CN110229708A - Carbon nanotube/two-dimension nano materials composite material and its preparation method and application - Google Patents
Carbon nanotube/two-dimension nano materials composite material and its preparation method and application Download PDFInfo
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- CN110229708A CN110229708A CN201910563233.5A CN201910563233A CN110229708A CN 110229708 A CN110229708 A CN 110229708A CN 201910563233 A CN201910563233 A CN 201910563233A CN 110229708 A CN110229708 A CN 110229708A
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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
- C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
- C10M2201/04—Elements
- C10M2201/041—Carbon; Graphite; Carbon black
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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
- C10M2201/085—Phosphorus oxides, acids or salts
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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
Abstract
The present invention relates to a kind of carbon nanotube/two-dimension nano materials composite materials, it is characterized in that, carbon nanotube and two-dimension nano materials obtain modified carbon nano-tube and modified two-dimension nano materials through oiliness dispersing agent is modified respectively, obtain the carbon nanotube/two-dimension nano materials composite material after loaded modified two-dimension nano materials on modified carbon nano-tube.The two-dimension nano materials are layered metal phosphates nanometer sheet, preferably bedded zirconium phosphate nanometer sheet.Gained carbon nanotube/two-dimension nano 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/two-dimensional 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.This
On the one hand the lubrication anti-wear effect of kind nano lubricating oil depends on the properties such as composition, size, the shape of added nano material；
On the other hand dispersibility of the added nano material in lubricating oil is depended on.General nano material is due to its specific surface area
Greatly, and mutually incompatible with oil, thus flocculation or precipitating can occur, the reunion of this nano material so that added material practical ruler
It is very little significantly to increase, reach micron even grade.The reunion of large scale greatly weakens nano material in oily phase in this way
In lubrication anti-wear effect, or even it is also poorer than not adding nano material.
Common 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..These nano materials are uniform and stable
The lubrication anti-wear effect for being distributed in oily phase raising lubricating oil that can be different degrees of.ZL201410382805.7 is invented
It is a kind of that two-dimension nano materials, such as zirconium phosphate nano sheet and zero-dimension nano particle, such as copper nano particles are passed through into collaboration dispersion mixing
Method, both greatly improve the dispersibility in oily phase, be prepared for the binary lubricating system of different structure nano material,
And greatly improve the lubrication anti-wear effect of nano lubricating oil.
For the abrasion resistance for improving lubricating oil, " friction and Wear Study of the carbon nanotube as lube oil additive, rubs
It wipes and learns journal, in 394-397 ", carbon nanotube 2005,25 (5): is shown into excellent wear resistence as lube oil additive
Can, the mill spot surfacing of carbon nanotubes lubricating oil, scratch is relatively thin and is evenly distributed.
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, lubricating oil
Abrasion resistance need to be improved.
In order to solve the above technical problems, the present invention provide it is a kind of by carbon nanotube and two-dimension nano materials, such as basic zirconium phosphate
Nanometer sheet is compound and the method for preparing composite nano lubrication anti-wear agent and composite nano lubricating oil, is sent out by friction testing
Existing, this composite nano lubrication anti-friction material effect is better than the nano material of each exclusive use.Since carbon nanotube is
Monodimension nanometer material, and basic zirconium phosphate is two-dimension nano materials, thus composite nano lubrication anti-wear agent prepared by the present invention
It is properly termed as structure composite type nano lubricating anti-friction material, the nano lubricating oil of preparation is properly termed as structure composite type nano lubricating
Oil.
Specifically, in view of the deficiencies of the prior art, the present invention provides the following technical scheme that
A kind of carbon nanotube/two-dimension nano materials composite material, which is characterized in that carbon nanotube and two-dimension nano materials point
Modified carbon nano-tube and modified two-dimension nano materials are not obtained through oiliness dispersing agent is modified, loads and changes on modified carbon nano-tube
The carbon nanotube/two-dimension nano materials composite material is obtained after property two-dimension nano materials.
Preferably, in above-mentioned composite material, the two-dimension nano materials are layered metal phosphates nanometer sheet, preferably layer
Shape zirconium phosphate nano sheet.
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 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 two-dimension nano materials and oiliness dispersing agent total amount is (1-
15): 20, preferably (1-10): 20.
Preferably, the mass ratio of carbon nanotube and the total amount of two-dimension nano materials and oiliness dispersing agent is (3-15): 20, more
Preferably, the mass ratio of carbon nanotube and the total amount of two-dimension nano materials and oiliness dispersing agent is (6-12): 20.
Preferably, two-dimension nano materials and the mass ratio of carbon nanotube are (2-10): 1, it is furthermore preferred that two-dimension nano materials
Mass ratio with carbon nanotube is (0.5-10): 1, more preferably (2.5-10): 1.
Preferably, carbon nanotube: two-dimension nano materials: oiliness dispersing agent=1:5:20,
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 diameter of the two-dimension nano materials is 50nm-5 μm, with a thickness of 2nm-
500nm。
Preferably, in above-mentioned composite material, the fat primary amine main chain includes the saturated hydrocarbyl that carbon chain lengths are C6-C22
Or C6-C22 unsaturated alkyl, the unsaturated alkyl are alkylene.
Preferably, in above-mentioned composite material, the fat primary amine is selected from n-hexylamine, n-octyl amine, n-Decylamine or n-dodecylamine.
Preferably, in above-mentioned composite material, the number of carbon-carbon double bond is 1-4 in the alkylene.
Preferably, in above-mentioned composite material, 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 in above-mentioned composite material, the primary amine is oleyl amine, i.e. 9- ten
Eight enamines.
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 two-dimension nano materials and oiliness dispersant, modified two-dimension nano materials are obtained after reaction；
(3) after mixing the modified carbon nano-tube and the modified two-dimension nano materials, carbon nanotube/bis- are 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/two-dimensional 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 (0.5-3):
100。
Preferably, in above-mentioned composite Nano lubricating oil, the mass ratio of composite material and lubricating oil is (0.8-3.0): 100,
Preferably (08-1.5): 100, more preferably 1:100.
Preferably, in above-mentioned composite Nano lubricating oil, the coefficient of friction of the composite Nano lubricating oil is 0.05-0.3, excellent
It is selected as 0.05-0.25, more preferably 0.05-0.15, wear scar diameter 0.5-2.5, preferably 0.5-2.0.
The present invention also provides above-mentioned carbon nanotube/two-dimension nano 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 two-dimension nano materials and oiliness dispersant, modified two-dimension nano materials are obtained after reaction；
(3) after mixing the modified carbon nano-tube and the modified two-dimension nano materials, carbon nanotube/bis- are 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:(2.5-10).
Preferably, in above-mentioned preparation method, in step (2), the mass ratio of two-dimension nano materials and oiliness dispersing agent is 1:
(0.1-50), preferably 1:(1.5-15).
Preferably, in above-mentioned preparation method, in step (3), by the modified carbon nano-tube and the modified two-dimensional 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/two-dimension nano materials composite material is added in lubricating oil, composite Nano lubricating oil is obtained.
The present invention also provides above-mentioned carbon nanotube/two-dimension nano materials composite materials or above-mentioned composite Nano lubricating oil to moisten
The application in lubricating oil field.
The invention has the advantages that the present invention gained carbon nanotube/two-dimension nano 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 scanning electron microscope (SEM) photograph of 1.1 gained zirconium phosphate nano sheet of embodiment.
Fig. 2 is the transmission electron microscope figure of single-walled carbon nanotube used in embodiment 1.1.
Fig. 3 is 1.1 gained single-walled carbon nanotube of embodiment/phosphoric acid zirconium composite material transmission electron microscope figure.
Fig. 4 is the transmission electron microscope figure of multi-walled carbon nanotube used in embodiment 2.1.
Fig. 5 is 2.1 resultant multi-wall carbon nanotube of embodiment/phosphoric acid zirconium composite material transmission electron microscope figure.
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/two-dimensional nano material
Expect composite material and the compounded lubricating oil comprising this material, uses oiliness dispersing agent modified respectively carbon nanotube and basic zirconium phosphate
Afterwards, then by modified zirconium phosphate it is carried on modified carbon nano-tube, composite nano materials is made, this material is added in lubricating oil,
The abrasion resistance of lubricating oil can greatly be improved.
In a kind of preferred embodiment, carbon nanotube of the present invention/two-dimension nano materials composite material formula are as follows:
Carbon nanotube: 2.5-10 parts, zirconium phosphate nano sheet: 5-50 parts, oil-soluble dispersant: 100 parts.Preferably, carbon nanometer in raw material
The mass ratio of pipe, basic zirconium phosphate and oiliness dispersing agent is 1:5:20.Preparation method includes the following steps:
Carbon nanotube and zirconium phosphate nano sheet are separately added into oiliness dispersing agent, is stirred to be placed in ball mill and grind
It is taken out after mill 20min, obtains structure composite type nano lubricating antiwear additive.Wherein:
Carbon nanotube can are as follows: single-walled carbon nanotube or multi-walled carbon nanotube and its derivative, carbon nanotube source: Shenzhen
Nanometer port Co., Ltd.
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 is the saturated hydrocarbyl that carbon chain lengths are C6-C22 or the unsaturated hydrocarbons of C6-C22
Amidine functional group is contained in base, 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.
Zirconium phosphate nano sheet is a kind of Two-dimensional Inorganic sheet granular materials, is usually synthesized by hydro-thermal method or circumfluence method,
Its thickness is usually nanoscale, and size dimension is in nanoscale or micron order, and therefore, basic zirconium phosphate is also referred to as zirconium phosphate nano sheet.
In the present invention, the synthetic method of the zirconium phosphate nano sheet includes the following steps:
Basic zirconium chloride is added in phosphoric acid solution, back flow reaction under the conditions of oil bath, after product is washed with deionized,
Zirconium phosphate nano sheet is obtained after drying and grinding.Wherein, the concentration of the phosphoric acid solution is 2-5mol/L, the basic zirconium chloride and phosphorus
The mass volume ratio of acid solution is (15g-25g): 100ml；Oil bath temperature is 100-150 DEG C, reaction time 12-48h.
In a kind of preferred embodiment, the synthetic method of the zirconium phosphate nano sheet: the flask for being about 200ml in volume
In, by the ZrOCl of 20.0g2·8H2O is mixed with the phosphoric acid that 100ml concentration is 3.0mol/L and is poured into wherein.After mixing evenly, will
Beaker is placed in back flow reaction in 100 DEG C of oil bath and for 24 hours, flask is taken out after naturally cooling to room temperature, reaction product is spent
Three times, by the way that product is collected by centrifugation, then, obtained sample after drying for 24 hours, is ground at 65 DEG C for ionized water water washing to obtain the final product
To zirconium phosphate nano sheet white powder.
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: composite nano materials: 0.5-
3 parts, lubricating oil: 100 parts.Preferably, the mass ratio of composite nano materials and lubricating oil is 1:100.
It in the present invention, is preferably formulated are as follows: contain structure composite type nano lubricating antiwear additive in composite Nano lubricating oil
1.0%, wherein carbon nanotube in structure composite type nano abrasion-resistant additive: zirconium phosphate nano sheet: oiliness dispersing agent=1:5:20.
Sample preparation and test: it is equal that structure composite type nano lubricating antiwear additive is added to mechanical stirring in basic mineral oil
It is even, it is prepared into structure composite type nano lubricating oil.Nano lubricating oil is carried out the friction of ball disk method by ASTM G99-95 standard to survey
Examination.
Carbon nanotube of the present invention/two-dimension nano 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 |
| Phosphoric acid | Purity: 85% | Tianjin Yong great chemical reagent Co., Ltd |
| 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 |
Device therefor information in 2 embodiment of the present invention of table
1 single-walled carbon nanotube of embodiment/basic zirconium phosphate composite nano materials
Embodiment 1.1
One, the preparation of zirconium phosphate nano sheet
In the flask that volume is about 200ml, by the ZrOCl of 20.0g2·8H2The phosphorus that O and 100ml concentration are 3.0mol/L
Acid-mixed conjunction is poured into wherein.After mixing evenly, beaker is placed in in 100 DEG C of oil bath back flow reaction for 24 hours, room to be naturally cooled to
Flask is taken out after temperature, and reaction product is washed with deionized three times, by the way that product is collected by centrifugation, then, the sample that will be obtained
At 65 DEG C after drying for 24 hours, grinding obtains zirconium phosphate nano sheet white powder.
The scanning electron microscope (SEM) photograph (SEM figure) of zirconium phosphate nano sheet is as shown in Figure 1, the original basic zirconium phosphate prepared as seen from the figure
Nanometer sheet has two-dimensional slice layer structure, and diameter is about 100nm.
Two, carbon nanotube/basic zirconium phosphate composite nano materials preparation
(1) 1g single-walled carbon nanotube is added in 10g oleyl amine, modified carbon nano-tube is obtained after stirring；
(2) the above-mentioned zirconium phosphate nano sheet of 5g is added in 10g oleyl amine, modified zirconium phosphate is obtained after stirring；
(3) modified carbon nano-tube is added in ball mill with modified zirconium phosphate and is mixed, taken out after ball milling 20min, obtain carbon
Nanotube/basic zirconium phosphate composite nano materials.
The transmission electron microscope figure (TEM figure) of single-walled carbon nanotube is unprocessed as shown in Fig. 2, as seen from the figure
Single-walled carbon nanotube flock together mostly, be difficult to disperse.
1.1 gained carbon nanotube of embodiment/basic zirconium phosphate composite nano materials transmission electron microscope figure as shown in figure 3,
As seen from the figure, two kinds of different nano materials of structure are compound, and the two can disperse well.
Three, the preparation of composite Nano lubricating oil
Above-mentioned carbon nanotube/basic zirconium phosphate composite nano materials 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 1.2
One, the preparation of zirconium phosphate nano sheet
In the flask that volume is about 200ml, by the ZrOCl of 15.0g2·8H2The phosphorus that O and 100ml concentration are 3.0mol/L
Acid-mixed conjunction is poured into wherein.After mixing evenly, beaker is placed in back flow reaction 20h, room to be naturally cooled in 120 DEG C of oil bath
Flask is taken out after temperature, and reaction product is washed with deionized three times, by the way that product is collected by centrifugation, then, the sample that will be obtained
At 65 DEG C after drying for 24 hours, grinding obtains zirconium phosphate nano sheet white powder.
The size that the present embodiment gained zirconium phosphate nano sheet is detected with the identical method of embodiment 1.1 is 150nm.
Two, carbon nanotube/basic zirconium phosphate composite nano materials preparation
(1) 1g single-walled carbon nanotube is added in 10g oleyl amine, modified carbon nano-tube is obtained after stirring；
(2) the above-mentioned zirconium phosphate nano sheet of 5g is added in 10g oleyl amine, modified zirconium phosphate is obtained after stirring；
(3) modified carbon nano-tube is added in ball mill with modified zirconium phosphate and is mixed, taken out after ball milling 20min, obtain carbon
Nanotube/basic zirconium phosphate composite nano materials.
It is detected with the identical method of embodiment 1.1 it is found that two kinds of different nano materials of structure are compound, the two can be very
Good dispersion.
Three, the preparation of composite Nano lubricating oil
Above-mentioned carbon nanotube/basic zirconium phosphate composite nano materials 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 1.3
One, the preparation of zirconium phosphate nano sheet
In the flask that volume is about 200ml, by the ZrOCl of 25.0g2·8H2The phosphorus that O and 100ml concentration are 5.0mol/L
Acid-mixed conjunction is poured into wherein.After mixing evenly, beaker is placed in back flow reaction 40h, room to be naturally cooled in 150 DEG C of oil bath
Flask is taken out after temperature, and reaction product is washed with deionized three times, by the way that product is collected by centrifugation, then, the sample that will be obtained
At 65 DEG C after drying for 24 hours, grinding obtains zirconium phosphate nano sheet white powder.
The size that the present embodiment gained zirconium phosphate nano sheet is detected with the identical method of embodiment 1.1 is 200nm.
Two, carbon nanotube/basic zirconium phosphate composite nano materials preparation
(1) 1g single-walled carbon nanotube is added in 10g oleyl amine, modified carbon nano-tube is obtained after stirring；
(2) the above-mentioned zirconium phosphate nano sheet of 5g is added in 10g oleyl amine, modified zirconium phosphate is obtained after stirring；
(3) modified carbon nano-tube is added in ball mill with modified zirconium phosphate and is mixed, taken out after ball milling 20min, obtain carbon
Nanotube/basic zirconium phosphate composite nano materials.
It is detected with the identical method of embodiment 1.1 it is found that two kinds of different nano materials of structure are compound, the two can be very
Good dispersion.
Three, the preparation of composite Nano lubricating oil
Above-mentioned carbon nanotube/basic zirconium phosphate composite nano materials 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 1.4
One, the preparation of zirconium phosphate nano sheet
In the flask that volume is about 200ml, by the ZrOCl of 15.0g2·8H2The phosphorus that O and 100ml concentration are 2.0mol/L
Acid-mixed conjunction is poured into wherein.After mixing evenly, beaker is placed in back flow reaction 20h, room to be naturally cooled in 120 DEG C of oil bath
Flask is taken out after temperature, and reaction product is washed with deionized three times, by the way that product is collected by centrifugation, then, the sample that will be obtained
At 65 DEG C after drying for 24 hours, grinding obtains zirconium phosphate nano sheet white powder.
The size that the present embodiment gained zirconium phosphate nano sheet is detected with the identical method of embodiment 1.1 is 120nm.
Two, carbon nanotube/basic zirconium phosphate composite nano materials preparation
(1) 0.5g single-walled carbon nanotube is added in 5g oleyl amine, modified carbon nano-tube is obtained after stirring；
(2) the above-mentioned zirconium phosphate nano sheet of 5g is added in 15g oleyl amine, modified zirconium phosphate is obtained after stirring；
(3) modified carbon nano-tube is added in ball mill with modified zirconium phosphate and is mixed, taken out after ball milling 20min, obtain carbon
Nanotube/basic zirconium phosphate composite nano materials.
It is detected with the identical method of embodiment 1.1 it is found that two kinds of different nano materials of structure are compound, the two can be very
Good dispersion.
Three, the preparation of composite Nano lubricating oil
Above-mentioned carbon nanotube/basic zirconium phosphate composite nano materials 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 1.5
One, the preparation of zirconium phosphate nano sheet
In the flask that volume is about 200ml, by the ZrOCl of 20.0g2·8H2The phosphorus that O and 100ml concentration are 3.0mol/L
Acid-mixed conjunction is poured into wherein.After mixing evenly, beaker is placed in in 100 DEG C of oil bath back flow reaction for 24 hours, room to be naturally cooled to
Flask is taken out after temperature, and reaction product is washed with deionized three times, by the way that product is collected by centrifugation, then, the sample that will be obtained
At 65 DEG C after drying for 24 hours, grinding obtains zirconium phosphate nano sheet white powder.
Two, carbon nanotube/basic zirconium phosphate composite nano materials preparation
(1) 1g single-walled carbon nanotube is added in 10g n-hexylamine, modified carbon nano-tube is obtained after stirring；
(2) the above-mentioned zirconium phosphate nano sheet of 2g is added in 10g n-hexylamine, modified zirconium phosphate is obtained after stirring；
(3) modified carbon nano-tube is added in ball mill with modified zirconium phosphate and is mixed, taken out after ball milling 20min, obtain carbon
Nanotube/basic zirconium phosphate composite nano materials.
It is detected with the identical method of embodiment 1.1 it is found that two kinds of different nano materials of structure are compound, the two can be very
Good dispersion.
Three, the preparation of composite Nano lubricating oil
Above-mentioned carbon nanotube/basic zirconium phosphate composite nano materials 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 1.6
One, the preparation of zirconium phosphate nano sheet
Zirconium phosphate nano sheet is prepared according to the identical method of embodiment 1.1.
Two, carbon nanotube/basic zirconium phosphate composite nano materials preparation
(1) 2g single-walled carbon nanotube is added in 10g oleyl amine, modified carbon nano-tube is obtained after stirring；
(2) the above-mentioned zirconium phosphate nano sheet of 5g is added in 10g oleyl amine, modified zirconium phosphate is obtained after stirring；
(3) modified carbon nano-tube is added in ball mill with modified zirconium phosphate and is mixed, taken out after ball milling 20min, obtain carbon
Nanotube/basic zirconium phosphate composite nano materials.
Three, the preparation of composite Nano lubricating oil
Above-mentioned carbon nanotube/basic zirconium phosphate composite nano materials 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 1.7
One, the preparation of zirconium phosphate nano sheet
Zirconium phosphate nano sheet is prepared according to the identical method of embodiment 1.1.
Two, carbon nanotube/basic zirconium phosphate composite nano materials preparation
(1) 0.5g single-walled carbon nanotube is added in 5g n-dodecylamine, modified carbon nano-tube is obtained after stirring；
(2) the above-mentioned zirconium phosphate nano sheet of 1g is added in 15g n-dodecylamine, modified zirconium phosphate is obtained after stirring；
(3) modified carbon nano-tube is added in ball mill with modified zirconium phosphate and is mixed, taken out after ball milling 20min, obtain carbon
Nanotube/basic zirconium phosphate composite nano materials.
Three, the preparation of composite Nano lubricating oil
Above-mentioned carbon nanotube/basic zirconium phosphate composite nano materials 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 1.8
One, the preparation of zirconium phosphate nano sheet
Zirconium phosphate nano sheet is prepared according to the identical method of embodiment 1.1.
Two, carbon nanotube/basic zirconium phosphate composite nano materials preparation
(1) 0.5g single-walled carbon nanotube is added in 5g polyetheramine D2000, modified carbon nano-tube is obtained after stirring；
(2) the above-mentioned zirconium phosphate nano sheet of 10g is added in 15g polyetheramine D2000, modified zirconium phosphate is obtained after stirring；
(3) modified carbon nano-tube is added in ball mill with modified zirconium phosphate and is mixed, taken out after ball milling 20min, obtain carbon
Nanotube/basic zirconium phosphate composite nano materials.
Three, the preparation of composite Nano lubricating oil
Above-mentioned carbon nanotube/basic zirconium phosphate composite nano materials 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 1.9
One, the preparation of zirconium phosphate nano sheet
Zirconium phosphate nano sheet is prepared according to the identical method of embodiment 1.1.
Two, carbon nanotube/basic zirconium phosphate composite nano materials preparation
(1) 2g single-walled carbon nanotube is added in 10g oleyl amine, modified carbon nano-tube is obtained after stirring；
(2) the above-mentioned zirconium phosphate nano sheet of 1g is added in 10g oleyl amine, modified zirconium phosphate is obtained after stirring；
(3) modified carbon nano-tube is added in ball mill with modified zirconium phosphate and is mixed, taken out after ball milling 20min, obtain carbon
Nanotube/basic zirconium phosphate composite nano materials.
Three, the preparation of composite Nano lubricating oil
Above-mentioned carbon nanotube/basic zirconium phosphate composite nano materials 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 1.10
One, the preparation of zirconium phosphate nano sheet
Zirconium phosphate nano sheet is prepared according to the identical method of embodiment 1.1.
Two, carbon nanotube/basic zirconium phosphate composite nano materials preparation
(1) 2g single-walled carbon nanotube is added in 5g oleyl amine, modified carbon nano-tube is obtained after stirring；
(2) the above-mentioned zirconium phosphate nano sheet of 10g is added in 15g oleyl amine, modified zirconium phosphate is obtained after stirring；
(3) modified carbon nano-tube is added in ball mill with modified zirconium phosphate and is mixed, taken out after ball milling 20min, obtain carbon
Nanotube/basic zirconium phosphate composite nano materials.
Three, the preparation of composite Nano lubricating oil
Above-mentioned carbon nanotube/basic zirconium phosphate composite nano materials 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 1.11
One, the preparation of zirconium phosphate nano sheet
Zirconium phosphate nano sheet is prepared according to the identical method of embodiment 1.1.
Two, carbon nanotube/basic zirconium phosphate composite nano materials preparation
(1) 1g single-walled carbon nanotube is added in 5g oleyl amine, modified carbon nano-tube is obtained after stirring；
(2) the above-mentioned zirconium phosphate nano sheet of 10g is added in 15g oleyl amine, modified zirconium phosphate is obtained after stirring；
(3) modified carbon nano-tube is added in ball mill with modified zirconium phosphate and is mixed, taken out after ball milling 20min, obtain carbon
Nanotube/basic zirconium phosphate composite nano materials.
Three, the preparation of composite Nano lubricating oil
Above-mentioned carbon nanotube/basic zirconium phosphate composite nano materials 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 1.12
One, the preparation of zirconium phosphate nano sheet
Zirconium phosphate nano sheet is prepared according to the identical method of embodiment 1.1.
Two, carbon nanotube/basic zirconium phosphate composite nano materials preparation
(1) 2.5g single-walled carbon nanotube is added in 15g oleyl amine, modified carbon nano-tube is obtained after stirring；
(2) the above-mentioned zirconium phosphate nano sheet of 5g is added in 5g oleyl amine, modified zirconium phosphate is obtained after stirring；
(3) modified carbon nano-tube is added in ball mill with modified zirconium phosphate and is mixed, taken out after ball milling 20min, obtain carbon
Nanotube/basic zirconium phosphate composite nano materials.
Three, the preparation of composite Nano lubricating oil
Above-mentioned carbon nanotube/basic zirconium phosphate composite nano materials 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 1.13
One, the preparation of zirconium phosphate nano sheet
Zirconium phosphate nano sheet is prepared according to the identical method of embodiment 1.1.
Two, carbon nanotube/basic zirconium phosphate composite nano materials preparation
(1) 1g single-walled carbon nanotube is added in 5g oleyl amine, modified carbon nano-tube is obtained after stirring；
(2) the above-mentioned zirconium phosphate nano sheet of 15g is added in 15g oleyl amine, modified zirconium phosphate is obtained after stirring；
(3) modified carbon nano-tube is added in ball mill with modified zirconium phosphate and is mixed, taken out after ball milling 20min, obtain carbon
Nanotube/basic zirconium phosphate composite nano materials.
Three, the preparation of composite Nano lubricating oil
Above-mentioned carbon nanotube/basic zirconium phosphate composite nano materials 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 1.14
1.1 gained carbon nanotube of embodiment/basic zirconium phosphate composite nano materials 5g is added in 100g oleyl amine, compound receive is obtained
Rice lubricating oil.
Comparative example 1.1
Take 100g mineral oil, as lubricating oil described in comparative example 1.1.
Comparative example 1.2
(1) single-walled carbon nanotube 1g is added in 20g oleyl amine, is taken out after ball milling 20min, obtains antiwear additive；
(2) antiwear additive 1g obtained by step (1) is added in 100g mineral oil, obtains lubricating oil.
Comparative example 1.3
(1) 1.1 gained zirconium phosphate nano sheet 5g of embodiment is added in 20g oleyl amine, takes out, is resisted after ball milling 20min
Grinding agent；
(2) antiwear additive 1g obtained by step (1) is added in 100g mineral oil, obtains lubricating oil.
Comparative example 1.4
According to 1.1 the method for embodiment, oleyl amine is removed, obtains composite Nano lubrication by the identical step of embodiment 1.1
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
2 multi-walled carbon nanotubes of embodiment/basic zirconium phosphate composite nano materials
Embodiment 2.1
One, the preparation of zirconium phosphate nano sheet
In the flask that volume is about 200ml, by the ZrOCl of 20.0g2·8H2The phosphorus that O and 100ml concentration are 3.0mol/L
Acid-mixed conjunction is poured into wherein.After mixing evenly, beaker is placed in in 100 DEG C of oil bath back flow reaction for 24 hours, room to be naturally cooled to
Flask is taken out after temperature, and reaction product is washed with deionized three times, by the way that product is collected by centrifugation, then, the sample that will be obtained
At 65 DEG C after drying for 24 hours, grinding obtains zirconium phosphate nano sheet white powder.
Two, carbon nanotube/basic zirconium phosphate composite nano materials preparation
(1) 1g multi-walled carbon nanotube is added in 10g oleyl amine, modified carbon nano-tube is obtained after stirring；
(2) the above-mentioned zirconium phosphate nano sheet of 5g is added in 10g oleyl amine, modified zirconium phosphate is obtained after stirring；
(3) modified carbon nano-tube is added in ball mill with modified zirconium phosphate and is mixed, taken out after ball milling 20min, obtain carbon
Nanotube/basic zirconium phosphate composite nano materials.
The transmission electron microscope figure (TEM figure) of multi-walled carbon nanotube is unprocessed as shown in figure 4, as seen from the figure
Multi-walled carbon nanotube reunite it is serious.
2.1 gained carbon nanotube of embodiment/basic zirconium phosphate composite nano materials transmission electron microscope figure as shown in figure 5,
As seen from the figure, two kinds of different nano materials of structure are compound, and the two can disperse well.
Three, the preparation of composite Nano lubricating oil
Above-mentioned carbon nanotube/basic zirconium phosphate composite nano materials 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 2.2-2.14
Select multi-walled carbon nanotube that embodiment is prepared respectively with the identical method of embodiment 1.2- embodiment 1.14
The multi-walled carbon nanotube of 2.2-2.14/basic zirconium phosphate composite nano materials and composite Nano lubricating oil.
Comparative example 2.1
Take 100g mineral oil, as lubricating oil described in comparative example 2.1.
Comparative example 2.2-2.4
Select multi-walled carbon nanotube that comparative example 2.2-2.4 is prepared respectively with the identical method of comparative example 1.2-1.4
Nano material and 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 4.
The abrasion resistance of 4 embodiment of table, 2 each sample
It can be concluded that, individually add zirconium phosphate nano sheet by the data comparison in two above table or individually addition carbon is received
The nano lubricating oil of mitron has certain lubrication anti-wear effect to be promoted, but effect is not so good as the structure composite type nanometer containing the two
Lubricating oil；Gained carbon nanotube/two-dimension nano materials composite material of the present invention can be used as lubrication anti-wear agent, be added to lubrication
In oil, the abrasion resistance of lubricating oil can be effectively improved.
Claims (15)
1. a kind of carbon nanotube/two-dimension nano materials composite material, which is characterized in that carbon nanotube and two-dimension nano materials difference
Modified carbon nano-tube and modified two-dimension nano materials are obtained through oiliness dispersing agent is modified, it is loaded modified on modified carbon nano-tube
The carbon nanotube/two-dimension nano materials composite material is obtained after two-dimension nano materials.
2. composite material according to claim 1, wherein the two-dimension nano materials are layered metal phosphates nanometer sheet,
Preferably bedded zirconium phosphate nanometer sheet.
3. composite material according to claim 1 or claim 2, wherein the oiliness dispersing agent is selected from fat primary amine or polyetheramine.
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 two-dimension nano materials and oiliness dispersing agent total amount
Mass ratio be (1-15): 20, preferably (1-10): 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 diameter of the two-dimension nano materials is 50nm-5 μ
M, with a thickness of 2nm-500nm.
8. according to any one of the claim 3-7 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 two-dimension nano materials and oiliness dispersant, modified two-dimension nano materials are obtained after reaction；
(3) after mixing the modified carbon nano-tube and the modified two-dimension nano materials, the carbon nanotube/bis- wieners are obtained
Rice composites.
10. a kind of composite Nano lubricating oil, which is characterized in that including any one of the claim 1-9 carbon nanotube/bis- wieners
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
(0.5-3): 100.
12. a kind of carbon nanotube/two-dimension nano 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 two-dimension nano materials and oiliness dispersant, modified two-dimension nano materials are obtained after reaction；
(3) after mixing the modified carbon nano-tube and the modified two-dimension nano materials, the carbon nanotube/bis- wieners are obtained
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 two-dimension nano 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/two-dimension nano materials composite material is added in lubricating oil, is obtained compound
Nano lubricating oil.
15. any one of the claim 1-9 carbon nanotube/two-dimension nano 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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