CN102911774A - Lubricating grease containing carbon nanotubes and preparation method of lubricating grease - Google Patents
Lubricating grease containing carbon nanotubes and preparation method of lubricating grease Download PDFInfo
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- CN102911774A CN102911774A CN2012104189297A CN201210418929A CN102911774A CN 102911774 A CN102911774 A CN 102911774A CN 2012104189297 A CN2012104189297 A CN 2012104189297A CN 201210418929 A CN201210418929 A CN 201210418929A CN 102911774 A CN102911774 A CN 102911774A
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Abstract
The invention relates to lubricating grease containing carbon nanotubes and a preparation method of the lubricating grease. The lubricating grease comprises bentonite as a thickening agent, refined mineral oil or synthetic oil as base oil, padding of carbon nanotube, and a polarity disperse assisting agent. The preparation method includes the steps of adding the carbon nanotubes treated in all base oil, adding organic bentonite for pre-dispersing, adding propylene carbonate as the polarity disperse assisting agent until a black uniform paste-structured lubricating grease is formed in a reactor, and finally obtaining the lubricating grease product. Compared with conventional bentonite lubricating grease, abrasion resistance performance of the lubricating grease containing carbon nanotubes is remarkably improved, and stability performance of high-temperature rubber bodies of the bentonite lubricating grease can be improved. A new application field is developed in nano lubricating materials for the carbon nanotube.
Description
Technical field
The present invention relates to lubricating grease of a kind of carbon nanotubes and preparation method thereof, preparation technology is special, and the lubricating grease of preparation has good high temperature extreme pressure and antiwear behavior.
Background technology
Nano material has obtained comparatively deep research in the lubricating oil field at present, but the rarely seen report of the application in the lubricating grease field.Some scholars once were studied the tribology behavior of several nanoparticles, had proved that nanoparticle has preferably tribological property.How advanced person's nanotechnology and traditional grease manufacture industry organically being merged and demonstrate fully its advantage, has been the problem of pendulum in face of ours.
Carbon nanotube is the novel carbon nanomaterial of finding at the end of last century, structure and graphite and C
60Similar, can be regarded as to be rolled by certain mode by graphene layer and form.It not only has superpower toughness, and has excellent self-lubricating property.Because the hollow tubular structure of carbon nanotube, interlayer is with the Van der Waals force combination, chemical stability is high, easily be deposited on the friction metallic surface, form deposited film, and because the tubular structure of carbon nanotube makes its easily Free-rolling between friction pair, form " lubricant film ", " little bearing ", play friction-reducing and antiwear action.In addition, the resistance to elevated temperatures of carbon nanotube excellence and low thermal expansivity, good fatigue resistance, axial tensile strength and wear resistance also provide new approach for preparing high temperature resistant heavy loading lubricant.
Carbon nanotube as slip additive, is used to some extent in solid lubricant and lubricating oil, and made some progress.At present, some are also arranged about the report of carbon nanotube in lubricating grease, but what its major part was outstanding is heat conductivility and the conductivity of carbon nanotube, and at the rare report of abrasion resistance, resistance to elevated temperatures of lubricating grease, this patent is intended to develop a kind of bentonite-thickened grease of carbon nanotubes, promotes to a certain extent the combination of nanotechnology and conventional grease.Yet, because chemically modified has certain destruction to the tube wall of carbon nanotube, therefore only carbon nanotube has been carried out purifying and brachymemma in this patent.
Summary of the invention
The invention provides lubricating grease of a kind of carbon nanotubes and preparation method thereof, this grease composition comprises viscosifying agent, base oil and compositions of additives.This lubricating grease is satisfying high-temperature behavior, is preventing from can also effectively increasing the friction and wear behavior of lubricating grease under the prerequisite of other performances such as copper corrosion performance.
The concrete technical scheme of the present invention is as follows:
A kind of lubricating grease of carbon nanotubes, its composition and quality percentage composition are as follows:
Viscosifying agent is wilkinite: 5-20%;
Base oil is refined mineral oil or synthetic oil: 70-90%;
Carbon nanotube filler: 0.5-3%;
Polarity dispersion aids: be the 30%-60% of organobentonite quality.
Described wilkinite is the organic amine modified alta-mud.
100 ℃ of viscosity of described base oil are 5～50mm
2/ s, base oil comprise a kind of in paraffin base mineral oil, naphthenic mineral oil, synthetic hydrocarbon lubricating oil, polysiloxane based lubricating oil or the lubricating oil in esters.
Described carbon nanotube is multi-walled carbon nano-tubes.
Described polarity dispersion aids is propylene carbonate.
The preparation of greases method of a kind of carbon nanotubes of the present invention the steps include:
(1), the purifying of carbon nanotube and brachymemma: the initial carbon nanotube is added in the nitration mixture, ultrasonic in 50～80 ℃ water-bath, remove wherein impurity and catalyst residue particle, then use deionized water wash, and with the tetrafluoroethylene filtering with microporous membrane in 0.35～0.55 μ m aperture, until the pH value is 7, then in 80 ℃ of vacuum drying ovens, more than the dry 12h, make the carbon nanotube of purifying brachymemma; Nitration mixture is that volume ratio is the vitriol oil and the concentrated nitric acid of 3:1;
(2), the carbon nanotube of processing is joined in whole base oils, under high-speed stirring, be heated to 90～100 ℃, until being distributed in the base oil of even carbon nanotube;
(3), subsequently slowly add organobentonite and carry out pre-dispersedly, itself and base oil are mixed, stir at least 10min, until the organobentonite complete wetting;
(4), add polarity dispersion aids propylene carbonate, under agitation continue to mix 30～40min, and constantly carry out circulation shear, until thing forms the paste structure of lubricating grease black even in the still, in this process, keep 80～90 ℃ of temperature in the kettle;
(5), thing in the still is ground by homogenizer, namely get grease product.
Compare with traditional bentonite-thickened grease, lubricating grease of the present invention has following advantage: the anti-wear performance that (a) can obviously improve lubricating grease; (b) can improve the high temperature colloid stability of bentonite-thickened grease.
This invention has been opened up a new Application Areas for carbon nanotube in nano-lubricating material.
Embodiment
Carbon nanotube in all examples all is through the multi-walled carbon nano-tubes after purifying and the brachymemma, concrete steps are: the initial carbon nanotube is added in the nitration mixture (volume ratio of the vitriol oil and concentrated nitric acid is 3:1), in 50～80 ℃ water-bath about ultrasonic 12h, remove wherein impurity and catalyst residue particle, then use deionized water wash, and with the tetrafluoroethylene filtering with microporous membrane in 0.35～0.55 μ m aperture, until pH value is 7, then in 80 ℃ of vacuum drying ovens, more than the dry 12h, make the carbon nanotube of purifying brachymemma.
Embodiment 1:
Multi-walled carbon nano-tubes and 1080g paraffinic base mineral base oil that 24g processed are put in the stirring tank, are warming up to 90～100 ℃ under the high-speed stirring, and under this temperature high-speed stirring 0.5h.Reduce subsequently stirring velocity, slowly add the 60g organobentonite, stir 20～30min, make the organobentonite complete wetting.After thing forms pre-gelled in still, add the 36g propylene carbonate, continue high-speed stirring 30～40min, and carry out circulation shear, until the paste architecture of thing formation lubricating grease black even in the still.Temperature in the kettle remains on 80～90 ℃ always in this process.Thing grinds through colloidal mill in the last still, gets product.
Material proportion is described as follows:
Organobentonite: 5%;
Refined wax base mineral base oil: 90%;
Multi-walled carbon nano-tubes: 2%;
Propylene carbonate polarity dispersion aids: be 60% of organobentonite quality.
Embodiment 2:
Multi-walled carbon nano-tubes and 600g naphthenic mineral base oil that 6g processed are put in the stirring tank, are warming up to 90～100 ℃ under the high-speed stirring, and under this temperature high-speed stirring 0.5h.Reduce subsequently stirring velocity, slowly add the 70g organobentonite, stir 20～30min, make the organobentonite complete wetting.After thing forms pre-gelled in still, add the 30g propylene carbonate, continue high-speed stirring 30～40min, and carry out circulation shear, until the paste architecture of thing formation lubricating grease black even in the still.Temperature in the kettle remains on 80～90 ℃ always in this process.Thing grinds through colloidal mill in the last still, gets product.
Material proportion is described as follows:
Organobentonite: 9.9%;
Refining naphthenic mineral base oil: 85%;
Multi-walled carbon nano-tubes: 0.85%;
Propylene carbonate polarity dispersion aids: be 42.9% of organobentonite quality.
Embodiment 3:
The synthetic hydrocarbon base oil of the multi-walled carbon nano-tubes that 15g was processed and 600g is put in the stirring tank, is warming up to 90～100 ℃ under the high-speed stirring, and under this temperature high-speed stirring 0.5h.Reduce subsequently stirring velocity, slowly add the 100g organobentonite, stir 20～30min, make the organobentonite complete wetting.After thing forms pre-gelled in still, add the 60g propylene carbonate, continue high-speed stirring 30～40min, and carry out circulation shear, until the paste grease structure of thing formation black even in the still.Temperature in the kettle remains on 80～90 ℃ always in this process.Thing grinds through colloidal mill in the last still, gets product.
Material proportion is described as follows:
Organobentonite: 12.9%;
Synthetic hydrocarbon base oil: 77.4%;
Multi-walled carbon nano-tubes: 1.9%;
Propylene carbonate polarity dispersion aids: be 60% of organobentonite quality.
Embodiment 4:
Multi-walled carbon nano-tubes and 560g polysiloxane group base oil that 4g processed are put in the stirring tank, are warming up to 90～100 ℃ under the high-speed stirring, and under this temperature high-speed stirring 0.5h.Reduce subsequently stirring velocity, slowly add the 160g organobentonite, stir 20～30min, make the organobentonite complete wetting.After thing forms pre-gelled in still, add the 76g propylene carbonate, continue high-speed stirring 30～40min, and carry out circulation shear, until the paste grease structure of thing formation black even in the still.Temperature in the kettle remains on 80～90 ℃ always in this process.Thing grinds through colloidal mill in the last still, gets product.
Material proportion is described as follows:
Organobentonite: 20%;
Polysiloxane basis oil: 70%;
Multi-walled carbon nano-tubes: 0.5%;
Propylene carbonate polarity dispersion aids: be 47.5% of organobentonite quality.
Embodiment 5:
Multi-walled carbon nano-tubes and 600g ester class base oil that 22.5g processed are put in the stirring tank, are warming up to 90～100 ℃ under the high-speed stirring, and under this temperature high-speed stirring 0.5h.Reduce subsequently stirring velocity, slowly add the 100g organobentonite, stir 20～30min, make the organobentonite complete wetting.After thing forms pre-gelled in still, add the 30g propylene carbonate, continue high-speed stirring 30～40min, and carry out circulation shear, until the paste grease structure of thing formation black even in the still.Temperature in the kettle remains on 80～90 ℃ always in this process.Thing grinds through colloidal mill in the last still, gets product.
Material proportion is described as follows:
Organobentonite: 13.3%;
Ester class base oil: 80%;
Multi-walled carbon nano-tubes: 3.0%;
Propylene carbonate polarity dispersion aids: be 30% of organobentonite quality.
In table 1, provided existing bentonite-thickened grease and according to the representative data of exemplary embodiment lubricating grease of the present invention.
The representative data of table 1 sample of the present invention and existing lubricating grease
1. test method: with the lubricating grease cone penetration box of packing into, in 200 ℃ baking oven, place 24h, then take out and survey immediately its cone penetration.As shown in Table 1, the high-temperature behavior of lubricating grease of the present invention, abrasion resistance and prevent that the copper corrosion performance is all better.
Lubricating grease of a kind of carbon nanotubes that the present invention proposes and preparation method thereof, be described by preferred embodiment, person skilled obviously can be within not breaking away from content of the present invention, spirit and scope to component as herein described with method is changed or suitably change and combination, realize the technology of the present invention.Special needs to be pointed out is, the replacement that all are similar and change apparent to those skilled in the artly, they are deemed to be included in spirit of the present invention, scope and the content.
Claims (10)
1. the lubricating grease of a carbon nanotubes, it is characterized in that forming and the quality percentage composition as follows:
Viscosifying agent is wilkinite: 5-20%;
Base oil is refined mineral oil or synthetic oil: 70-90%;
Solid packing: 0.5-3%;
Polarity dispersion aids: be the 30-60% of organobentonite quality.
2. lubricating grease claimed in claim 1 is characterized in that described wilkinite is the organic amine modified alta-mud.
3. lubricating grease claimed in claim 1 is characterized in that 100 ℃ of viscosity of described base oil are 5～50mm
2/ s, base oil comprise a kind of in paraffin base mineral oil, naphthenic mineral oil, synthetic hydrocarbon lubricating oil, polysiloxane based lubricating oil or the lubricating oil in esters.
4. the described lubricating grease of claim 1 is characterized in that described solid packing is multi-walled carbon nano-tubes.
5. the described lubricating grease of claim 1 is characterized in that described polarity dispersion aids is propylene carbonate.
6. the preparation of greases method of a kind of carbon nanotubes of claim 1, its characterization step is:
(1), the purifying of carbon nanotube and brachymemma: the initial carbon nanotube is added in the nitration mixture, ultrasonic in 50～80 ℃ water-bath, remove wherein impurity and catalyst residue particle, then use deionized water wash, and with the tetrafluoroethylene filtering with microporous membrane in 0.35～0.55 μ m aperture, until the pH value is 7, then in 80 ℃ of vacuum drying ovens, more than the dry 12h, make the carbon nanotube of purifying brachymemma;
(2), the carbon nanotube of processing is joined in whole base oils, under high-speed stirring, be heated to 90～100 ℃, until being distributed in the base oil of even carbon nanotube;
(3), subsequently add organobentonite and carry out pre-dispersedly, itself and base oil are mixed, stir at least 10min, until the organobentonite complete wetting;
(4), add polarity dispersion aids propylene carbonate, under agitation continue to mix 30～40min, and constantly carry out circulation shear, until thing forms the paste structure of black even in the still, in this process, keep 80～90 ℃ of temperature in the kettle;
(5), thing in the still is ground by homogenizer, namely get grease product.
7. according to preparation of greases method claimed in claim 6, it is characterized in that nitration mixture is that volume ratio is the vitriol oil and the concentrated nitric acid of 3:1.
8. according to preparation of greases method claimed in claim 6, the speed that it is characterized in that high-speed stirring is 3000～6000rpm.
9. according to preparation of greases method claimed in claim 6, it is characterized in that the most correct interpolation program of organobentonite and polarity dispersion aids is: 1. organobentonite auxiliary rheological agents; 2. interfacial agent (wetting agent, dispersion agent etc.).
10. according to lubricating grease claimed in claim 1, it is characterized in that, can also add oxidation inhibitor, rust-preventive agent, other extreme pressure anti-wear additives, structural stabilizing agent, tensio-active agent etc. in the lubricating grease.
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| CN2012104189297A CN102911774A (en) | 2012-10-26 | 2012-10-26 | Lubricating grease containing carbon nanotubes and preparation method of lubricating grease |
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| CN2012104189297A CN102911774A (en) | 2012-10-26 | 2012-10-26 | Lubricating grease containing carbon nanotubes and preparation method of lubricating grease |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105154204A (en) * | 2015-08-25 | 2015-12-16 | 俞凤鸣 | Novel lubricating grease |
| CN105586128A (en) * | 2015-12-09 | 2016-05-18 | 中国石油集团石油管工程技术研究院 | Thread compound special for drill collar and preparation method of thread compound |
| CN105647612A (en) * | 2014-11-14 | 2016-06-08 | 中国科学院宁波材料技术与工程研究所 | Lubricating grease containing a nanometer carbon material and a preparing method thereof |
| CN106367182A (en) * | 2016-08-31 | 2017-02-01 | 四川碳世界科技有限公司 | Lubricating oil containing carbon nanotube antiwear agent, and preparation method of lubricating oil |
| CN108822927A (en) * | 2018-03-30 | 2018-11-16 | 深圳市合诚润滑材料有限公司 | A kind of lubricating grease and preparation method thereof for CV joint for car |
| CN111808431A (en) * | 2020-07-02 | 2020-10-23 | 上海鸿辉光通科技股份有限公司 | Optical fiber filling paste with ultralow loss to optical fiber and preparation method thereof |
| CN112048354A (en) * | 2020-09-23 | 2020-12-08 | 上海虎头化工有限公司 | Long-acting high-temperature lubricating grease and preparation method thereof |
| CN112080329A (en) * | 2020-09-21 | 2020-12-15 | 中国科学院兰州化学物理研究所 | Multi-wall carbon nanotube nano friction reducer and application thereof |
| CN113372984A (en) * | 2021-06-29 | 2021-09-10 | 上海鸿辉光通科技股份有限公司 | Filling paste for semiconductive cable and preparation method thereof |
| CN114921281A (en) * | 2022-05-02 | 2022-08-19 | 杭州富阳金容润滑油脂有限公司 | Novel lubricating grease and production process thereof |
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| CN1847374A (en) * | 2006-04-14 | 2006-10-18 | 杨东彤 | Prepn process of carbon nanotube friction-reducing reinforcer |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105647612A (en) * | 2014-11-14 | 2016-06-08 | 中国科学院宁波材料技术与工程研究所 | Lubricating grease containing a nanometer carbon material and a preparing method thereof |
| CN105647612B (en) * | 2014-11-14 | 2018-07-06 | 中国科学院宁波材料技术与工程研究所 | A kind of lubricating grease containing nano-carbon material and preparation method thereof |
| CN105154204A (en) * | 2015-08-25 | 2015-12-16 | 俞凤鸣 | Novel lubricating grease |
| CN105586128A (en) * | 2015-12-09 | 2016-05-18 | 中国石油集团石油管工程技术研究院 | Thread compound special for drill collar and preparation method of thread compound |
| CN106367182A (en) * | 2016-08-31 | 2017-02-01 | 四川碳世界科技有限公司 | Lubricating oil containing carbon nanotube antiwear agent, and preparation method of lubricating oil |
| CN108822927A (en) * | 2018-03-30 | 2018-11-16 | 深圳市合诚润滑材料有限公司 | A kind of lubricating grease and preparation method thereof for CV joint for car |
| CN111808431A (en) * | 2020-07-02 | 2020-10-23 | 上海鸿辉光通科技股份有限公司 | Optical fiber filling paste with ultralow loss to optical fiber and preparation method thereof |
| CN112080329A (en) * | 2020-09-21 | 2020-12-15 | 中国科学院兰州化学物理研究所 | Multi-wall carbon nanotube nano friction reducer and application thereof |
| CN112048354A (en) * | 2020-09-23 | 2020-12-08 | 上海虎头化工有限公司 | Long-acting high-temperature lubricating grease and preparation method thereof |
| CN113372984A (en) * | 2021-06-29 | 2021-09-10 | 上海鸿辉光通科技股份有限公司 | Filling paste for semiconductive cable and preparation method thereof |
| CN113372984B (en) * | 2021-06-29 | 2023-03-10 | 上海鸿辉光通科技股份有限公司 | Filling paste for semiconductive cable and preparation method thereof |
| CN114921281A (en) * | 2022-05-02 | 2022-08-19 | 杭州富阳金容润滑油脂有限公司 | Novel lubricating grease and production process thereof |
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Application publication date: 20130206 |