CN105802699B - A kind of ferroso-ferric oxide/Wolfram disulfide nano compounded lubricant and preparation method thereof - Google Patents
A kind of ferroso-ferric oxide/Wolfram disulfide nano compounded lubricant and preparation method thereof Download PDFInfo
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- CN105802699B CN105802699B CN201610237297.2A CN201610237297A CN105802699B CN 105802699 B CN105802699 B CN 105802699B CN 201610237297 A CN201610237297 A CN 201610237297A CN 105802699 B CN105802699 B CN 105802699B
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M125/00—Lubricating compositions characterised by the additive being an inorganic material
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M125/00—Lubricating compositions characterised by the additive being an inorganic material
- C10M125/10—Metal oxides, hydroxides, carbonates or bicarbonates
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M125/00—Lubricating compositions characterised by the additive being an inorganic material
- C10M125/22—Compounds containing sulfur, selenium or tellurium
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M177/00—Special methods of preparation of lubricating compositions; Chemical modification by after-treatment of components or of the whole of a lubricating composition, not covered by other classes
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
- C10M2201/06—Metal compounds
- C10M2201/062—Oxides; Hydroxides; Carbonates or bicarbonates
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
- C10M2201/06—Metal compounds
- C10M2201/065—Sulfides; Selenides; Tellurides
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
- C10N2030/04—Detergent property or dispersant property
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
- C10N2030/06—Oiliness; Film-strength; Anti-wear; Resistance to extreme pressure
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- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
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- Inorganic Chemistry (AREA)
- Lubricants (AREA)
Abstract
The invention discloses a kind of ferroso-ferric oxide/Wolfram disulfide nano compounded lubricant, the molar ratio of ferroso-ferric oxide and tungsten disulfide is 0.1~0.2:1~2.The invention also discloses above-mentioned ferroso-ferric oxide/Wolfram disulfide nano compounded lubricant preparation methods, include the following steps: tungsten disulfide carrying out ball milling, then tungsten disulfide after ball milling is added in glycerol and carries out ultrasonic disperse, centrifugation obtains tungsten disulfide nano slices glycerol dispersion liquid；Into tungsten disulfide nano slices glycerol dispersion liquid, sodium oxalate, ferric chloride hexahydrate, sodium acetate are sequentially added, hydro-thermal reaction is carried out after ultrasonic disperse, ferroso-ferric oxide/Wolfram disulfide nano compounded lubricant is dried to obtain after cleaning.Gained lubricant of the invention has excellent greasy property, can significantly extend the effectively lubricating time, and present invention process is easy, safety, and yield is high, at low cost, is easy to large-scale production.
Description
Technical field
The present invention relates to solid lubricant technical field more particularly to a kind of ferroso-ferric oxide/Wolfram disulfide nano are compound
Lubricant and preparation method thereof.
Background technique
As the mankind deepen continuously to space probation, more and more spacecrafts are admitted to space.American National
Aeronautics and Space Administration points out, leads to spacecraft operation irregularity due to lubrication failure or unsuccessfully have become to influence spacecraft and have
Imitate active time a key factor, therefore, how to keep the good lubrication of spacecraft critical component be one very
Important problem.Studies have shown that the space dust, elemental oxygen, ultraviolet irradiation, extreme high/low temperature etc. in space environment cause
An important factor for lubricant failure, selects suitable lubricant extremely important for aircraft stable operation.At present for direct
It is exposed to for the aircraft moving component of space environment, using tungsten disulfide (WS2) make lubricant using relatively conventional, this is
Since it can be able to maintain lower coefficient of friction and the secondary abrasion loss of lesser friction in space environment, however, WS2Hold after friction
It easily falls off from frictional interface, therefore, how to extend WS2The secondary lubrication timeliness urgent need to resolve of friction in space.
Retrieval discovery, although WS can be synthesized by the methods of hydro-thermal method2Nanometer sheet, but these WS2Nanometer sheet preparation cost
It is higher, and there is still a need for improve in the effectively lubricating time of frictional interface.Nanometer Fe3O4It is that one kind has ferromagnetic nanoparticle,
It can be magnetized in the secondary friction process of ferromagnetism friction, therefore can firmly be adsorbed on frictional interface, if can be by nanometer Fe3O4With
WS2Nanometer sheet is compound, it is likely that forms new nano combined lubricant, extends WS2The lubrication timeliness of nanometer sheet.Although Yang
Et al. (Biomaterials, 2015,60:62-71) report WS2@Fe3O4Nuclear shell structure nano composite particles targeted therapy cancer
The effect of disease, it is well known that composition, structure, preparation process technique of material etc. can be to products for composite material
Performance have an important influence on and be difficult to it is anticipated that therefore WS2The exploitation of composite material still belongs to scientific experimentation scope, in addition, so far
The present has no Fe3O4/WS2Nano combined lubricant extends WS2Lubricate the relevant report in terms of timeliness.
Summary of the invention
Technical problems based on background technology, the invention proposes a kind of ferroso-ferric oxide/Wolfram disulfide nano is multiple
Lubricant is closed, gained lubricant has excellent greasy property, can significantly extend the effectively lubricating time, and present invention process
Easy, safety, yield is high, at low cost, is easy to large-scale production.
A kind of ferroso-ferric oxide proposed by the present invention/Wolfram disulfide nano compounded lubricant, ferroso-ferric oxide and curing
The molar ratio of tungsten is 0.1~0.2:1~2.
Preferably, the partial size of ferroso-ferric oxide is 80~160nm.
Above-mentioned ferroso-ferric oxide/Wolfram disulfide nano compounded lubricant preparation method that the present invention also proposes, including such as
Lower step:
S1, tungsten disulfide is subjected to ball milling, then tungsten disulfide after ball milling is added in glycerol and carries out ultrasonic disperse, be centrifuged
Obtain tungsten disulfide nano slices glycerol dispersion liquid；
S2, into tungsten disulfide nano slices glycerol dispersion liquid, sequentially add sodium oxalate, ferric chloride hexahydrate, sodium acetate, surpass
Hydro-thermal reaction is carried out after sound dispersion, ferroso-ferric oxide/Wolfram disulfide nano compounded lubricant is dried to obtain after cleaning.
Preferably, in S1, tungsten disulfide is milled to average grain diameter less than 5 μm, then tungsten disulfide after ball milling is added
The wetting of first glycerol, is subsequently added into the second glycerol and carries out ultrasonic disperse, is centrifuged, the unstripped particle in removal bottom, in collection
Layer solution obtains tungsten disulfide nano slices glycerol dispersion liquid.
Preferably, in S1, the w/v (g/mL) of tungsten disulfide and the first glycerol is 2.48~4.96 after ball milling:
20, the volume ratio of the first glycerol and the second glycerol is 0.8~1.2:3.8~4.2.
Preferably, in S1, the time of ultrasonic disperse is 20~30h, and the temperature of ultrasonic disperse is 110~130 DEG C.
Preferably, in S1, centrifugal speed is 2900~3100rpm, and centrifugation time is 9~11min.
Preferably, the weight ratio of tungsten disulfide after ball milling, sodium oxalate, ferric chloride hexahydrate and sodium acetate be 2.48~
4.96:0.134~0.268:0.270g~0.540:4.08~8.16.
Preferably, in S2, the temperature of ultrasonic disperse is 80~100 DEG C, and the time of ultrasonic disperse is 1h.
Preferably, in S2, the temperature of hydro-thermal reaction is 150~160 DEG C, the time of hydro-thermal reaction is 20~for 24 hours.
Preferably, it in S2, is cleaned using acetone.
Preferably, in S2, drying temperature is 48~52 DEG C, and drying time is 3.8~4.2h.
Rationally, the partial size of ferroso-ferric oxide is 80~160nm to lubricant composition of the invention, is dispersed in tungsten disulfide
Nanometer sheet surface can effectively improve the composition ratio and structure of the two, and by ferroso-ferric oxide by controlling reaction condition
The magnetism of nano particle can significantly extend tungsten disulfide nano slices in the effectively lubricating time of rubbing surface；In addition, ferroso-ferric oxide
Nano particle can also form micro- ball effect on tungsten disulfide nano slices surface, to further promote tungsten disulfide nano slices
Lubricant effect.Meanwhile by the control of preparation condition, lubricant product yield height of the invention, good dispersion, preparation cost compared with
Low, safe preparation process, is easy to large-scale production at simple process.
Specific embodiment
In the following, technical solution of the present invention is described in detail by specific embodiment.
Embodiment 1
Above-mentioned ferroso-ferric oxide/Wolfram disulfide nano compounded lubricant preparation method that the present invention also proposes, including such as
Lower step:
S1, tungsten disulfide is milled to average grain diameter less than 5 μm, 20mL then is added in tungsten disulfide after 2.48g ball milling
Glycerol wetting, is subsequently added into 80mL glycerol and carries out ultrasonic disperse, and the time of ultrasonic disperse is 22h, and the temperature of ultrasonic disperse is
110 DEG C, it is centrifuged 10min, centrifugal speed 3000rpm, the unstripped particle in removal bottom collects upper solution and obtains curing
Tungsten nanometer sheet glycerol dispersion liquid；
S2, into tungsten disulfide nano slices glycerol dispersion liquid, sequentially add 0.134g sodium oxalate, six chloride hydrate of 0.540g
Iron, 4.08g sodium acetate carry out hydro-thermal reaction after ultrasonic disperse, and the temperature of ultrasonic disperse is 85 DEG C, and the time of ultrasonic disperse is
1h, the temperature of hydro-thermal reaction are 160 DEG C, and the time of hydro-thermal reaction is 20h, and four oxidations are dried to obtain after being cleaned using acetone
Three-iron/Wolfram disulfide nano compounded lubricant, drying temperature are 50 DEG C, drying time 4h.
Embodiment 2
Above-mentioned ferroso-ferric oxide/Wolfram disulfide nano compounded lubricant preparation method that the present invention also proposes, including such as
Lower step:
S1, tungsten disulfide is milled to average grain diameter less than 5 μm, 20mL then is added in tungsten disulfide after 3.72g ball milling
Glycerol wetting, is subsequently added into 80mL glycerol and carries out ultrasonic disperse, and the time of ultrasonic disperse is 25h, and the temperature of ultrasonic disperse is
120 DEG C, it is centrifuged 10min, centrifugal speed 3000rpm, the unstripped particle in removal bottom collects upper solution and obtains curing
Tungsten nanometer sheet glycerol dispersion liquid；
S2, into tungsten disulfide nano slices glycerol dispersion liquid, sequentially add 0.268g sodium oxalate, six chloride hydrate of 0.405g
Iron, 6.12g sodium acetate carry out hydro-thermal reaction after ultrasonic disperse, and the temperature of ultrasonic disperse is 90 DEG C, and the time of ultrasonic disperse is
1h, the temperature of hydro-thermal reaction are 150 DEG C, and the time of hydro-thermal reaction is for 24 hours, four oxidations to be dried to obtain after being cleaned using acetone
Three-iron/Wolfram disulfide nano compounded lubricant, drying temperature are 50 DEG C, drying time 4h.
Embodiment 3
Above-mentioned ferroso-ferric oxide/Wolfram disulfide nano compounded lubricant preparation method that the present invention also proposes, including such as
Lower step:
S1, tungsten disulfide is milled to average grain diameter less than 5 μm, 20mL then is added in tungsten disulfide after 4.96g ball milling
Glycerol wetting, is subsequently added into 80mL glycerol and carries out ultrasonic disperse, and the time of ultrasonic disperse is 28h, and the temperature of ultrasonic disperse is
130 DEG C, it is centrifuged 10min, centrifugal speed 3000rpm, the unstripped particle in removal bottom collects upper solution and obtains curing
Tungsten nanometer sheet glycerol dispersion liquid；
S2, into tungsten disulfide nano slices glycerol dispersion liquid, sequentially add 0.201g sodium oxalate, six chloride hydrate of 0.270g
Iron, 8.16g sodium acetate carry out hydro-thermal reaction after ultrasonic disperse, and the temperature of ultrasonic disperse is 95 DEG C, and the time of ultrasonic disperse is
1h, the temperature of hydro-thermal reaction are 155 DEG C, and the time of hydro-thermal reaction is 22h, and four oxidations are dried to obtain after being cleaned using acetone
Three-iron/Wolfram disulfide nano compounded lubricant, drying temperature are 50 DEG C, drying time 4h.
Gained ferroso-ferric oxide/Wolfram disulfide nano compounded lubricant in embodiment 1 and embodiment 2 is respectively added to sky
Between the PAO lubricating oil of 1wt% is formed in lubricating oil, evaluate its greasy property with vacuum friction and wear test equipment.
As a result, it has been found that under the same terms, the effectively lubricating time of addition 1wt% tungsten disulfide nano slices PAO lubricating oil is
40min, and add the effective of 1wt% present invention gained ferroso-ferric oxide/Wolfram disulfide nano compounded lubricant PAO lubricating oil
For lubrication time up to 200min or more, coefficient of friction reduces by 33% and 36% respectively, and abrasion loss reduces by 30% and 38% respectively,
Show that ferroso-ferric oxide/Wolfram disulfide nano compounded lubricant obtained by the present invention has very excellent greasy property, and
The effectively lubricating time of tungsten disulfide can significantly be extended.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
Anyone skilled in the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention and its
Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (6)
1. a kind of ferroso-ferric oxide/Wolfram disulfide nano compounded lubricant preparation method, which is characterized in that including walking as follows
It is rapid:
S1, tungsten disulfide is subjected to ball milling, then tungsten disulfide after ball milling is added in glycerol and carries out ultrasonic disperse, centrifugation obtains
Tungsten disulfide nano slices glycerol dispersion liquid, the time of ultrasonic disperse are 20~30h, and the temperature of ultrasonic disperse is 110~130 DEG C；
Centrifugal speed is 2900~3100rpm, and centrifugation time is 9~11min；
S2, into tungsten disulfide nano slices glycerol dispersion liquid, sequentially add sodium oxalate, ferric chloride hexahydrate, sodium acetate, ultrasound point
Hydro-thermal reaction is carried out after dissipating, ferroso-ferric oxide/Wolfram disulfide nano compounded lubricant, the temperature of ultrasonic disperse are dried to obtain after cleaning
Degree is 80~100 DEG C, and time of ultrasonic disperse is 1h, and the temperature of hydro-thermal reaction is 150~160 DEG C, and the time of hydro-thermal reaction is
20~for 24 hours；
Wherein, the molar ratio of ferroso-ferric oxide and tungsten disulfide is 0.1~0.2:1~2, the partial size of ferroso-ferric oxide is 80~
160nm。
2. ferroso-ferric oxide/Wolfram disulfide nano compounded lubricant preparation method, feature exist according to claim 1
In, in S1, tungsten disulfide is milled to average grain diameter less than 5 μm, the wetting of the first glycerol then is added in tungsten disulfide after ball milling,
It is subsequently added into the second glycerol and carries out ultrasonic disperse, be centrifuged, the unstripped particle in removal bottom collects upper solution and obtains two sulphur
Change tungsten nanometer sheet glycerol dispersion liquid.
3. ferroso-ferric oxide/Wolfram disulfide nano compounded lubricant preparation method, feature exist according to claim 2
In, in S1, after ball milling the w/v (g/mL) of tungsten disulfide and the first glycerol be 2.48~4.96:20, the first glycerol and
The volume ratio of second glycerol is 0.8~1.2:3.8~4.2.
4. ferroso-ferric oxide/Wolfram disulfide nano compounded lubricant preparation method, feature exist according to claim 3
In the weight ratio of, tungsten disulfide after ball milling, sodium oxalate, ferric chloride hexahydrate and sodium acetate be 2.48~4.96:0.134~
0.268:0.270g~0.540:4.08~8.16.
5. ferroso-ferric oxide/Wolfram disulfide nano compounded lubricant preparation method, feature exist according to claim 3
In being cleaned using acetone in S2.
6. ferroso-ferric oxide according to claim 4 or 5/Wolfram disulfide nano compounded lubricant preparation method, feature
It is, in S2, drying temperature is 48~52 DEG C, and drying time is 3.8~4.2h.
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| CN108251185B (en) * | 2018-01-22 | 2021-06-01 | 湖南金润昌石油有限责任公司 | Preparation and application of nano material composition used as lubricating oil additive |
| CN108504141A (en) * | 2018-03-09 | 2018-09-07 | 浙江华源颜料股份有限公司 | A kind of method that liquid phase high temperature and pressure cladding prepares heatproof iron oxide yellow |
| CN110157516B (en) * | 2019-06-27 | 2021-11-23 | 合肥工业大学 | Nano titanium dioxide/black phosphorus nanosheet composite lubricant and preparation method thereof |
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| WO2008091406A2 (en) * | 2006-09-21 | 2008-07-31 | Inframat Corporation | Lubricant-hard-ductile nanocomposite coatings and methods of making |
| CN101379168A (en) * | 2006-01-12 | 2009-03-04 | 阿肯色大学评议会 | Nanoparticle compositions and methods for making and using the same |
| CN102863025A (en) * | 2012-09-25 | 2013-01-09 | 镇江市高等专科学校 | Preparation method of piece-shaped tungsten disulfide nanometer lubricating oil additive |
| CN105087105A (en) * | 2015-09-11 | 2015-11-25 | 合肥工业大学 | Nano-molybdenum disulfide magnetic lubricant and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101379168A (en) * | 2006-01-12 | 2009-03-04 | 阿肯色大学评议会 | Nanoparticle compositions and methods for making and using the same |
| WO2008091406A2 (en) * | 2006-09-21 | 2008-07-31 | Inframat Corporation | Lubricant-hard-ductile nanocomposite coatings and methods of making |
| CN102863025A (en) * | 2012-09-25 | 2013-01-09 | 镇江市高等专科学校 | Preparation method of piece-shaped tungsten disulfide nanometer lubricating oil additive |
| CN105087105A (en) * | 2015-09-11 | 2015-11-25 | 合肥工业大学 | Nano-molybdenum disulfide magnetic lubricant and preparation method thereof |
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