CN103289802A - Preparation method of graphene lubricating grease - Google Patents
Preparation method of graphene lubricating grease Download PDFInfo
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- CN103289802A CN103289802A CN2013102282440A CN201310228244A CN103289802A CN 103289802 A CN103289802 A CN 103289802A CN 2013102282440 A CN2013102282440 A CN 2013102282440A CN 201310228244 A CN201310228244 A CN 201310228244A CN 103289802 A CN103289802 A CN 103289802A
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Abstract
The invention relates to a preparation method of a graphene lubricating grease. The graphene lubricating grease as a compound is prepared from the following components in parts by weight: 100 parts of lubricating grease and 0.001 to 0.1 part of surface-modified graphene powder, wherein the surface-modified graphene powder is prepared by using a solvent method; a surface-modified coupling agent accounts for 0.5wt%-2wt% of the graphene powder; the graphene is dispersed in a solvent containing the coupling agent at the temperature of 30 to 60 DEG C and then is filtered and dried, thereby obtaining the modified graphene powder. As the method is used, the defects of poor mixing uniformity, low utilization rate, high addition quantity and the like in the prior art are overcome. By utilizing the characteristics of the graphene which is ultrathin, ultrahard and superlubricant as well as in corrosion resistance and high-temperature resistance, based on the higher molecular modification of the surface of the graphene and the high-dispersion mixing of the graphene with a lubricating agent, the graphene-based lubricating product is prepared. The graphene-based lubricating product can be used for obviously improving the lubricating performance of the lubricating agent, so that the friction and the abrasion of a mechanical movement surface are reduced greatly. Thus, the effects of material saving and energy conservation are realized.
Description
Technical field
The invention belongs to lubrication technical field, particularly a kind of Graphene preparation of greases method.
Background technology
According to internal authority mechanism statistics, metallic substance wearing and tearing, corrosion and fatigue three lossies account for 30% of gross industrial output value, and frictional wear is universal phenomenon in nature.Frictionloss the primary energy source in the world about 1/3rd, wearing and tearing are to cause one of three kinds of topmost forms of material and damage of facilities and inefficacy, and are lubricated then be the effective technology that reduces friction, reduces or avoid wearing and tearing.Development have good resistance polishing machine, high bearing capacity, to wear surface have certain repairing effect, to adding up according to internal authority mechanism, metallic substance wearing and tearing, corrosion and fatigue three lossies account for 30% of gross industrial output value, and frictional wear is universal phenomenon in nature.Frictionloss the primary energy source in the world about 1/3rd, wearing and tearing are to cause one of three kinds of topmost forms of material and damage of facilities and inefficacy, and are lubricated then be the effective technology that reduces friction, reduces or avoid wearing and tearing.Development has good resistance polishing machine, high bearing capacity, wear surface is had the lubrication technology of certain repairing effect, environmentally safe or less contamination, is chemistry and one of important topic of Materials science and tribology in the present age.
It mainly is the organic compound of sulfur-bearing, chlorine and phosphorus that traditional extreme pressure grease improves extreme pressure and antiwear behavior, although extreme pressure property is better, sulphur, chlorine and phosphorus compound can produce corrosion and problem of environmental pollution.And the efficient extreme pressure anti-wear additives of the zinc dialkyl dithiophosphate of widespread use (ZDDP), the needs that now seemed and be difficult to adapt to the situation development.This be because: (1) element Zn can make some alloy bearing (mainly referring to argentiferous, plumbous parts) produce galvanic corrosion; (2) under the operating mode that is higher than 160 degree, can lose anti-oxidant and extreme pressure and antiwear behavior because sharply decomposing.Therefore, searching can overcome the focus that the circumscribed novel extreme pressure anti-wear additives of ZDDP has become the lubricating grease research and development.
It mainly is to be extreme pressure anti-wear additives with superfine graphite and molybdenumdisulphide pressed powder that the high temperature extreme pressure grease improves extreme pressure property; be exclusively used in the lubricated of high temperature friction parts under heavy loading/impact load or the humidity/contaminate environment and bearing, rust resistance and corrosion resistance protection to greatest extent is provided.The Applicable temperature scope :-20~+ 450 ℃, the highest intermittence, heatproof can reach 500 ℃.But the particle size of the superfine graphite that is to use and molybdenumdisulphide powder is micron-scale, and shortcoming is that mixing uniformity is poor, and utilization ratio is low, the addition height.
Graphene (Graphene) is a kind of novel material of the individual layer sheet structure that is made of carbon atom.Be a kind ofly to form the flat film that hexangle type is the honeycomb lattice by carbon atom with the sp2 hybridized orbital, have only the two-dimensional material of a carbon atom thickness.Graphene be at present the thinnest in the world be the hardest nano material also, the range of application of Graphene is wide.Ultra-thin according to Graphene, the characteristic of intensity super large, Graphene can be widely used in each field, such as the ultralight flak jackets, ultra-thin and ultra-light type aircraft material etc.Graphene is the highest material of human known strength, and is also harder than diamond, and strength ratio is taller last 100 times of best iron and steel in the world.
Summary of the invention
Purpose of the present invention just is to overcome above-mentioned defective, develops a kind of Graphene preparation of greases method.
Technical scheme of the present invention is:
A kind of Graphene preparation of greases method, its major technique is characterised in that the component of described mixture and content consist of: 100 weight part lubricating grease, the surface modified graphite alkene powder of 0.001-0.1 weight part; What described surface modified graphite alkene powder adopted is solvent method, the surface modification coupling agent is the weight content 0.5-2% of Graphene powder, under temperature 30-60 ℃ condition, Graphene is dispersed in the solvent that contains coupling agent and handles, filter, drying obtains the modified graphene powder.
Described lubricating grease comprises lithium soap grease, quicklime grease, sodium base grease, aluminium soap grease, complex soap lubricating grease, extreme pressure grease, silicic acid lubricating grease, synthetic grease.
The weight content of Graphene is 0.1%-0.001% in the above-mentioned mixture, and preferred weight content is 0.001%-0.004%.
Among the above-mentioned preparation method, described lubricating grease comprises lithium soap grease, quicklime grease, sodium base grease, aluminium soap grease, complex soap lubricating grease, extreme pressure grease, silicic acid lubricating grease, synthetic grease.
Among the above-mentioned preparation method, what the Graphene modification was adopted is solvent method, and wherein the surface modification coupling agent is the 0.5-2% of Graphene, is preferably 0.5-1.0%.
Among the above-mentioned preparation method, the surface modification coupling agent is silica-based coupling agent, aluminium base coupling agent, and titanium base coupling agent, the aluminium base coupling agent of titanium, a kind of or two or more in the titanium zirconium base coupling agent.
Among the above-mentioned preparation method, Graphene and coupling agent solvent are handled 3-8h under temperature 30-60 ℃ condition, handle 3-5h under preferred 30-40 ℃ of condition.
Among the above-mentioned preparation method, Graphene is to mix, shear, grind in homogeneous, the degassing stage or two at preparation of greases stage saponification reaction, the dehydration that heats up, high temperature refining, chilling to add more than the stage.
Advantage of the present invention and effect are to utilize the characteristic of ultra-thin, superhard, super lubricated, corrosion-resistant, the high-temperature stability of Graphene, macromolecule modified and mix with the lubricant high dispersive by Graphene surface, the graphene-based lubricated product of system, this product can significantly improve the lubricity of lubricant, significantly reduce the friction and wear on mechanical movement surface, have material-saving and effect of saving energy.
Other concrete advantages of the present invention and effect will go on to say below.
Description of drawings
Fig. 1---each data contrast synoptic diagram in the various embodiments of the present invention.
Embodiment
Embodiment 1:
The 1g Graphene is joined the solvent that contains the silica-based coupling agent of 0.02g, be 60 ℃ in temperature and handle 3h, make the modified graphene powder after filtration, the drying; With the preheating of grease base plinth oil, add hydroxystearic acid then, calcium hydroxide aqueous solution and 0.1% above-mentioned modified graphene, be warming up to 200-220 ℃ of dehydration after 3 hours 105-110 ℃ of saponification, be chilled to temperature 150-170 ℃, shearing then, homogeneous and the degassing make graphene-based quicklime grease.
Embodiment 2:
The 1g Graphene is joined the solvent that contains 0.005g titanium base coupling agent, be 30 ℃ in temperature and handle 3h, make the modified graphene powder after filtration, the drying.With the preheating of grease base plinth oil, add hydroxystearic acid and lime acetate compound fat acid calcium then, be warming up to 200-220 ℃ of dehydration after 3 hours 105-110 ℃ of saponification, be chilled to temperature 150-170 ℃, the above-mentioned modified graphene of adding 0.05%, shearing then, homogeneous and the degassing make graphene-based compound calcium grease.
Embodiment 3:
The 1g Graphene is joined the solvent that contains the aluminium base coupling agent of 0.01g, be 40 ℃ in temperature and handle 8h, make the modified graphene powder after filtration, the drying.With the preheating of grease base plinth oil, add hydroxystearic acid then, aqueous sodium hydroxide solution, add 0.004% above-mentioned modified graphene after 3 hours 105-110 ℃ of saponification, be warming up to 200-220 ℃ of dehydration, be chilled to temperature 150-170 ℃, shearing then, homogeneous and the degassing make graphene-based sodium base grease.
Embodiment 4:
The 1g Graphene is joined the solvent that contains the aluminium base coupling agent of 0.005g titanium, be 60 ℃ in temperature and handle 3h, make the modified graphene powder after filtration, the drying.With the preheating of grease base plinth oil, add hydroxystearic acid and aluminum stearate then, add 0.004% above-mentioned modified graphene after 3 hours 105-110 ℃ of saponification, be warming up to 200-220 ℃ of dehydration, be chilled to temperature 150-170 ℃, shearing then, homogeneous and the degassing make graphene-based aluminium soap grease.
Embodiment 5:
The 1g Graphene is joined the solvent that contains 0.005g titanium zirconium base coupling agent, be 60 ℃ in temperature and handle 3h, make the modified graphene powder after filtration, the drying.With the preheating of grease base plinth oil, add hydroxystearic acid and silicic acid then, be warming up to 200-220 ℃ of dehydration after 3 hours 105-110 ℃ of saponification, be chilled to temperature 150-170 ℃, the above-mentioned modified graphene of adding 0.004%, shearing then, homogeneous and the degassing make graphene-based silicic acid lubricating grease.
Embodiment 6:
The 1g Graphene is joined the solvent that contains 0.005g titanium zirconium base coupling agent, be 60 ℃ in temperature and handle 6h, make the modified graphene powder after filtration, the drying.With the preheating of grease base plinth oil, add hydroxystearic acid and silicic acid then, be warming up to 200-220 ℃ of dehydration after 3 hours 105-110 ℃ of saponification, be chilled to temperature 150-170 ℃, add then shear behind 0.05% the above-mentioned modified graphene, homogeneous and the degassing, make graphene-based quicklime grease.
Embodiment 7:
The 1g Graphene is joined the solvent that contains 0.01g titanium zirconium base coupling agent, be 60 ℃ in temperature and handle 5h, make the modified graphene powder after filtration, the drying.Synthetic oil preheating with lubricating grease, add hydroxystearic acid and tetrafluoroethylene lubricated granules then, be warming up to 200-220 ℃ of dehydration after 3 hours 105-110 ℃ of saponification, be chilled to temperature 150-170 ℃, add then shear behind 0.1% the above-mentioned modified graphene, homogeneous and the degassing, make graphene-based synthetic grease.
Embodiment 8:
The 1g Graphene is joined the solvent that contains 0.008g titanium zirconium base coupling agent, be 60 ℃ in temperature and handle 3h, make the modified graphene powder after filtration, the drying.Synthetic oil preheating with lubricating grease, add hydroxystearic acid and tetrafluoroethylene lubricated granules then, be warming up to 200-220 ℃ of dehydration after 3 hours 105-110 ℃ of saponification, be chilled to temperature 150-170 ℃, add then shear behind 0.1% the above-mentioned modified graphene, homogeneous and the degassing, make graphene-based synthetic grease.
As shown in Figure 1:
Check embodiment 1-8, as can be seen, the steel ball (Chrome Alloy Steel) with the production of U.S. Faville-Le Vally company in four-ball tester of general graphite extreme pressure grease in Graphene and the market is carried out wear-resistant collaborative comparison, and the compare extreme pressure property of conventional graphite lubricating grease of Graphene lubricating grease significantly improves.
Claims (8)
1. a Graphene preparation of greases method is characterized in that the component of described mixture and content consist of: 100 weight part lubricating grease, the surface modified graphite alkene powder of 0.001-0.1 weight part; What described surface modified graphite alkene powder adopted is solvent method, the surface modification coupling agent is the weight content 0.5-2% of Graphene powder, under temperature 30-60 ℃ condition, Graphene is dispersed in the solvent that contains coupling agent and handles, filter, drying obtains the modified graphene powder.
2. a kind of Graphene preparation of greases method according to claim 1 is characterized in that described lubricating grease comprises lithium soap grease, quicklime grease, sodium base grease, aluminium soap grease, complex soap lubricating grease, extreme pressure grease, silicic acid lubricating grease, synthetic grease.
3. a kind of Graphene preparation of greases method as claimed in claim 1 is characterized in that component and content composition: 100 weight part lubricating grease, the surface modified graphite alkene powder of 0.001-0.1 weight part.
4. a kind of Graphene preparation of greases method as claimed in claim 1 is characterized in that the surface modification coupling agent is the 0.5-2% of Graphene powder.
5. a kind of Graphene preparation of greases method as claimed in claim 1 is characterized in that it is solvent method that modification is adopted, and Graphene and coupling agent solvent are handled 3-8h under temperature 30-60 ℃ condition, and filtration, drying obtain the modified graphene powder.
6. a kind of Graphene preparation of greases method as claimed in claim 1 is characterized in that the modification coupling agent is silica-based coupling agent, aluminium base coupling agent, and titanium base coupling agent, the aluminium base coupling agent of titanium, a kind of or two or more in the titanium zirconium base coupling agent.
7. a kind of Graphene preparation of greases method as claimed in claim 1 is characterized in that Graphene is to add in the preparation of greases process, and namely original position is synthetic.
8. a kind of Graphene preparation of greases method as claimed in claim 1 is characterized in that Graphene is to mix, shear, grind in homogeneous, the degassing stage or two at preparation of greases stage saponification reaction, the dehydration that heats up, high temperature refining, chilling to add more than the stage.
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Application publication date: 20130911 |