CN110387281A - Carbon nanotube/zero dimensional nanometer materials composite material and its preparation method and application - Google Patents
Carbon nanotube/zero dimensional nanometer materials composite material and its preparation method and application Download PDFInfo
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- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M141/00—Lubricating compositions characterised by the additive being a mixture of two or more compounds covered by more than one of the main groups C10M125/00 - C10M139/00, each of these compounds being essential
- C10M141/06—Lubricating compositions characterised by the additive being a mixture of two or more compounds covered by more than one of the main groups C10M125/00 - C10M139/00, each of these compounds being essential at least one of them being an organic nitrogen-containing compound
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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
- C10M161/00—Lubricating compositions characterised by the additive being a mixture of a macromolecular compound and a non-macromolecular compound, each of these compounds being essential
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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
- C10M2201/04—Elements
- C10M2201/041—Carbon; Graphite; Carbon black
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- 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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- 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
- C10M2201/14—Inorganic compounds or elements as ingredients in lubricant compositions inorganic compounds surface treated with organic compounds
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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
- C10M2203/00—Organic non-macromolecular hydrocarbon compounds and hydrocarbon fractions as ingredients in lubricant compositions
- C10M2203/10—Petroleum or coal fractions, e.g. tars, solvents, bitumen
- C10M2203/1006—Petroleum or coal fractions, e.g. tars, solvents, bitumen used as base 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
- C10M2215/00—Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
- C10M2215/02—Amines, e.g. polyalkylene polyamines; Quaternary amines
- C10M2215/04—Amines, e.g. polyalkylene polyamines; Quaternary amines having amino groups bound to acyclic or cycloaliphatic carbon atoms
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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
- C10M2217/00—Organic macromolecular compounds containing nitrogen as ingredients in lubricant compositions
- C10M2217/06—Macromolecular compounds obtained by functionalisation op polymers with a nitrogen containing compound
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- 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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Abstract
The present invention relates to a kind of carbon nanotube/zero dimensional nanometer materials composite materials, it is characterized in that, carbon nanotube and zero dimensional nanometer materials obtain modified carbon nano-tube and modified zero dimensional nanometer materials through oiliness dispersing agent is modified respectively, obtain the carbon nanotube/zero dimensional nanometer materials composite material after loaded modified zero dimensional nanometer materials on modified carbon nano-tube.Gained carbon nanotube/zero dimensional nanometer materials composite material of the invention can be used as lubrication anti-wear agent, is added in lubricating oil, can be effectively improved the abrasion resistance of lubricating oil, and cost is relatively low for the method for the invention, easy to operate, high-efficiency environment friendly is with a wide range of applications.
Description
Technical field
The present invention relates to Material Fields, relate generally to anti-friction material field, and in particular to a kind of carbon nanotube/zero-dimension nano
Composites and its preparation method and application.
Background technique
Specific inorganic nano material is added in lubricating oil can greatly promote the lubrication anti-wear effect of lubricating oil.Often
Nano lubricating added material includes metal and metal oxide nanoparticles, ceramic nanoparticles, rare earth compound nano
Particle, carbon nanomaterial and other inorganic nonmetallic nanometer materials etc..By these nano materials it is uniform and stable be distributed to oil
The lubrication anti-wear effect of raising lubricating oil that can be different degrees of in phase.
ZL201410382805.7 invented it is a kind of by two-dimension nano materials, such as zirconium phosphate nano sheet and zero-dimension nano
Grain greatly improves dispersibility of the two in oily phase, is prepared for if copper nano particles are by the method for collaboration dispersion mixing
The binary lubricating system of different structure nano material, and greatly improve the lubrication anti-wear effect of nano lubricating oil.
A kind of extreme pressure anti-wear additives are disclosed application No. is the patent of invention of 201410345812.X, including silicon powder 1-10%,
Magnesia 0.5-5%, aluminium powder 20-70%, phosphoesterase 30 .5-5%, nickel powder 0.1-1%, two Bians, two sulphur 0.1-1%, molybdenum naphthenate
1-5% and molybdenum disulfide 5-10% can increase the hardness of piece surface, improve wearability, extend the working life of friction parts.
Application No. is 201510508363.0 patents of invention to disclose a kind of engine oil antiwear additive, has base oil, resists
Oxygen agent, detersive, dispersing agent, extreme pressure anti-wear additives, rust oxidation, pour-point depressant, metal deactivator, Nano-Zinc, tungsten disulfide group
At the extreme pressure anti-wear additives are trithiophenyl phosphate.This antiwear additive can give full play to comprehensive effect of lubricating oil, set to machinery
Standby senile abrasion has very strong repair.
Summary of the invention
Technical problem solved by the present invention is lubrication oil antiwear agent at present the phenomenon that there are still flocculation or precipitatings, and cost
Higher, the abrasion resistance of lubricating oil need to be improved.
In order to solve the above technical problems, the present invention provide it is a kind of by monodimension nanometer material carbon nanotube and zero-dimension nano particle
Method that is compound, preparing nano lubricating antiwear additive and nano lubricating oil, is found by friction testing, it is this and meanwhile include it is one-dimensional with
The effect of the structure composite type nano lubricating oil of zero dimensional nanometer materials is better than the nano material of each exclusive use.
Specifically, in view of the deficiencies of the prior art, the present invention provides the following technical scheme that
A kind of carbon nanotube/zero dimensional nanometer materials composite material, which is characterized in that carbon nanotube and zero dimensional nanometer materials point
Modified carbon nano-tube and modified zero dimensional nanometer materials are not obtained through oiliness dispersing agent is modified, loads and changes on modified carbon nano-tube
The carbon nanotube/zero dimensional nanometer materials composite material is obtained after property zero dimensional nanometer materials.
Preferably, in above-mentioned composite material, the oiliness dispersing agent is selected from fat primary amine or polyetheramine.
Preferably, in above-mentioned composite material, the zero dimensional nanometer materials are selected from metal or metallic compound, the metal choosing
From magnesium, aluminium and positioned at the 4th period of the periodic table of elements and the 5th period and belong to IB, IIB, IIIB, IVB, VB, VIB, VIIB,
One or more of VIII, IIIA, IVA race metallic element, be preferably selected from copper, zinc, magnesium, aluminium, titanium, zirconium, tin, in iron
It is one or more kinds of；The metallic compound is the oxide of one or more kinds of above-mentioned metals.
Wherein, the metallic compound is selected from the one or more of zirconium oxide, copper oxide, titanium oxide or aluminium oxide.
Preferably, in above-mentioned composite material, the mass ratio of the carbon nanotube and oiliness dispersing agent total amount is (0.5-
2.5): 20, preferably (0.5-2): 20.
Preferably, in above-mentioned composite material, the mass ratio of the zero dimensional nanometer materials and oiliness dispersing agent total amount is (1-
10): 20, preferably (1-5): 20.
Preferably, in above-mentioned composite material, the total amount of carbon nanotube and zero dimensional nanometer materials and the quality of oiliness dispersing agent
Than for (2-6): 20, it is furthermore preferred that the mass ratio of carbon nanotube and the total amount of zero dimensional nanometer materials and oiliness dispersing agent is (3.5-
6): 20.
Preferably, in above-mentioned composite material, the mass ratio of zero dimensional nanometer materials and carbon nanotube is (1-10): 1, more preferably
, the mass ratio of zero dimensional nanometer materials and carbon nanotube is (3-6): 1.
Preferably, carbon nanotube: zero dimensional nanometer materials: dispersing agent=1:3:20.
Preferably, in above-mentioned composite material, the length of the carbon nanotube is 10nm -10 μm, diameter 2nm-50nm.
Preferably, in above-mentioned composite material, the partial size of the zero dimensional nanometer materials is 10nm-10 μm.
Preferably, in above-mentioned composite material, the fat primary amine main chain includes the saturated hydrocarbyl that carbon chain lengths are C6-C22
Or the primary amine of C6-C22 unsaturated alkyl, it is preferred that the unsaturated alkyl is alkylene.
Preferably, in above-mentioned composite material, the number of carbon-carbon double bond is 1-4 in the alkylene.
Preferably, the carbon chain lengths of the primary amine are preferably C12-C20.
It is furthermore preferred that the carbon chain lengths of the primary amine are C18, the primary amine is oleyl amine, i.e. 9- octadecenyl amine.
Preferably, in above-mentioned composite material, the polyetheramine main chain is polyether structure, and amidine functional group is contained in end；It is excellent
Choosing, the quantity of ether is 5-100 in the polyetheramine
Preferably, in above-mentioned composite material, the composite material is prepared by the method comprising following step:
(1) by carbon nanotube and oiliness dispersant, modified carbon nano-tube is obtained after reaction；
(2) by zero dimensional nanometer materials and oiliness dispersant, modified zero dimensional nanometer materials are obtained after reaction；
(3) after mixing the modified carbon nano-tube and the modified zero dimensional nanometer materials, carbon nanotube/zero is obtained
Dimension nano material composite material.
The present invention also provides a kind of composite Nano lubricating oil, which is characterized in that including above-mentioned carbon nanotube/zero-dimension nano material
Expect composite material and lubricating oil.
Preferably, in above-mentioned composite Nano lubricating oil, the mass ratio of the composite material and lubricating oil is (0.5-5):
100, preferably (0.5-3): 100.
Preferably, the mass ratio of the composite material and lubricating oil is (1.0-3): 100, more preferably 3:100.
Preferably, in above-mentioned composite Nano lubricating oil, the coefficient of friction of the composite Nano lubricating oil is 0.15-0.4, excellent
It is selected as 0.2-0.3, wear scar diameter 1.0-3.0, preferably 1.0-2.0.
The present invention also provides above-mentioned carbon nanotube/zero dimensional nanometer materials composite material preparation methods, which is characterized in that packet
Include following step:
(1) by carbon nanotube and oiliness dispersant, modified carbon nano-tube is obtained after reaction；
(2) by zero dimensional nanometer materials and oiliness dispersant, modified zero dimensional nanometer materials are obtained after reaction；
(3) after mixing the modified carbon nano-tube and the modified zero dimensional nanometer materials, carbon nanotube/zero is obtained
Dimension nano material composite material.
Preferably, in above-mentioned preparation method, in step (1), the mass ratio of carbon nanotube and oiliness dispersing agent is 1:
(0.01-50), preferably 1:(2-20).
Preferably, in above-mentioned preparation method, in step (2), the mass ratio of zero dimensional nanometer materials and oiliness dispersing agent is 1:
(0.1-50), preferably 1:(1-10).
Preferably, in above-mentioned preparation method, in step (3), by the modified carbon nano-tube and the modified zero-dimension nano
It further include the process of ball milling after material mixing.
The present invention also provides the preparation methods of above-mentioned composite Nano lubricating oil, which is characterized in that includes the following steps:
Above-mentioned carbon nanotube/zero dimensional nanometer materials composite material is added in lubricating oil, composite Nano lubricating oil is obtained.
The present invention also provides above-mentioned carbon nanotube/zero dimensional nanometer materials composite materials or above-mentioned composite Nano lubricating oil to moisten
The application in lubricating oil field.
In the present invention, the zero dimensional nanometer materials refer to that at least one dimension is in nanoscale range in three-dimensional space
The particle of (1-100nm).
The invention has the advantages that the present invention gained carbon nanotube/zero dimensional nanometer materials composite material can be used as lubrication it is wear-resistant
Agent is added in lubricating oil, can be effectively improved the abrasion resistance of lubricating oil, and cost is relatively low for the method for the invention, operation letter
Single, high-efficiency environment friendly is with a wide range of applications.
Detailed description of the invention
Fig. 1 is the transmission electron microscope figure of 1 gained zirconium oxide of embodiment.
Fig. 2 is the transmission electron microscope figure of multi-walled carbon nanotube used in embodiment 1.
Specific embodiment
It need to be improved in view of the abrasion resistance of current lubricating oil, the present invention provides a kind of carbon nanotube/zero-dimension nano material
Expect composite material and the compounded lubricating oil comprising this material, uses oiliness dispersing agent modified respectively carbon nanotube and zirconium oxide
Afterwards, then by modified zirconia it is carried on modified carbon nano-tube, composite material is made, this material is added in lubricating oil, it can pole
The big abrasion resistance for improving lubricating oil.
In a kind of preferred embodiment, composite material of the present invention the preparation method comprises the following steps: by carbon nanotube and oxidation
Zirconium nano particle is separately added into oleyl amine, is stirred to be placed in ball mill and be taken out after grinding 30min, obtains carbon nanotube-
Zirconia nanopowder lubrication anti-wear agent.Wherein: the mass ratio of carbon nanotube and Zirconium oxide nano grain is 1:(1-5), preferably
1:3。
Monodimension nanometer material: carbon nanotube: single-walled carbon nanotube or multi-walled carbon nanotube and its derivative, carbon nanotube are come
Source: Nanometer Port Co., Ltd., Shenzhen.
Oil-soluble dispersant: oleyl amine or other oil-soluble dispersants.The oleyl amine that this experiment uses is from Aladdin Reagent Company
Purchase.
In the present invention, the oiliness dispersing agent is selected from fat primary amine or polyetheramine.
The fat primary amine refers to that main chain includes the saturated hydrocarbyl that carbon chain lengths are C6-C22 or the unsaturation of C6-C22
Amidine functional group is contained in alkyl, end.Such as: n-hexylamine, n-octyl amine, n-Decylamine, n-dodecylamine or oleyl amine etc..
Preferably, the unsaturated alkyl of the fat primary amine is alkylene, it is furthermore preferred that carbon-carbon double bond in the alkylene
Number be 1-4.
Preferably, the carbon chain lengths of the primary amine be C12-C20, more preferably 18, the primary amine be oleyl amine, i.e. 9- ten
Eight enamines.
Polyetheramine of the present invention refers to that main chain is polyether structure, and the polymer of amidine functional group is contained in end, such as:
Jeffamine polyetheramine D230, D400, D2000 or T403 etc..
Preferably, the quantity of ether is 5-100 in the polyetheramine, such as: polyetheramine D2000, ether number are 33
It is a.
Preferably formula is in the present invention: containing nano combined lubrication anti-wear agent 3.0% in lubricating oil, wherein nano combined
Lubricate carbon nanotube in antiwear additive: zirconium oxide: oleyl amine=1:3:20.
Zirconium oxide is a kind of zero dimension inorganic nanoparticles material, in the present invention, the synthesis side of the Zirconium oxide nano grain
Method includes the following steps:
Ammonium hydroxide is added in zirconium oxychloride aqueous solution, adjusting pH is 8-10, after sample is washed drying after reaction, in 800-
1000 DEG C of calcining 2-5h, obtain zirconium oxide；Wherein, the concentration of basic zirconium chloride be 0.2-0.5mol/L, zirconium oxychloride aqueous solution with
The volume ratio of ammonium hydroxide is 100:(0.1-10).
In a kind of preferred embodiment, zirconium oxide the preparation method comprises the following steps: preparing ZrOCl2·8H2O's (Aladdin purchase)
Molar concentration is the aqueous solution of 0.2mol/L, after being uniformly mixed, appropriate ammonium hydroxide is added into mixed liquor, adjusts mixed liquor
PH=9, sample after the filtering and washing dry 2h at 100 DEG C, later 900 DEG C of high-temperature calcination 2h.
Wherein, oil-soluble dispersant is oleyl amine or oil soluble polyether amine etc..
In another preferred embodiment, the formula of compounded lubricating oil of the present invention are as follows: ground nano lubricating
Antiwear additive is added in basic mineral oil (Shuan Long lubricating oil Science and Technology Ltd., South Korea) that mechanical stirring is uniform, is prepared into nanometer profit
Lubricating oil.Concentration of the antiwear additive in lubricating oil be 0.5-5%, preferably 3%.
Nano lubricating oil is subjected to ball disk method friction testing by ASTM G99-95 standard.
Carbon nanotube of the present invention/zero dimensional nanometer materials composite wood is further illustrated below by specific embodiment
Material, compounded lubricating oil and its preparation method and application.
In the following embodiments, the information of each reagent used and instrument is as follows:
Agents useful for same information in 1 embodiment of the present invention of table
| Experimental material | Specification | Producer |
| ZrOCl2.8H2O | Purity: 99% | Shanghai Aladdin biochemical technology limited liability company |
| Mineral oil | Saybolt viscosity: 250N | Shuan Long lubricating oil Science and Technology Ltd., South Korea |
| Single-walled carbon nanotube | Ash content: < 3% | Nanometer Port Co., Ltd., Shenzhen |
| Multi-walled carbon nanotube | Ash content: < 3% | Nanometer Port Co., Ltd., Shenzhen |
| Oleyl amine | 9- octadecenyl amine | Shanghai Aladdin biochemical technology limited liability company |
| N-hexylamine | Shanghai Aladdin biochemical technology limited liability company | |
| N-dodecylamine | Shanghai Aladdin biochemical technology limited liability company | |
| Polyetheramine D2000 | Shanghai Aladdin biochemical technology limited liability company | |
| Titanium oxide | Shanghai Aladdin biochemical technology limited liability company | |
| Magnesia | Shanghai Aladdin biochemical technology limited liability company |
Device therefor information in 2 embodiment of the present invention of table
| Experimental facilities | Model | Producer |
| Ball mill | YXQM-2L | Changsha meter Qi experimental instruments and equipment limited |
| Batch-type furnace | KSL-1400X | Hefei Ke Jing Materials Technology Ltd. |
| High resolution transmission electron microscopy (TEM) | FEI Tecnai G2F30 | FEI Co., the U.S. |
| Friction and wear test instrument | UMT-2 | German Brooker company |
Embodiment 1
One, the preparation of zirconium oxide
Prepare ZrOCl2·8H2The molar concentration of O is the aqueous solution of 0.2mol/L, mixed to 100ml after being uniformly mixed
It closes and 1ml concentrated ammonia liquor is added in liquid, adjust the pH=9 of mixed liquor, the sample after filtering and washing dry 2h, Zhi Houli at 100 DEG C
With batch-type furnace, 900 DEG C of high-temperature calcination 2h, obtain zirconium oxide in air atmosphere.
The transmission electron microscope figure (TEM figure) of zirconium oxide is as shown in Figure 1, the zirconia particles prepared as seen from the figure
Partial size is 40nm.
Two, carbon nanotube/Zirconia composite nano material preparation
(1) 1g multi-walled carbon nanotube is added in 5g oleyl amine, modified carbon nano-tube is obtained after stirring；
(2) 3g zirconium oxide is added in 15g oleyl amine, modified zirconia is obtained after stirring；
(3) modified carbon nano-tube is added in ball mill with modified zirconia and is mixed, taken out after ball milling 30min, obtain carbon
Nanotube/Zirconia composite nano material.
The transmission electron microscope figure (TEM figure) of raw material multi-walled carbon nanotube as shown in Fig. 2, as seen from the figure, without
The multi-walled carbon nanotube agglomeration of processing is serious.Carbon nanotube/zirconium oxide as obtained by known to transmission electron microscope detection
In composite material, the different nano material of two kinds of structures can be dispersed well.
Three, the preparation of composite Nano lubricating oil
Above-mentioned carbon nanotube/Zirconia composite nano material 0.5g is taken, is added in 100g mineral oil, after mechanical stirring is uniform
Obtain composite Nano lubricating oil, wherein composite nano materials account for the 0.5% of mineral oil quality.
Embodiment 2
One, the preparation of zirconium oxide
Prepare ZrOCl2·8H2The molar concentration of O is the aqueous solution of 0.5mol/L, mixed to 100ml after being uniformly mixed
It closes and 2ml concentrated ammonia liquor is added in liquid, adjust the pH=8 of mixed liquor, the sample after filtering and washing dry 2h, Zhi Houli at 100 DEG C
With batch-type furnace, 800 DEG C of high-temperature calcination 5h, obtain zirconium oxide in air atmosphere.
The partial size that the present embodiment gained zirconium oxide is detected with the identical method of embodiment 1 is 45nm.
Two, carbon nanotube/Zirconia composite nano material preparation
(1) 1g multi-walled carbon nanotube is added in 5g oleyl amine, modified carbon nano-tube is obtained after stirring；
(2) 3g zirconium oxide is added in 15g oleyl amine, modified zirconia is obtained after stirring；
(3) modified carbon nano-tube is added in ball mill with modified zirconia and is mixed, taken out after ball milling 30min, obtain carbon
Nanotube/Zirconia composite nano material.
Three, the preparation of composite Nano lubricating oil
Above-mentioned carbon nanotube/Zirconia composite nano material 1g is taken, is added in 100g mineral oil, after mechanical stirring is uniform
To composite Nano lubricating oil, wherein composite nano materials account for the 1% of mineral oil quality.
Embodiment 3
One, the preparation of zirconium oxide
Prepare ZrOCl2·8H2The molar concentration of O is the aqueous solution of 0.3mol/L, mixed to 100ml after being uniformly mixed
It closes and 1.5ml concentrated ammonia liquor is added in liquid, adjust the pH=10 of mixed liquor, the dry 2h at 100 DEG C of the sample after filtering and washing, later
Using batch-type furnace, 1000 DEG C of high-temperature calcination 2h, obtain zirconium oxide in air atmosphere.
The partial size that the present embodiment gained zirconium oxide is detected with the identical method of embodiment 1 is 43nm.
Two, carbon nanotube/Zirconia composite nano material preparation
(1) 1g multi-walled carbon nanotube is added in 5g oleyl amine, modified carbon nano-tube is obtained after stirring；
(2) 3g zirconium oxide is added in 15g oleyl amine, modified zirconia is obtained after stirring；
(3) modified carbon nano-tube is added in ball mill with modified zirconia and is mixed, taken out after ball milling 30min, obtain carbon
Nanotube/Zirconia composite nano material.
Three, the preparation of composite Nano lubricating oil
Above-mentioned carbon nanotube/Zirconia composite nano material 3g is taken, is added in 100g mineral oil, after mechanical stirring is uniform
To composite Nano lubricating oil, wherein composite nano materials account for the 3% of mineral oil quality.
Embodiment 4
One, the preparation of zirconium oxide
Prepare ZrOCl2·8H2The molar concentration of O is the aqueous solution of 0.2mol/L, mixed to 100ml after being uniformly mixed
It closes and 1ml concentrated ammonia liquor is added in liquid, adjust the pH=9 of mixed liquor, the sample after filtering and washing dry 2h, Zhi Houli at 100 DEG C
With batch-type furnace, 900 DEG C of high-temperature calcination 2h, obtain zirconium oxide in air atmosphere.
The partial size that the present embodiment gained zirconium oxide is detected with the identical method of embodiment 1 is 40nm.
Two, carbon nanotube/Zirconia composite nano material preparation
(1) 1g multi-walled carbon nanotube is added in 5g oleyl amine, modified carbon nano-tube is obtained after stirring；
(2) 3g zirconium oxide is added in 15g oleyl amine, modified zirconia is obtained after stirring；
(3) modified carbon nano-tube is added in ball mill with modified zirconia and is mixed, taken out after ball milling 30min, obtain carbon
Nanotube/Zirconia composite nano material.
Three, the preparation of composite Nano lubricating oil
Above-mentioned carbon nanotube/Zirconia composite nano material 5g is taken, is added in 100g mineral oil, after mechanical stirring is uniform
To composite Nano lubricating oil, wherein composite nano materials account for the 5% of mineral oil quality.
Embodiment 5
One, the preparation of zirconium oxide
Prepare ZrOCl2·8H2The molar concentration of O is the aqueous solution of 0.2mol/L, mixed to 100ml after being uniformly mixed
It closes and 1ml concentrated ammonia liquor is added in liquid, adjust the pH=9 of mixed liquor, the sample after filtering and washing dry 2h, Zhi Houli at 100 DEG C
With batch-type furnace, 900 DEG C of high-temperature calcination 2h, obtain zirconium oxide in air atmosphere.
The partial size that the present embodiment gained zirconium oxide is detected with the identical method of embodiment 1 is 40nm.
Two, carbon nanotube/Zirconia composite nano material preparation
(1) 1g multi-walled carbon nanotube is added in 10g oleyl amine, modified carbon nano-tube is obtained after stirring；
(2) 1g zirconium oxide is added in 10g oleyl amine, modified zirconia is obtained after stirring；
(3) modified carbon nano-tube is added in ball mill with modified zirconia and is mixed, taken out after ball milling 30min, obtain carbon
Nanotube/Zirconia composite nano material.
Three, the preparation of composite Nano lubricating oil
Above-mentioned carbon nanotube/Zirconia composite nano material 3g is taken, is added in 100g mineral oil, after mechanical stirring is uniform
To composite Nano lubricating oil, wherein composite nano materials account for the 3% of mineral oil quality.
Embodiment 6
One, the preparation of zirconium oxide
Prepare ZrOCl2·8H2The molar concentration of O is the aqueous solution of 0.2mol/L, mixed to 100ml after being uniformly mixed
It closes and 1ml concentrated ammonia liquor is added in liquid, adjust the pH=9 of mixed liquor, the sample after filtering and washing dry 2h, Zhi Houli at 100 DEG C
With batch-type furnace, 900 DEG C of high-temperature calcination 2h, obtain zirconium oxide in air atmosphere.
The partial size that the present embodiment gained zirconium oxide is detected with the identical method of embodiment 1 is 40nm.
Two, carbon nanotube/Zirconia composite nano material preparation
(1) 1g multi-walled carbon nanotube is added in 5g oleyl amine, modified carbon nano-tube is obtained after stirring；
(2) 5g zirconium oxide is added in 15g oleyl amine, modified zirconia is obtained after stirring；
(3) modified carbon nano-tube is added in ball mill with modified zirconia and is mixed, taken out after ball milling 30min, obtain carbon
Nanotube/Zirconia composite nano material.
Three, the preparation of composite Nano lubricating oil
Above-mentioned carbon nanotube/Zirconia composite nano material 3g is taken, is added in 100g mineral oil, after mechanical stirring is uniform
To composite Nano lubricating oil, wherein composite nano materials account for the 3% of mineral oil quality.
Embodiment 7
One, the preparation of zirconium oxide
Zirconium oxide is prepared with the identical method of embodiment 1.
Two, carbon nanotube/Zirconia composite nano material preparation
(1) 0.5g single-walled carbon nanotube is added in 5g oleyl amine, modified carbon nano-tube is obtained after stirring；
(2) 3g zirconium oxide is added in 15g oleyl amine, modified zirconia is obtained after stirring；
(3) modified carbon nano-tube is added in ball mill with modified zirconia and is mixed, taken out after ball milling 30min, obtain carbon
Nanotube/Zirconia composite nano material.
Three, the preparation of composite Nano lubricating oil
Above-mentioned carbon nanotube/Zirconia composite nano material 3g is taken, is added in 100g mineral oil, after mechanical stirring is uniform
To composite Nano lubricating oil, wherein composite nano materials account for the 3% of mineral oil quality.
Embodiment 8
One, the preparation of zirconium oxide
Zirconium oxide is prepared with the identical method of embodiment 1.
Two, carbon nanotube/Zirconia composite nano material preparation
(1) 0.5g multi-walled carbon nanotube is added in 10g n-hexylamine, modified carbon nano-tube is obtained after stirring；
(2) 1g zirconium oxide is added in 10g n-hexylamine, modified zirconia is obtained after stirring；
(3) modified carbon nano-tube is added in ball mill with modified zirconia and is mixed, taken out after ball milling 30min, obtain carbon
Nanotube/Zirconia composite nano material.
Three, the preparation of composite Nano lubricating oil
Above-mentioned carbon nanotube/Zirconia composite nano material 3g is taken, is added in 100g mineral oil, after mechanical stirring is uniform
To composite Nano lubricating oil, wherein composite nano materials account for the 3% of mineral oil quality.
Embodiment 9
One, the preparation of zirconium oxide
Zirconium oxide is prepared with the identical method of embodiment 1.
Two, carbon nanotube/Zirconia composite nano material preparation
(1) 0.5g multi-walled carbon nanotube is added in 5g oleyl amine, modified carbon nano-tube is obtained after stirring；
(2) 5g zirconium oxide is added in 15g oleyl amine, modified zirconia is obtained after stirring；
(3) modified carbon nano-tube is added in ball mill with modified zirconia and is mixed, taken out after ball milling 30min, obtain carbon
Nanotube/Zirconia composite nano material.
Three, the preparation of composite Nano lubricating oil
Above-mentioned carbon nanotube/Zirconia composite nano material 3g is taken, is added in 100g mineral oil, after mechanical stirring is uniform
To composite Nano lubricating oil, wherein composite nano materials account for the 3% of mineral oil quality.
Embodiment 10
One, the preparation of zirconium oxide
Zirconium oxide is prepared with the identical method of embodiment 1.
Two, carbon nanotube/titanium oxide composite nano materials preparation
(1) 2g multi-walled carbon nanotube is added in 10g n-dodecylamine, modified carbon nano-tube is obtained after stirring；
(2) 3g titanium oxide is added in 10g n-dodecylamine, modified zirconia is obtained after stirring；
(3) modified carbon nano-tube is added in ball mill with modified zirconia and is mixed, taken out after ball milling 30min, obtain carbon
Nanotube/Zirconia composite nano material.
Three, the preparation of composite Nano lubricating oil
Above-mentioned carbon nanotube/Zirconia composite nano material 3g is taken, is added in 100g mineral oil, after mechanical stirring is uniform
To composite Nano lubricating oil, wherein composite nano materials account for the 3% of mineral oil quality.
Embodiment 11
One, the preparation of zirconium oxide
Zirconium oxide is prepared with the identical method of embodiment 1.
Two, carbon nanotube/Zirconia composite nano material preparation
(1) 2g multi-walled carbon nanotube is added in 10g oleyl amine, modified carbon nano-tube is obtained after stirring；
(2) 1g zirconium oxide is added in 10g oleyl amine, modified zirconia is obtained after stirring；
(3) modified carbon nano-tube is added in ball mill with modified zirconia and is mixed, taken out after ball milling 30min, obtain carbon
Nanotube/Zirconia composite nano material.
Three, the preparation of composite Nano lubricating oil
Above-mentioned carbon nanotube/Zirconia composite nano material 3g is taken, is added in 100g mineral oil, after mechanical stirring is uniform
To composite Nano lubricating oil, wherein composite nano materials account for the 3% of mineral oil quality.
Embodiment 12
One, the preparation of zirconium oxide
Zirconium oxide is prepared with the identical method of embodiment 1.
Two, carbon nanotube/magnesia composite nano materials preparation
(1) 2g multi-walled carbon nanotube is added in 5g polyetheramine D2000, modified carbon nano-tube is obtained after stirring；
(2) 5g magnesia is added in 15g polyetheramine D2000, modified zirconia is obtained after stirring；
(3) modified carbon nano-tube is added in ball mill with modified zirconia and is mixed, taken out after ball milling 30min, obtain carbon
Nanotube/Zirconia composite nano material.
Three, the preparation of composite Nano lubricating oil
Above-mentioned carbon nanotube/Zirconia composite nano material 3g is taken, is added in 100g mineral oil, after mechanical stirring is uniform
To composite Nano lubricating oil, wherein composite nano materials account for the 3% of mineral oil quality.
Embodiment 13
One, the preparation of zirconium oxide
Zirconium oxide is prepared with the identical method of embodiment 1.
Two, carbon nanotube/Zirconia composite nano material preparation
(1) 2.5g multi-walled carbon nanotube is added in 10g oleyl amine, modified carbon nano-tube is obtained after stirring；
(2) 3g zirconium oxide is added in 10g oleyl amine, modified zirconia is obtained after stirring；
(3) modified carbon nano-tube is added in ball mill with modified zirconia and is mixed, taken out after ball milling 30min, obtain carbon
Nanotube/Zirconia composite nano material.
Three, the preparation of composite Nano lubricating oil
Above-mentioned carbon nanotube/Zirconia composite nano material 3g is taken, is added in 100g mineral oil, after mechanical stirring is uniform
To composite Nano lubricating oil, wherein composite nano materials account for the 3% of mineral oil quality.
Embodiment 14
One, the preparation of zirconium oxide
Zirconium oxide is prepared with the identical method of embodiment 1.
Two, carbon nanotube/Zirconia composite nano material preparation
(1) 1g multi-walled carbon nanotube is added in 5g oleyl amine, modified carbon nano-tube is obtained after stirring；
(2) 8g zirconium oxide is added in 15g oleyl amine, modified zirconia is obtained after stirring；
(3) modified carbon nano-tube is added in ball mill with modified zirconia and is mixed, taken out after ball milling 30min, obtain carbon
Nanotube/Zirconia composite nano material.
Three, the preparation of composite Nano lubricating oil
Above-mentioned carbon nanotube/Zirconia composite nano material 3g is taken, is added in 100g mineral oil, after mechanical stirring is uniform
To composite Nano lubricating oil, wherein composite nano materials account for the 3% of mineral oil quality.
Embodiment 15
1 gained carbon nanotube of Example/Zirconia composite nano material 8g is added in 100g mineral oil, mechanical stirring
Composite Nano lubricating oil is obtained after uniformly, wherein composite nano materials account for the 8% of mineral oil quality.
Embodiment 16
Using oleic acid as oiliness dispersing agent, lubricating oil is prepared with the identical method of embodiment 1.
Comparative example 1
Take 100g mineral oil, as lubricating oil described in comparative example 1.
Comparative example 2
(1) 1g multi-walled carbon nanotube is added in 20g oleyl amine, is taken out after ball milling 30min, obtains antiwear additive.
(2) the above-mentioned antiwear additive of 3g is added in 100g mineral oil, obtains lubricating oil.
Comparative example 3
(1) 1 gained zirconium oxide of 3g embodiment is added in 20g oleyl amine, is taken out after ball milling 30min, obtains antiwear additive.
(2) the above-mentioned antiwear additive of 3g is added in 100g mineral oil, obtains lubricating oil.
Comparative example 4
Untreated multi-walled carbon nanotube 3g is added in 100g mineral oil in 1 raw material of Example, forms lubricating oil.
Comparative example 5
(1) untreated multi-walled carbon nanotube 1g in 1 raw material of Example, after being mixed with 1 gained zirconium oxide 3g of embodiment,
Ball milling 30min obtains antiwear additive；
(2) it takes antiwear additive 3g obtained by above-mentioned steps to be added in 100g mineral oil, forms lubricating oil.
Nano lubricating oil obtained by above-described embodiment and comparative example is carried out the friction of ball disk method by ASTM G99-95 standard to survey
Examination, acquired results are as shown in table 3.
The abrasion resistance of each sample in 3 embodiment 1 of table
It can be concluded that, the nanometer of carbon nanotube or Zirconium oxide nano grain is individually added by the data comparison in the above table
Lubricating oil has certain lubrication anti-wear effect to be promoted, but effect is not as good as the structure composite type nano lubricating simultaneously containing the two
Oil；Gained carbon nanotube/Zirconia composite nano material of the invention can be used as lubrication anti-wear agent, is added in lubricating oil, can have
Effect improves the abrasion resistance of lubricating oil.
Claims (15)
1. a kind of carbon nanotube/zero dimensional nanometer materials composite material, which is characterized in that carbon nanotube and zero dimensional nanometer materials difference
Modified carbon nano-tube and modified zero dimensional nanometer materials are obtained through oiliness dispersing agent is modified, it is loaded modified on modified carbon nano-tube
The carbon nanotube/zero dimensional nanometer materials composite material is obtained after zero dimensional nanometer materials.
2. composite material according to claim 1, wherein the oiliness dispersing agent is selected from fat primary amine or polyetheramine.
3. composite material according to claim 1 or claim 2, wherein the zero dimensional nanometer materials are selected from metal or metallic compound,
The metal be selected from magnesium, aluminium and positioned at the 4th period of the periodic table of elements and the 5th period and belong to IB, IIB, IIIB, IVB, VB,
One or more of VIB, VIIB, VIII, IIIA, IVA race metallic element, be preferably selected from copper, zinc, magnesium, aluminium, titanium, zirconium,
One or more of tin, iron；The metallic compound is the oxide of one or more kinds of above-mentioned metals.
4. any one of -3 composite material according to claim 1, wherein the matter of the carbon nanotube and oiliness dispersing agent total amount
Amount is than being (0.5-2.5): 20, preferably (0.5-2): 20.
5. any one of -4 composite material according to claim 1, wherein the zero dimensional nanometer materials and oiliness dispersing agent total amount
Mass ratio be (1-10): 20, preferably (1-5): 20.
6. any one of -5 composite material according to claim 1, wherein the length of the carbon nanotube is 10nm -10 μm, directly
Diameter is 2nm-50nm.
7. any one of -6 composite material according to claim 1, wherein the partial size of the zero dimensional nanometer materials is 10nm-10 μ
m。
8. according to any one of the claim 2-6 composite material, wherein the fat primary amine main chain is comprising carbon chain lengths
The saturated hydrocarbyl or C6-C22 unsaturated alkyl of C6-C22, the unsaturated alkyl is preferably alkylene.
9. any one of -8 composite material according to claim 1, wherein the composite material is by the method comprising following step
It is prepared:
(1) by carbon nanotube and oiliness dispersant, modified carbon nano-tube is obtained after reaction；
(2) by zero dimensional nanometer materials and oiliness dispersant, modified zero dimensional nanometer materials are obtained after reaction；
(3) it after mixing the modified carbon nano-tube and the modified zero dimensional nanometer materials, obtains the carbon nanotube/zero dimension and receives
Rice composites.
10. a kind of composite Nano lubricating oil, which is characterized in that received including any one of the claim 1-9 carbon nanotube/zero dimension
Rice composites and lubricating oil.
11. composite Nano lubricating oil according to claim 10, wherein the mass ratio of the composite material and lubricating oil is
(0.5-5): 100, preferably (0.5-3): 100.
12. a kind of carbon nanotube/zero dimensional nanometer materials composite material preparation method, which is characterized in that include the following steps:
(1) by carbon nanotube and oiliness dispersant, modified carbon nano-tube is obtained after reaction；
(2) by zero dimensional nanometer materials and oiliness dispersant, modified zero dimensional nanometer materials are obtained after reaction；
(3) it after mixing the modified carbon nano-tube and the modified zero dimensional nanometer materials, obtains the carbon nanotube/zero dimension and receives
Rice composites.
13. preparation method according to claim 12, wherein in step (3), by the modified carbon nano-tube and the modification
It further include the process of ball milling after zero dimensional nanometer materials mixing.
14. a kind of preparation method of composite Nano lubricating oil, which is characterized in that include the following steps:
Any one of the claim 1-9 carbon nanotube/zero dimensional nanometer materials composite material is added in lubricating oil, is obtained compound
Nano lubricating oil.
15. any one of the claim 1-9 carbon nanotube/zero dimensional nanometer materials composite material or claim 10-11 are any
Application of the item composite Nano lubricating oil in lubricating oil field.
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