CN109097156A - A kind of lubricating grease graphene-based calcium carbonate nano composite material and preparation method - Google Patents
A kind of lubricating grease graphene-based calcium carbonate nano composite material and preparation method Download PDFInfo
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- CN109097156A CN109097156A CN201810985889.1A CN201810985889A CN109097156A CN 109097156 A CN109097156 A CN 109097156A CN 201810985889 A CN201810985889 A CN 201810985889A CN 109097156 A CN109097156 A CN 109097156A
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M125/00—Lubricating compositions characterised by the additive being an inorganic material
- C10M125/10—Metal oxides, hydroxides, carbonates or bicarbonates
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M125/00—Lubricating compositions characterised by the additive being an inorganic material
- C10M125/18—Compounds containing halogen
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M125/00—Lubricating compositions characterised by the additive being an inorganic material
- C10M125/20—Compounds containing nitrogen
-
- 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
-
- 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
- C10M2201/042—Carbon; Graphite; Carbon black halogenated, i.e. graphite fluoride
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
- C10M2201/06—Metal compounds
- C10M2201/061—Carbides; Hydrides; Nitrides
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
- C10M2201/06—Metal compounds
- C10M2201/062—Oxides; Hydroxides; Carbonates or bicarbonates
-
- 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 invention discloses a kind of lubricating grease graphene-based calcium carbonate nano composite material and the preparation methods that belong to grease additive field.The graphene-based calcium carbonate nano composite material is stannic oxide/graphene nano calcium carbonate, N doping stannic oxide/graphene nano calcium carbonate, Fluorin doped stannic oxide/graphene nano calcium carbonate, it is by the way that graphene-based dispersion liquid to be added in nanometer calcium carbonate dispersion liquid, the 360w ultrasound 0.5h under room temperature, then it is centrifuged at a high speed, product is obtained in 60 DEG C of dry 18h.Coefficient of friction, the especially coefficient of friction in running-in stage can be effectively reduced in the graphene-based calcium carbonate nano composite material, improves the antifriction performance of lubricating grease, and preparation method is simple, and reaction condition is mild, at low cost.
Description
Technical field
The invention belongs to grease additive field, in particular to a kind of lubricating grease is compound with graphene-based calcium carbonate nano
Material and preparation method.
Background technique
With the fast development of modern industry, the energy, Environmental and resource issue are increasingly serious, high bearing capacity and environment friend
The research and development of good novel lubricating oil additive are extremely urgent.Because nanometer calcium carbonate has wear-resistant, cheap and environmentally friendly
Nano-calcium carbonate particles are added directly into lubricant grease by advantage, scientific research personnel, to develop into novel environmental close friend's
Multifunctional lubricating additive.
Although nano-calcium carbonate particles can make the abrasion resistance of lubricant grease be greatly improved as lubricating additive,
But there are still the problems that bearing capacity is inadequate and running-in stage coefficient of friction is higher.The study found that nano-calcium carbonate particles are in lithium-
When rubbing in calcium-base grease, the coefficient of friction in load running-in stage in 300-500N is unstable, and load is in 400N or more
When big particle size lubricant coefficient of friction it is highly unstable, load cannot form effectively lubricating when being 500N.Chinese section
Lanzhou Chemical Physics research institute Wang Xiao wave seminar of institute takes a kind of new method to attempt to solve the above problems: by two kinds of differences
The Nano particles of calcium carbonate of partial size is added in lubricating grease after mixing according to different proportion, and research finds that its bearing capacity can be from
400N is increased to 600N, but the serious seizing phenomenon of running-in stage appearance under top load, and running-in stage coefficient of friction is higher to ask
Topic is not still solved effectively.
Summary of the invention
The purpose of the present invention is to provide a kind of lubricating grease graphene-based calcium carbonate nano composite material and preparation method,
It is characterized in that, the graphene-based calcium carbonate nano composite material is stannic oxide/graphene nano calcium carbonate, N doping oxidation stone
Black alkene nanometer calcium carbonate, Fluorin doped stannic oxide/graphene nano calcium carbonate, wherein graphene oxide, N doping graphene oxide, fluorine
Adulterate graphene oxide content be graphene-based calcium carbonate nano composite material 0.78wt.%, 1.56wt.%,
3.125wt.%, 6.25wt.%.
The preparation method of the graphene-based calcium carbonate nano composite material the following steps are included:
(1) 2-10g CaO is digested to obtain calcium hydroxide suspension with the 100mL secondary distilled water that temperature is 80 DEG C, it is old
After changing overnight, lauric acid/ethanol solution of 0-30mL0.05-0.50mol/L is added, is stirred to react 2h at room temperature, then constant temperature
CO is passed through with 0.2-1.5L/min rate in water-bath2Gas carries out carburizing reagent, and pH meter tracks the pH value variation of reaction solution, to pH
Stop reaction when value is 7, product, which is filtered, washed, obtains nano-calcium carbonate calcium product with after 60 DEG C of vacuum drying.
(2) nanometer calcium carbonate for weighing 0.240-1.920g step (1) preparation is dispersed in 240mL dehydrated alcohol, 400w
Ultrasonic disperse 1h obtains finely dispersed nanometer calcium carbonate dispersion liquid, concentration 1-8mg/mL.
(3) 0.024-0.120g graphene oxide or N doping graphene oxide or Fluorin doped graphite oxide are accurately weighed
Alkene is dispersed in 120mL water, 400w ultrasonic disperse 2h, glass bar auxiliary stirring, 4 DEG C of refrigerator preservations, concentration 0.2-1mg/
mL。
(4) the graphene-based dispersion liquid of 7.5mL, 15mL, 30mL, 60mL step (3) is taken to be added to step (2) respectively
In 240mL nanometer calcium carbonate dispersion liquid, 360w ultrasound 0.5h, is then centrifuged at a high speed under room temperature, and product is in 60 DEG C of dryings
18h, obtain graphene oxide or N doping graphene oxide or Fluorin doped graphene oxide content be 0.78wt.%,
The graphene-based calcium carbonate nano composite material of 1.56wt.%, 3.125wt.%, 6.25wt.%.
The tribological property of the graphene-based calcium carbonate nano composite material of further test preparation, the method is as follows:
(1) the graphene-based calcium carbonate nano composite material for weighing 0.5-8g step (4) is added to machine in 100g areidofat
Tool stirring grinds three times on three-roll grinder after mixing and the profit that graphene-based calcium carbonate content is 0.5-8wt.% is made
Consistent lubricant sample.
(2) using SRV-IV type micro-moving frictional wear testing machine from tape test set testing friction coefficient, test condition is such as
Under: testing time 30min, test temperature are 25 DEG C, test load 100N, test frequency 20Hz, test amplitude 1mm.It is used
On try and lower examination disk material is 52100 steel of SAE, 60 ± 2HRC of hardness.On try surface roughness be 0.025 ± 0.005
μm, diameter 10mm, lower examination dish cart surface roughness is about 0.016 μm, diameter 24mm, thickness 7.85mm.
The invention has the benefit that providing a kind of lubricating grease graphene-based calcium carbonate nano composite material and preparation
Method, prepared graphene-based calcium carbonate nano composite material are uniformly dispersed, and do not occur significantly to reunite, preceding compared with compound
The shape and size of material, each particle are not substantially change, which effectively reduces areidofat running-in stage peace
Coefficient of friction run time steady, improves tribological property.Preparation process of the invention simultaneously is simple to operation, reaction condition
Mildly, at low cost.
Detailed description of the invention
Fig. 1 is the transmission electron microscope picture of graphene oxide calcium carbonate nano composite material prepared by embodiment 1；
Fig. 2 is the transmission electron microscope picture of N doping graphene oxide calcium carbonate nano composite material prepared by embodiment 2；
Fig. 3 is the transmission electron microscope picture of Fluorin doped graphene oxide calcium carbonate nano composite material prepared by embodiment 3；
Fig. 4 is the change of the coefficient of friction that is related to of embodiment 1 relational graph (1) and coefficient of friction that change over time in 2min
Change curve graph (2)；
Wherein BASE is areidofat, CaCO3For nano-calcium carbonate particles prepared by embodiment 1, GO3 is the preparation of embodiment 1
Graphene oxide calcium carbonate nano composite material；
Fig. 5 is the change of the coefficient of friction that is related to of embodiment 2 relational graph (1) and coefficient of friction that change over time in 2min
Change curve graph (2)；
Wherein BASE is areidofat, CaCO3For nano-calcium carbonate particles prepared by embodiment 2, NGO4 is the preparation of embodiment 2
N doping graphene oxide calcium carbonate nano composite material；
Fig. 6 is the change of the coefficient of friction that is related to of embodiment 3 relational graph (1) and coefficient of friction that change over time in 2min
Change curve graph (2)；
Wherein BASE is areidofat, CaCO3For nano-calcium carbonate particles prepared by embodiment 3, FGO1 is the preparation of embodiment 3
Fluorin doped graphene oxide calcium carbonate nano composite material.
Specific embodiment
The present invention provides a kind of lubricating grease graphene-based calcium carbonate nano composite material and preparation method, below with reference to
The present invention is described further for drawings and examples.
Embodiment 1:
(1) 5.6g CaO is digested to obtain calcium hydroxide suspension with the 100mL secondary distilled water that temperature is 80 DEG C, is aged
After overnight, lauric acid/ethanol solution of the 0.1mol/L of 15mL is added, is stirred to react 2h at room temperature, then 20 DEG C of waters bath with thermostatic control
In CO is passed through with 1.0L/min rate2Gas carries out carburizing reagent, and pH meter tracks the pH value variation of reaction solution, when pH value is 7
Stop reaction, product, which is filtered, washed, obtains nano-calcium carbonate calcium product with after 60 DEG C of vacuum drying.
(2) nanometer calcium carbonate for weighing 0.9600g step (1) preparation is dispersed in 240mL dehydrated alcohol, 400w ultrasound point
1h is dissipated, the nanometer calcium carbonate dispersion liquid of 4mg/mL is obtained.
(3) it accurately weighs 0.1200g graphene oxide to be dispersed in 120mL water, 400w ultrasonic disperse 2h, glass bar auxiliary
Stirring, 4 DEG C of refrigerator preservations, concentration 1mg/mL.
(4) graphene oxide dispersion of 30mL step (3) is taken to be added in the dispersion liquid of step (2), under room temperature
360w ultrasound 0.5h, is then centrifuged at a high speed, and in 60 DEG C of dry 18h, obtain graphene oxide content is product
The graphene oxide calcium carbonate nano composite material of 3.125wt.%.
(5) the graphene oxide calcium carbonate nano composite material 1.5g for accurately weighing step (4), is added to 100g areidofat
Middle mechanical stirring grinds the graphene oxide calcium carbonate lubrication of three times obtained 1.5wt.% on three-roll grinder after mixing
Rouge sample.
(6) SRV-IV type micro-moving frictional wear testing machine is selected, testing time 30min, test temperature are 25 DEG C, test
Load 100N, test frequency 20Hz, test amplitude 1mm.It tries on used and lower examination disk material is 52100 steel of SAE, hardness
60±2HRC.On try surface roughness be 0.025 ± 0.005 μm, diameter 10mm, lower examination dish cart surface roughness is about 0.016 μ
M, diameter 24mm, thickness 7.85mm.
In conjunction with attached drawing 4, discovery is added to the areidofat of graphite oxide alkenyl calcium carbonate nano composite material and is added to and receives
The areidofat and additive-free areidofat of rice calcium carbonate granule are compared, and the average friction coefficient in half an hour reduces respectively
29.4%, 15.95%, the running-in stage and it is steady run time, coefficient of friction and fluctuating range are optimal.
Embodiment 2:
(1) 5.6g CaO is digested to obtain calcium hydroxide suspension with the 100mL secondary distilled water that temperature is 80 DEG C, is aged
After overnight, lauric acid/ethanol solution of the 0.1mol/L of 15mL is added, is stirred to react 2h at room temperature, then 20 DEG C of waters bath with thermostatic control
In CO is passed through with 1.0L/min rate2Gas carries out carburizing reagent, and pH meter tracks the pH value variation of reaction solution, when pH value is 7
Stop reaction, product, which is filtered, washed, obtains nano-calcium carbonate calcium product with after 60 DEG C of vacuum drying.
(2) nanometer calcium carbonate for weighing 0.9600g step (1) preparation is dispersed in 240mL dehydrated alcohol, 400w ultrasound point
1h is dissipated, the nanometer calcium carbonate dispersion liquid of 4mg/mL is obtained.
(3) it accurately weighs 0.1200g N doping graphene oxide to be dispersed in 120mL water, 400w ultrasonic disperse 2h, glass
Stick auxiliary stirring, 4 DEG C of refrigerator preservations, concentration 1mg/mL.
(4) the N doping graphene oxide dispersion of 60mL step (3) is taken to be added in the dispersion liquid of step (2), Yu Chang
The lower 360w ultrasound 0.5h of temperature, is then centrifuged at a high speed, product obtains N doping graphene oxide content in 60 DEG C of dry 18h
For the N doping graphene oxide calcium carbonate nano composite material of 6.25wt.%.
(5) the N doping graphene oxide calcium carbonate nano composite material 1.5g for accurately weighing step (4), is added to 100g
Mechanical stirring in areidofat grinds the N doping graphite oxide of three times obtained 1.5wt.% on three-roll grinder after mixing
Olefinic carbon acid grease of calcium sample.
(6) SRV-IV type micro-moving frictional wear testing machine is selected, testing time 30min, test temperature are 25 DEG C, test
Load 100N, test frequency 20Hz, test amplitude 1mm.It tries on used and lower examination disk material is 52100 steel of SAE, hardness
60±2HRC.On try surface roughness be 0.025 ± 0.005 μm, diameter 10mm, lower examination dish cart surface roughness is about 0.016 μ
M, diameter 24mm, thickness 7.85mm.
In conjunction with attached drawing 5, discovery is added to the areidofat of N doping graphite oxide alkenyl calcium carbonate nano composite material and adds
The areidofat and additive-free areidofat for having added nano-calcium carbonate particles are compared, the average friction coefficient difference in half an hour
Reduce 20.62%, 5.52%, the running-in stage and it is steady run time, antifriction performance significantly improves.
Embodiment 3:
(1) 5.6g CaO is digested to obtain calcium hydroxide suspension with the 100mL secondary distilled water that temperature is 80 DEG C, is aged
After overnight, lauric acid/ethanol solution of the 0.1mol/L of 15mL is added, is stirred to react 2h at room temperature, then 20 DEG C of waters bath with thermostatic control
In CO is passed through with 1.0L/min rate2Gas carries out carburizing reagent, and pH meter tracks the pH value variation of reaction solution, when pH value is 7
Stop reaction, product, which is filtered, washed, obtains nano-calcium carbonate calcium product with after 60 DEG C of vacuum drying.
(2) nanometer calcium carbonate for weighing 0.9600g step (1) preparation is dispersed in 240mL dehydrated alcohol, 400w ultrasound point
1h is dissipated, the nanometer calcium carbonate dispersion liquid of 4mg/mL is obtained.
(3) it accurately weighs 0.1200g Fluorin doped graphene oxide to be dispersed in 120mL water, 400w ultrasonic disperse 2h, glass
Stick auxiliary stirring, 4 DEG C of refrigerator preservations, concentration 1mg/mL.
(4) the Fluorin doped graphene oxide dispersion of 7.5mL step (3) is taken to be added in the dispersion liquid of step (2), Yu Chang
The lower 360w ultrasound 0.5h of temperature, is then centrifuged at a high speed, product obtains Fluorin doped graphene oxide content in 60 DEG C of dry 18h
For the Fluorin doped graphene oxide calcium carbonate nano composite material of 0.78wt.%.
(5) the Fluorin doped stannic oxide/graphene nano calcium carbonate nano composite material 1.5g for accurately weighing step (4), is added to
Mechanical stirring in 100g areidofat grinds the Fluorin doped oxidation of three times obtained 1.5wt.% on three-roll grinder after mixing
Graphene carbonic acid grease of calcium sample.
(6) SRV-IV type micro-moving frictional wear testing machine is selected, testing time 30min, test temperature are 25 DEG C, test
Load 100N, test frequency 20Hz, test amplitude 1mm.It tries on used and lower examination disk material is 52100 steel of SAE, hardness
60±2HRC.On try surface roughness be 0.025 ± 0.005 μm, diameter 10mm, lower examination dish cart surface roughness is about 0.016 μ
M, diameter 24mm, thickness 7.85mm.
In conjunction with attached drawing 6, discovery is added to the areidofat of Fluorin doped graphite oxide alkenyl calcium carbonate nano composite material and adds
The areidofat and additive-free areidofat for having added nano-calcium carbonate particles are compared, the average friction coefficient difference in half an hour
Reduce 26.80%, 12.88%, the running-in stage and it is steady run time, antifriction performance is significantly increased.
Claims (5)
1. a kind of graphene-based calcium carbonate nano composite material of lubricating grease, which is characterized in that the graphene-based calcium carbonate is received
Nano composite material is stannic oxide/graphene nano calcium carbonate, N doping stannic oxide/graphene nano calcium carbonate, Fluorin doped graphene oxide
Nanometer calcium carbonate, wherein graphene oxide, N doping graphene oxide, Fluorin doped graphene oxide content are graphene-based carbonic acid
0.78wt.%, 1.56wt.%, 3.125wt.%, 6.25wt.% of calcium nanocomposite.
2. a kind of graphene-based calcium carbonate nano composite material of lubricating grease according to claim 1, which is characterized in that institute
Stating graphene oxide, N doping graphene oxide, Fluorin doped graphene oxide is finely dispersed layer structure.
3. a kind of lubricating grease preparation method of graphene-based calcium carbonate nano composite material, which is characterized in that including following step
It is rapid:
(1) 2-10g CaO is digested to obtain calcium hydroxide suspension with the 100mL secondary distilled water that temperature is 80 DEG C, was aged
Night is added lauric acid/ethanol solution of 0-30mL 0.05-0.50mol/L, 2h is stirred to react at room temperature, then in water bath with thermostatic control
CO2 gas is passed through with 0.2-1.5L/min rate and carries out carburizing reagent, and it is 7 to pH value that pH meter, which tracks the pH value variation of reaction solution,
When stop reaction, product be filtered, washed with 60 DEG C vacuum drying after obtains nano-calcium carbonate calcium product；
(2) nanometer calcium carbonate for weighing 240-1920mg step (1) preparation is dispersed in 240mL dehydrated alcohol, 400w ultrasound point
1h is dissipated, finely dispersed nanometer calcium carbonate dispersion liquid, concentration 1-8mg/mL are obtained；
(3) 24-120mg graphene oxide or N doping graphene oxide or Fluorin doped graphene oxide are accurately weighed, is dispersed in
In 120mL water, 400w ultrasonic disperse 2h, glass bar auxiliary stirring, concentration 0.2-1mg/mL, 4 DEG C of refrigerator preservations；
(4) the graphene-based dispersion liquid of 7.5mL, 15mL, 30mL, 60mL step (3) is taken to be added to the 240mL of step (2) respectively
In nanometer calcium carbonate dispersion liquid, 360w ultrasound 0.5h, is then centrifuged at a high speed under room temperature, and product is obtained in 60 DEG C of dry 18h
To graphene oxide or N doping graphene oxide or Fluorin doped graphene oxide content be 0.78wt.%, 1.56wt.%,
The graphene-based calcium carbonate nano composite material of 3.125wt.%, 6.25wt.%.
4. a kind of preparation method of the graphene-based calcium carbonate nano composite material of lubricating grease according to claim 3,
It is characterized in that, the calcium carbonate is the nanometer calcium carbonate of calcite crystal form, partial size 20-100nm.
5. a kind of preparation method of the graphene-based calcium carbonate nano composite material of lubricating grease according to claim 3,
It is characterized in that, the lauric acid is chemical additives.
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| CN111892982A (en) * | 2020-08-21 | 2020-11-06 | 北京化工大学 | Preparation method of nitrogen-doped nano lubricating material |
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Application publication date: 20181228 |