ethyl alcohol, carrying out vacuum drying to obtain black powder, wherein the structure of the black powder is that an FeS2 nanosphere coats on a graphene sheet layer, and dimension is 450 nm-800 nm. According to the preparation method, materials are easily available, price is low, preparation process is simple, parameters are easy to control, production process is safe and environment-friendly, and therefore, the preparation method is especially suitable for large-scale industrial production.
Description
Technical field
The present invention relates to field of nanometer material technology, particularly, is a kind of FeS
2the preparation method of-Graphene composite Nano lubricant.
Background technology
In recent years, transition-metal sulphides MS
2(M=Mo, W, Fe, Zn etc.), due to its unique physicochemical property and novel structure, get more and more people's extensive concerning and further investigate.These materials are extensively used as lithium ion cell electrode, lubricating oil additive, new catalyst and thermoelectric material etc.As the important a member in transition-metal sulphides, FeS
2(pyrite) there are very high photoabsorption coefficient (α=6 * 10, visible region
5cm
-1) and suitable band gap width (Eg=0.95eV) its excellent optics, electrochemistry and magnetic behavior make it in fields such as solar energy photoelectric conversion technology, specific function electrode materials and electromagnetic materials, have good potential application foreground in addition.Especially, FeS
2have laminate structure, between atom, respectively with covalent bonds, interlayer, with weak Van der Waals force combination, is used as lubricating oil additive slip between easy genetic horizon when being subject to shearing force, thereby plays the effect of antifriction.But at present, to its as solid additive the rare report of research in tribological field.FeS
2common preparation method mainly contain electrodip process, heat curing system, chemical vapor transportation method, Laser vaporization, spray pyrolysis, solvent-thermal method etc., all more complicated.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of FeS2-Graphene composite Nano lubricant, raw material is easy to get, cheap, and preparation technology is simple, parameter is easily controlled, and production process safety and environmental protection is particularly suitable for large-scale industrial production.
A kind of FeS
2the preparation method of-Graphene composite Nano lubricant, is characterized in that comprising the steps:
(1) matrix graphite alkene, source of iron iron protochloride, dispersion agent are added to the water and make solution, regulating pH value is alkalescence, adds vulcanizing agent thiocarbamide, and solution is mixed, standby;
The mol ratio of iron protochloride and thiocarbamide is 2:1-1:3; The mol ratio of Graphene and iron protochloride is 4:1-1:1; The mol ratio 1:4-1:10 of dispersion agent and iron protochloride;
Described dispersion agent is cats product, and as cetyl trimethylammonium bromide, or other materials is as polyvinylpyrrolidone.
(2) solution is moved into stainless steel cauldron, sealing, after 140 ℃～240 ℃ hydro-thermal reaction 16h, is cooled to room temperature, uses deionized water wash products, more repeatedly cleans with dehydrated alcohol, obtains black powder after vacuum-drying, and structure is FeS
2nanometer ball is coated on graphene sheet layer, and size is at 450-800nm.
Compare with traditional preparation method, the present invention adopts hydrothermal method to synthesize FeS
2, temperature of reaction is lower, preparation process gentle pollution-free, product purity is higher and FeS
2nano-powder particle size evenly, good dispersity, it is added as lubricating oil additive to in base oil, after test, it has good frictional behaviour.
Accompanying drawing explanation
Fig. 1 is the FeS that the present invention makes
2field emission scanning electron microscope (SEM) photo of-Graphene composite Nano lubricant.The SEM figure of 16 hours prepared products of hydro-thermal reaction in the stainless steel cauldron that Fig. 1 is is liner at tetrafluoroethylene at 180 ℃.Fig. 1 a can find out prepared size uniform, dispersed ball-like structure FeS preferably
2be grown on graphene sheet layer, its size is between 450-800nm and particle surface smoother (Fig. 1 b).
Fig. 2 is the FeS that the present invention makes
2the XRD spectra of-Graphene composite Nano lubricant.As can be seen from the figure, all peak positions all fit like a glove with standard diffractogram (JCPDS No.71-2219), and do not have other assorted peaks to occur, illustrate that reaction product is the FeS that purity is higher
2cubic system, counting lattice lattice constant is 0.5431nm.In figure, each diffraction peak is all strong and sharp-pointed, shows FeS
2the degree of crystallinity of nano-powder is very good.(because the amount of Graphene seldom can only be seen Graphene laminate structure partly, in XRD, the peak value of Graphene cannot detect).
Embodiment
By embodiment, further describe the present invention below, as known by the technical knowledge, the present invention also can describe by other the scheme that does not depart from the technology of the present invention feature, and therefore changes within the scope of the present invention all or that be equal in the scope of the invention are all included in the invention.
Embodiment 1:
0.1g Graphene is dissolved in to 20ml deionized water for ultrasonic 1h, then add respectively the polyvinylpyrrolidone (PVP) of 0.3g and the iron(ic) chloride of 0.2g, dripping until completely dissolved 5ml concentration is the NaOH solution of 0.5M, then adds the thiocarbamide of 0.2g, magnetic agitation 30min.Solution is transferred to 180 ℃ of insulation reaction 16h in the band teflon-lined stainless steel cauldron of 50ml.Be cooled to room temperature, centrifuge washing, in vacuum drying oven, 60 ℃ of vacuum-drying 8h, obtain black powder.
Embodiment 2:
Difference from Example 1 is polyvinylpyrrolidone to replace with cetyl trimethylammonium bromide.
Embodiment 3: difference from Example 1 is that the consumption of Graphene is 0.2g, and dispersion agent is cetyl trimethylammonium bromide.
Consumption and the processing parameter of the component that embodiment 4 to embodiment 7 adopts are as shown in table 1:
Table 1
The Graphene laminate structure that seldom can only see part in the amount of Graphene, in XRD, the peak value of Graphene cannot detect).
Embodiment
By embodiment, further describe the present invention below, as known by the technical knowledge, the present invention also can describe by other the scheme that does not depart from the technology of the present invention feature, and therefore changes within the scope of the present invention all or that be equal in the scope of the invention are all included in the invention.
Embodiment 1:
0.1g Graphene is dissolved in to 20ml deionized water for ultrasonic 1h, then add respectively the polyvinylpyrrolidone (PVP) of 0.3g and the iron(ic) chloride of 0.2g, dripping until completely dissolved 5ml concentration is the NaOH solution of 0.5M, then adds the thiocarbamide of 0.2g, magnetic agitation 30min.Solution is transferred to 180 ℃ of insulation reaction 16h in the band teflon-lined stainless steel cauldron of 50ml.Be cooled to room temperature, centrifuge washing, in vacuum drying oven, 60 ℃ of vacuum-drying 8h, obtain black powder.
Embodiment 2:
Difference from Example 1 is polyvinylpyrrolidone to replace with cetyl trimethylammonium bromide.
Embodiment 3: difference from Example 1 is that the consumption of Graphene is 0.2g, and dispersion agent is cetyl trimethylammonium bromide.
Consumption and the processing parameter of the component that embodiment 4 to embodiment 7 adopts are as shown in table 1:
Table 1
Frictional behaviour experiment: experimental technique, utilizes ultrasonic generator by dispersion agent span80 and product FeS
2-Graphene composite Nano lubricant is distributed in base oil (paraffin) uniformly, and the dirty solution oil sample frictional experiment that to be mixed with containing massfraction be 1%-5% carries out frictional experiment (it is 5% friction that table 2 just lists out massfraction) on CETR UMT-2 multifunction friction wear testing machine.Adopt the contact of ball-disc type, rotating speed is 50～400rpm, and load is 10N～50N, and experimental period is 30min.Testing Stainless Steel Ball model used is 440-C(9Cr18), diameter is 3mm, hardness is HRC62.
Embodiment 1 to 3 gained FeS
2the frictional coefficient of-Graphene composite Nano lubricant is as shown in table 2:
Table 2
Claims (3)
1. a preparation method for ferrous disulfide-Graphene composite Nano lubricant, is characterized in that comprising the steps:
(1) matrix graphite alkene, source of iron iron protochloride, dispersion agent are added to the water and make solution, regulating pH value is alkalescence, adds vulcanizing agent thiocarbamide, and solution is mixed, standby;
(2) solution is moved into stainless steel cauldron, sealing, after 140 ℃～240 ℃ hydro-thermal reaction 16h, is cooled to room temperature, uses deionized water wash products, more repeatedly cleans with dehydrated alcohol, obtains black powder after vacuum-drying, and structure is FeS
2nanometer ball is coated on graphene sheet layer, and size is at 450-800nm.
2. the preparation method of ferrous disulfide-Graphene composite Nano lubricant according to claim 1, is characterized in that described dispersion agent is cetyl trimethylammonium bromide or polyvinylpyrrolidone.
3. the preparation method of ferrous disulfide-Graphene composite Nano lubricant according to claim 1, the mol ratio that it is characterized in that iron protochloride and thiocarbamide is 2:1-1:3; The mol ratio of Graphene and iron protochloride is 4:1-1:1; The mol ratio 1:4-1:10 of dispersion agent and iron protochloride.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106378170A (en) * | 2016-08-16 | 2017-02-08 | 镇江市高等专科学校 | A graphitic carbon nitride/silver carbonate/silver bromide ternary composite nano-material, a preparing method thereof and uses of the nano-material |
| CN106702423A (en) * | 2016-11-23 | 2017-05-24 | 广东轻工职业技术学院 | Iron disulfide/nitrogen-doped graphene nanocomposite, preparation and application |
| CN107308956A (en) * | 2017-06-23 | 2017-11-03 | 哈尔滨工业大学 | A kind of preparation method of the efficient many iron sulfide of out-phase class fenton catalyst |
| CN107916158A (en) * | 2017-11-14 | 2018-04-17 | 蚌埠市嘉实机电设备制造有限公司 | A kind of lube oil additive |
| CN108144631A (en) * | 2017-12-25 | 2018-06-12 | 中国科学技术大学 | The preparation method of transition metal sulfide catalyst, preparation method and aromatic amine compound |
| CN109626444A (en) * | 2019-01-18 | 2019-04-16 | 哈尔滨工业大学 | A kind of spherical FeS of multi-pore channel sub-micron2Preparation method |
| CN111463439A (en) * | 2019-01-21 | 2020-07-28 | 中国科学院福建物质结构研究所 | Composite, bifunctional catalyst containing composite and electrochemical neutralization energy battery |
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| CN102796590A (en) * | 2012-08-24 | 2012-11-28 | 江苏大学 | Preparation method for tubular graphene/MoS2 nanocomposite material |
| CN102910615A (en) * | 2012-08-24 | 2013-02-06 | 江苏大学 | Preparation method of graphene oxide/iron disulfide composite nano particles |
| CN103289790A (en) * | 2012-06-08 | 2013-09-11 | 梅滨 | Novel antifriction lubricant additive containing nano ferrous sulphide |
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| CN102694171A (en) * | 2012-06-08 | 2012-09-26 | 浙江大学 | Hydrothermal preparation method for composite material of single-layer WS2 and graphene |
| CN103289790A (en) * | 2012-06-08 | 2013-09-11 | 梅滨 | Novel antifriction lubricant additive containing nano ferrous sulphide |
| CN102796590A (en) * | 2012-08-24 | 2012-11-28 | 江苏大学 | Preparation method for tubular graphene/MoS2 nanocomposite material |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106378170A (en) * | 2016-08-16 | 2017-02-08 | 镇江市高等专科学校 | A graphitic carbon nitride/silver carbonate/silver bromide ternary composite nano-material, a preparing method thereof and uses of the nano-material |
| CN106702423A (en) * | 2016-11-23 | 2017-05-24 | 广东轻工职业技术学院 | Iron disulfide/nitrogen-doped graphene nanocomposite, preparation and application |
| CN107308956A (en) * | 2017-06-23 | 2017-11-03 | 哈尔滨工业大学 | A kind of preparation method of the efficient many iron sulfide of out-phase class fenton catalyst |
| CN107916158A (en) * | 2017-11-14 | 2018-04-17 | 蚌埠市嘉实机电设备制造有限公司 | A kind of lube oil additive |
| CN108144631A (en) * | 2017-12-25 | 2018-06-12 | 中国科学技术大学 | The preparation method of transition metal sulfide catalyst, preparation method and aromatic amine compound |
| CN108144631B (en) * | 2017-12-25 | 2020-12-25 | 中国科学技术大学 | Transition metal sulfide catalyst, method for producing same, and method for producing aromatic amine compound |
| CN109626444A (en) * | 2019-01-18 | 2019-04-16 | 哈尔滨工业大学 | A kind of spherical FeS of multi-pore channel sub-micron2Preparation method |
| CN109626444B (en) * | 2019-01-18 | 2021-03-23 | 哈尔滨工业大学 | Porous channel submicron spherical FeS2Preparation method of (1) |
| CN111463439A (en) * | 2019-01-21 | 2020-07-28 | 中国科学院福建物质结构研究所 | Composite, bifunctional catalyst containing composite and electrochemical neutralization energy battery |
| CN111463439B (en) * | 2019-01-21 | 2022-02-18 | 中国科学院福建物质结构研究所 | Composite, bifunctional catalyst containing composite and electrochemical neutralization energy battery |
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Address after: 212028 No. 518, Chang Xiang Road, University Park, Zhenjiang, Jiangsu Patentee after: Zhenjiang College Address before: Zhenjiang City, Jiangsu Province, 212003 Jingkou District Road No. 61 Patentee before: Zhenjiang College |