CN106398804A - Carbon nanotube anti-wear reagent for lubricating oil and preparation method thereof - Google Patents
Carbon nanotube anti-wear reagent for lubricating oil and preparation method thereof Download PDFInfo
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- CN106398804A CN106398804A CN201610773707.5A CN201610773707A CN106398804A CN 106398804 A CN106398804 A CN 106398804A CN 201610773707 A CN201610773707 A CN 201610773707A CN 106398804 A CN106398804 A CN 106398804A
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- Prior art keywords
- lubricating oil
- preparation
- carbon nano
- ball milling
- antiwear additive
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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
- C10M125/02—Carbon; Graphite
-
- 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
- C10M159/00—Lubricating compositions characterised by the additive being of unknown or incompletely defined constitution
- C10M159/12—Reaction products
-
- 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
- C10M163/00—Lubricating compositions characterised by the additive being a mixture of a compound of unknown or incompletely defined constitution and a non-macromolecular compound, each of these compounds being essential
-
- 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
-
- 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
- C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
- C10M2207/10—Carboxylix acids; Neutral salts thereof
- C10M2207/12—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms
- C10M2207/125—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids
- C10M2207/126—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids monocarboxylic
-
- 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
- C10M2229/00—Organic macromolecular compounds containing atoms of elements not provided for in groups C10M2205/00, C10M2209/00, C10M2213/00, C10M2217/00, C10M2221/00 or C10M2225/00 as ingredients in lubricant compositions
-
- 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
-
- 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
- C10N2030/76—Reduction of noise, shudder, or vibrations
-
- 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
- C10N2040/00—Specified use or application for which the lubricating composition is intended
- C10N2040/25—Internal-combustion engines
-
- 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
- C10N2070/00—Specific manufacturing methods for lubricant compositions
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Lubricants (AREA)
Abstract
The invention discloses a carbon nanotube anti-wear reagent for lubricating oil and a preparation method thereof, and belongs to the field of lubricating oil additives. Multiwalled carbon nanotubes are used as a raw material, purification is carried out with concentrated sulfuric acid for 0.5-2 hours, and ball milling treatment is carried out, and the anti-wear reagent is obtained. After impurities in the multiwalled carbon nanotubes are removed, ball milling is carried out in order to obtain the anti-wear reagent for lubricating oil, the anti-wear reagent is dispersed in the lubricating oil, and dispersibility is obviously improved; compared with common lubricating oil, the lubricating oil with the anti-wear reagent added can obviously reduce noise in the engine, reduce loss of mechanical energy of engines due to friction, and improve engine power output.
Description
Technical field
The present invention relates to lubricant additive field, more particularly, to a kind of carbon nano-tube lubricant antiwear additive and its preparation side
Method.
Background technology
Lubricating oil is used in all kinds automobile, in plant equipment to reduce friction, the liquid of protection machinery and workpiece
Or semisolid lubricants, act primarily as the effect such as lubrication.Lubricant effect in order to strengthen lubricating oil acts on, and usually adds in lubricating oil
Enter certain additive, such as antiwear additive, for reducing friction so that machinery obtains sufficient lubrication, so that the efficiency of machinery
Improve, reduce energy resource consumption, prolonged mechanical life-span.
The species of antiwear additive is a lot, and wherein, CNT is a kind of new anti-friction material.
Nanoparticle, due to its special physical and chemical performance and less particle size, becomes as lube oil additive
Study hotspot for lubricating area in recent years.In the Nanoparticles as Additive in Liquid Paraffin having researched and developed, including simple substance nano-powder
As Nano diamond granule, nano-oxide and sulfide, nano inorganic salt and high molecular nano-microsphere, metal such as Cu etc., and
Propose " micro- bearing ", " lubricating film ', the multiple wear-resistant and Mechanism of Friction Reduction such as " the 3rd body reparation " and " surface polishing repair ".
CNT has high toughness, and structure is similar to graphite and C60, and its tube wall has the hexagon knot of graphite linings
Structure, therefore has excellent self-lubricating property.CNT is added to formation composite in other materials, profit as enhancing
With its special tubular structure and high tenacity, have been achieved for certain at the raising aspect such as matrix mechanical property and anti-wear performance
Progress.
At present, had using CNT as lube oil additive report, such as Chinese Patent Application No.
200510031996th, patent name：A kind of method preparing carbon nano-tube lubricant；Such as Chinese Patent Application No. again
200610043593rd, a kind of preparation method of carbon nanotube friction-reducing reinforcer of patent name, and such as Chinese Patent Application No.
2007103085783rd, patent name：A kind of preparation method of multi-walled carbon nano-tubes lube oil additive.Above-mentioned patent report,
All there is a problem of that preparation method is complicated, preparation cost is high, and, being uniformly dispersed, the aspect such as abrasion resistance, however it remains carry
Rise space.
Content of the invention
The purpose of the present invention is that provides a kind of preparation method of carbon nano-tube lubricant antiwear additive, to solve above-mentioned asking
Topic.
To achieve these goals, the technical solution used in the present invention is such：A kind of carbon nano-tube lubricant antiwear additive
Preparation method, is raw material using multi-walled carbon nano-tubes, through concentrated sulphuric acid purification 0.5-2 h, then carries out ball-milling treatment, obtains final product.
Carbon nanotube diameter after being processed using this method is 20～60 nm, purity>97%.
As preferred technical scheme：Described multi-walled carbon nano-tubes is prepared from for catalytic cracking of hydrocarbon method.
The preparation method of multi-walled carbon nano-tubes is more, such as chemical vapour deposition technique, and its ultimate principle is containing carbon source
Gas（Or steam）Flow through and decompose during catalyst surface, generate CNT, conventional carbon-source gas have C6H6、 C2H2、C2H4
Deng.Yacaman etc. adopts earliest 25% ferrum/graphite granule as catalyst, decomposes 9% acetylene/nitrogen system during lower 700 DEG C of normal pressure
Obtain CNT；It is catalyst that Amelincks etc. adopts Co, and ethylene obtains spiral helicine CNT, Chinese science for carbon source
Institute's CAS Institute of Physics chemical vapour deposition technique high-volume has synthesized the CNT of marshalling, and port is opened.This Shen
" catalytic cracking of hydrocarbon method " please refers to aforesaid " chemical vapour deposition technique ".
As preferred technical scheme：During ball milling, ball-milling treatment 0.5-2h under 400-600 r/min.Suitable ball milling
Speed and time, the performance of gained antiwear additive can be improved further.
As preferred technical scheme：During ball milling, ball milling often carries out 15 min and stops 10 min.Mechanical milling process can be prevented
Middle heating is serious.
The present invention also provides the lubrication oil antiwear agent that a kind of said method prepares.
CNT after above-mentioned ball milling is added in lubricating oil well prepared in advance, being simultaneously introduced mass ratio is 0.01
~ 2% dispersant, mass ratio is 0.01 ~ 1% emulsifying agent, ultrasonic disperse 20 min, then is sufficiently stirred for, and obtains containing different quality
The lubricating oil of fraction CNT, the mass fraction scope of its CNT is 0.01 ~ 5%；Wherein, described dispersant is main
Composition is siliceous surfactant and montanic acid resin blends；Described emulsifying agent is sodium stearate and Fructus Gleditsia emulsifying agent.
Compared with prior art, it is an advantage of the current invention that：Ball milling after multi-walled carbon nano-tubes remove impurity is moistened by the present invention
Lubricating oil antiwear additive, is scattered in lubricating oil, and its dispersibility significantly improves, and compared to common lubricating oil, adds this
The lubricating oil of bright antiwear additive can significantly reduce the noise of electromotor, and noise can reduce by more than 30%, reduce electromotor because
The mechanical energy loss 10.3% rubbing and producing.
Specific embodiment
Below in conjunction with embodiment, the invention will be further described.
Embodiment 1：
A kind of carbon nano-tube lubricant antiwear additive, its preparation method is：
The multi-walled carbon nano-tubes that selection catalytic cracking of hydrocarbon method is prepared, removes remaining through concentrated sulphuric acid purification 1 h
The impurity such as catalyst granules, then ball-milling treatment 1h under 500 r/min, in order to prevent serious, the ball that generates heat in mechanical milling process
Mill often carries out 15 min and stops 10 min, and the carbon nanotube diameter after process is 20～60 nm, purity>97%；
CNT after ball milling is added in lubricating oil well prepared in advance, being simultaneously introduced mass ratio is 0.02% dispersant,
Mass ratio is 0.08% emulsifying agent, ultrasonic disperse 20 min, then is sufficiently stirred for, and obtaining mass fraction is 0.05% CNT lubrication
Oil.
Lubricating oil after blending is carried out subpackage, carries out the experiment of storage stability, the shuttle after 12 months simultaneously
Have no the CNT of sedimentation, liquid oil stable homogeneous.
Embodiment 2：
A kind of carbon nano-tube lubricant antiwear additive, its preparation method is：
The multi-walled carbon nano-tubes that selection catalytic cracking of hydrocarbon method is prepared, removes residual through concentrated sulphuric acid purification 0.5 h
The impurity such as remaining catalyst granules, then ball-milling treatment 2h under 400 r/min, in order to prevent generating heat seriously in mechanical milling process,
Ball milling often carries out 15 min and stops 10 min, and the carbon nanotube diameter after process is 20～60 nm, purity>97%；
CNT after ball milling is added in lubricating oil well prepared in advance, being simultaneously introduced mass ratio is 0.01% dispersant,
Mass ratio is 0.01% emulsifying agent, ultrasonic disperse 20 min, then is sufficiently stirred for, and obtaining mass fraction is 0.02% CNT lubrication
Oil.
Lubricating oil after blending is carried out subpackage, carries out the experiment of storage stability, the shuttle after 12 months simultaneously
Have no the CNT of sedimentation, liquid oil stable homogeneous.
Embodiment 3：
A kind of carbon nano-tube lubricant antiwear additive, its preparation method is：
The multi-walled carbon nano-tubes that selection catalytic cracking of hydrocarbon method is prepared, removes remnants' through concentrated sulphuric acid purification 2h
The impurity such as catalyst granules, then ball-milling treatment 0.5h under 600 r/min, in order to prevent serious, the ball that generates heat in mechanical milling process
Mill often carries out 15 min and stops 10 min, and the carbon nanotube diameter after process is 20～60 nm, purity>97%；
CNT after ball milling is added in lubricating oil well prepared in advance, being simultaneously introduced mass ratio is 2% dispersant, matter
Amount ratio is 0.01% emulsifying agent, ultrasonic disperse 20 min, then is sufficiently stirred for, and obtaining mass fraction is 5% carbon nano-tube lubricant.
Lubricating oil after blending is carried out subpackage, carries out the experiment of storage stability, the shuttle after 12 months simultaneously
Have no the CNT of sedimentation, liquid oil stable homogeneous.
Embodiment 4 performance test
Big Cherokee version in 2014,100 kilometers of tests of highway, speed 80km/ hour；Using common lubricant, its oil consumption
For 12.6L；Add the antiwear additive that embodiment 1 is obtained, adding proportion is 0.05%, its oil consumption is 10.8L, fuel-economizing 14.3% is started
Machine starts steadily, and power output is stable.In-car noise, by 65 decibels, is reduced to 40 decibels.
Embodiment 5 performance test
Buick Regal version in 2015,100 kilometers of tests of highway, speed 80km/ hour；Using common lubricant, its oil consumption
For 9.6L；Add the antiwear additive that embodiment 1 is obtained, adding proportion is 0.03%, its oil consumption is 7.8L, fuel-economizing 18.7%, electromotor
Start steadily, power output is stable.
Embodiment 6 antiwear and friction reduction property is tested
Model machine, under flameout state, drags electromotor with electric dynamometer, uses base lubricant oils and carbon nano-tube lubricant respectively
Tested, the mechanical loss power comparative test result of electromotor is shown in Table 1.
Table 1 model machine mechanical loss power result of the test
Note：Rate of change=（Carbon nano-tube lubricant base lubricant oils）÷ base lubricant oils × 100%
The foregoing is only presently preferred embodiments of the present invention, not in order to limit the present invention, all spirit in the present invention and
Any modification, equivalent and improvement of being made within principle etc., should be included within the scope of the present invention.
Claims (5)
1. a kind of preparation method of carbon nano-tube lubricant antiwear additive it is characterised in that：It is raw material using multi-walled carbon nano-tubes, warp
Concentrated sulphuric acid purification 0.5-2 h, then carries out ball-milling treatment, obtains final product.
2. carbon nano-tube lubricant antiwear additive according to claim 1 preparation method it is characterised in that：Described many walls carbon
Nanotube is prepared from for catalytic cracking of hydrocarbon method.
3. carbon nano-tube lubricant antiwear additive according to claim 1 preparation method it is characterised in that：During ball milling,
Ball-milling treatment 0.5-2h under 400-600 r/min.
4. carbon nano-tube lubricant antiwear additive according to claim 1 preparation method it is characterised in that：
During ball milling, ball milling often carries out 15 min and stops 10 min.
5. the lubrication oil antiwear agent that the method for claim 1-5 any one prepares.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610773707.5A CN106398804A (en) | 2016-08-31 | 2016-08-31 | Carbon nanotube anti-wear reagent for lubricating oil and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610773707.5A CN106398804A (en) | 2016-08-31 | 2016-08-31 | Carbon nanotube anti-wear reagent for lubricating oil and preparation method thereof |
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| CN106398804A true CN106398804A (en) | 2017-02-15 |
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| CN201610773707.5A Pending CN106398804A (en) | 2016-08-31 | 2016-08-31 | Carbon nanotube anti-wear reagent for lubricating oil and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113512456A (en) * | 2018-11-12 | 2021-10-19 | 东莞理工学院 | Preparation process of lubricating oil containing cuprous oxide composite modified graphene |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1528870A (en) * | 2003-07-01 | 2004-09-15 | 李幼清 | Nano antiwear agent, and preparing method and use thereof |
| EP1893528A1 (en) * | 2005-06-20 | 2008-03-05 | Nanocyl S.A. | Method for producing carbon nanotubes |
| WO2007033438A9 (en) * | 2005-09-20 | 2008-04-24 | Nanocyl Sa | Catalyst system for a multi -walled carbon nanotube production process |
| CN103154215A (en) * | 2010-09-28 | 2013-06-12 | 道达尔炼油与销售部 | Lubricant composition |
-
2016
- 2016-08-31 CN CN201610773707.5A patent/CN106398804A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1528870A (en) * | 2003-07-01 | 2004-09-15 | 李幼清 | Nano antiwear agent, and preparing method and use thereof |
| EP1893528A1 (en) * | 2005-06-20 | 2008-03-05 | Nanocyl S.A. | Method for producing carbon nanotubes |
| WO2007033438A9 (en) * | 2005-09-20 | 2008-04-24 | Nanocyl Sa | Catalyst system for a multi -walled carbon nanotube production process |
| CN103154215A (en) * | 2010-09-28 | 2013-06-12 | 道达尔炼油与销售部 | Lubricant composition |
Non-Patent Citations (4)
| Title |
|---|
| 张玉龙等: "《纳米技术与纳米塑料》", 30 April 2002, 中国轻工业出版社 * |
| 徐鼐: "《通用级聚乳酸的改性与加工成型》", 31 January 2016, 中国科学技术大学出版社 * |
| 施利毅等: "《纳米材料》", 31 January 2007, 华东理工大学出版社 * |
| 黄启忠等: "《高性能炭/炭复合材料制备、结构与应用》", 31 December 2010, 中南大学出版社 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113512456A (en) * | 2018-11-12 | 2021-10-19 | 东莞理工学院 | Preparation process of lubricating oil containing cuprous oxide composite modified graphene |
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Application publication date: 20170215 |