Method for stably dispersing graphene powder in gear box oil
Technical Field
The invention relates to the field of graphene, in particular to a method for stably dispersing graphene powder in gear box oil.
Background
According to the quality level, the American Petroleum institute divides the automobile gear oil into five grades (GL-1-GL-5). GL-1-GL-3 has low performance requirement, and is used for lubricating spur gears, bevel gears, gearboxes, steering gears and other gears under general load. GL-4 is used for lubricating a hyperbolic gear transmission shaft and a manual transmission of an automobile under the conditions of high speed, low torque and low speed and high torque. GL-5 has the highest performance level and is used for lubricating a hyperbolic gear transmission shaft and a manual gearbox with high impact load under severe operating conditions. The gear oil of the gearbox is replaced once for 2 years or 6 kilometers under the normal driving condition
The automatic gearbox needs to frequently check the oil level of the gearbox and regularly replace the oil of the gearbox in maintenance, and a popular series of vehicle types are taken as an example: vehicles equipped with automatic or manual gearboxes require that the automatic gearbox oil and oil grid must be changed every sixty thousand kilometers, and for vehicles equipped with gearbox oil filters, the filters must be changed simultaneously when changing oil.
After the gear box runs for a period of time, a large amount of scrap iron is generated due to abrasion, a small amount of scrap iron is attracted by the magnet on the oil plug, but the performance of lubricating oil is affected due to too much scrap iron, so that oil is changed at intervals, and the loss of the gear box is rapidly increased.
Generally, automobile manufacturers recommend replacement every 4-6 kilometers, the service life does not exceed 3 years, particularly, the automatic gearbox has high maintenance cost and high requirements on oil products. Not only the lubricating/heat dissipating/corrosion preventing function but also the power transmission function is required. Once the oil product does not reach the use standard of the gearbox, the parts of the gearbox can be seriously damaged, and even the temperature of the oil in the self-changing box rises to 80 ℃ under the ordinary driving condition, and the temperature is the normal working temperature of the ordinary atf. If atf can be constantly maintained at an operating temperature of 80 degrees Celsius, its lifetime can reach 150000 kilometers. However, if the temperature rises higher, the service life of the gearbox is reduced, the gearbox is scrapped, the maintenance and replacement cost of the gearbox is extremely high, and the maintenance difficulty is high.
The oil temperature of a gearbox of a vehicle is usually lower than 135 ℃ under the normal running state. However, when the vehicle is used excessively, such as an overloaded trailer, or is set in a snow or off-road mode in the four-wheel drive mode, the vehicle is running under an excessive slip condition of the torque converter, which may cause the gearbox oil temperature to reach 135 ℃. When the Oil temperature of the gearbox reaches 135 ℃, the additionally arranged Oil temperature Overheating prompting system of the gearbox simultaneously gives an early warning by displaying 'Oo 135 c' (note that 'Oo' means 'Oil over') information and sounding a bell. The purpose of early warning is to actively remind a user to park and hang a hand brake in a neutral position and keep an engine in an idling state, so that the liquid circulation is in a cooling mode to carry out rapid cooling until an alarm signal is not displayed any more. This operation will avoid the potential safety hazard that exists because the oil temperature continues to rise.
If the automobile user cannot take the parking action in time after receiving the early warning, the oil temperature overheating prompting system of the gearbox continuously gives an alarm, and meanwhile, the lubricating performance of the oil of the gearbox is weakened along with the rise of the oil temperature. When the oil temperature reaches 143 c, the gearbox oil is likely to lose lubrication properties, which will cause the internal components of the gearbox to fail due to frictional overheating.
The time interval from 135 ℃ when the warning is given to 143 ℃ when the gearbox oil or the lubrication performance is lost is greatly different according to different driving conditions on the spot. The time between driving is the shortest in the most extreme case. For example, if the vehicle is continuously stuck in sand for a long time (20 minutes) and the wheels rotate slowly, the time interval from the early warning is about 25 to 35 seconds until the oil temperature reaches 143 ℃. Once the user has not taken timely and effective action, which can cause the gearbox oil temperature to surge and exceed 200 ℃, the gearbox oil will boil or even splash. However, when the vehicle is used correctly, the temperature of the gearbox oil is difficult to reach 135 ℃ from 115 ℃, and the oil temperature can not rise to 143 ℃ continuously unless the vehicle is operated illegally, for example, the vehicle is operated in a red line area of an engine for a long time, and the transfer case is not used correctly, so that accidents occur.
Graphene (Graphene) is a new material with a monolayer sheet structure composed of carbon atoms. Is a two-dimensional material with a thickness of only one carbon atom, which is a hexagonal honeycomb lattice of planar thin films of carbon atoms with sp2 hybridized orbitals. In 2004, physicists andreli haim and costatin norworth schloff, manchester university, uk, succeeded in separating graphene from graphite in experiments, and confirmed that it can exist alone, and two people also obtained a 2010 nobel prize in physics together due to the "pioneer experiment on two-dimensional graphene materials".
Graphene is the thinnest and most rigid nanomaterial in the world, and is almost completely transparent, absorbing only 2.3% of light; the heat conductivity coefficient is as high as 5300W/m.K, higher than that of carbon nano tube and diamond, and its electron mobility is over 15000cm2The resistivity of the material is only about 10-6 omega cm and lower than that of copper or silver, and the material has the minimum resistivity in the world. Because of its extremely low resistivity and high electron transfer rate, it is expected to be used for developing a new generation of thinner and faster-conducting electronic devices or transistors. Since graphene is essentially a transparent and good conductor, it is also suitable for manufacturing transparent touch screens, optical panels, and even solar cells. Another characteristic of graphene is that the quantum hall effect can be observed at normal temperature.
The arrangement of carbon atoms of graphene is similar to that of a single-atomic layer of graphite, and is a single-layer two-dimensional crystal in which carbon atoms are arranged in a honeycomb lattice (honey comb lattice) in sp2 mixed domains. Graphene can be thought of as an atomic size network formed by carbon atoms and their covalent bonds. The nomenclature of graphene comes from the english graphete (graphite) + -ene (end of alkene). Graphene is considered to be a planar polycyclic aromatic hydrocarbon atom crystal.
The graphene has a very stable structure with only carbon-carbon bonds (carbon-carbon bonds)
The connection between the carbon atoms in the graphene is flexible, and when external force is applied to the graphene, the carbon atom surface can be bent and deformed, so that the carbon atoms do not need to be rearranged to adapt to the external force, and the structure is kept stable. This stable lattice structure gives graphene excellent thermal conductivity.
The advent of graphene has caused a worldwide research booming. The lubricant is the thinnest one of the known materials, has firm and hard materials, and has excellent chemical stability and excellent mechanical lubricating property at room temperature. It has the following distinctiveness:
firstly, the method comprises the following steps: graphene is the strongest material in the world, and it has been estimated that if graphene is used to form a film (thickness of about 100 nm) having a thickness corresponding to the thickness of a common plastic food packaging bag, it will withstand the pressure of about two tons of heavy articles without breaking.
Secondly, the method comprises the following steps: graphene is the best conductive material in the world.
The graphene material is also an excellent modifier, and has very unique advantages in mechanical lubrication, especially on the addition of gearbox oil of an engine. In the prior art, commercially available graphene is dispersed in an organic solvent, a dispersing agent is added, and then the graphene is dispersed in gear box oil by intense friction mixing of a high-shear machine. The disadvantages of the current products are as follows:
1) generally, the quality of the graphene powder sold in the market is quite different, the number of layers of the graphene may be different from 100 to 500, the ratio of the area to the thickness of a microchip is about 3000 times, and the area of the microchip is large and the lattice is complete. Traditional graphene gearbox oil is prepared by a high-shear force method, and graphene powder is inserted into molecules of the gearbox oil at a high speed of 2000-20000 rpm, so that the defect that the graphene powder is easily damaged and the gearbox oil is also damaged is overcome.
2) In the market, the intense physical shearing force is mostly utilized, so that the basic structures of graphene and gearbox oil are damaged, and the serious agglomeration effect is caused.
Disclosure of Invention
The invention aims to provide a simple method for stably dispersing graphene powder in gearbox oil.
In order to achieve the above object, the present invention provides a method for stably dispersing graphene powder in gearbox oil, which is characterized by comprising the following steps:
gear box oil pretreatment: expanding the molecules of the gearbox oil by a physical method or heating to open the molecular chains to obtain pretreated gearbox oil;
pretreatment of graphene powder: vibrating graphene powder by modulated ultrasonic waves, wherein the vibration frequency is 40-240 Hz, and obtaining pretreated graphene powder;
mixing and stirring: mixing the obtained pretreated gear box oil and the pretreated graphene powder together, slowly stirring to insert the graphene powder into long-chain molecules of the gear box oil, maintaining a stable state to enable the molecules to be mature, and completing the insertion.
Further, in the step of gear box oil pretreatment, the physical method is stirring equipment, and stirring is carried out at a constant speed of 30-200 rpm for 30 minutes-1 hour;
the heating is 50-100 ℃; preferably, the heating is 50-80 ℃.
Further, in the step of preprocessing the graphene powder, oscillation is carried out for 20-40 minutes under the condition of 40-60 Hz, then the frequency is gradually increased at the speed of 15-25 Hz/minute, the frequency is increased to 230-250 Hz after 8-15 minutes, and oscillation is continuously carried out for 30-40 minutes.
Further, in the step of preprocessing the graphene powder, the oscillation condition is that oscillation is carried out for 20-40 minutes at 40-60 Hz, then the frequency is gradually increased to the speed of 20 Hz/minute, the frequency is increased to 240Hz after 10 minutes, and oscillation is continuously carried out for 30-40 minutes.
Further, the weight usage ratio of the gear box oil pretreated in the mixing and stirring step to the graphene powder pretreated in the mixing and stirring step is (0.1-10): 100, respectively; preferably, (3-10): 100.
further, in the mixing and stirring step, the low-speed stirring is carried out at 20-40 rpm and 80-100 ℃ for 3-6 hours; preferably, it is 30rpm, 80 ℃ and stirred for 4 hours.
Further, the stable state is maintained at 30-200 rpm, 80-100 ℃ for 3-6 hours.
The invention also provides a product prepared by the method for stably dispersing the graphene powder in the gear box oil.
Those skilled in the art are aware of: the viscosity of the grease generally decreases with the increase of temperature, and the viscosity must be kept as consistent as possible in the mechanism of the gearbox oil, so additives are generally added or the physical properties of the gearbox oil are generally changed, so that the gearbox oil keeps a certain range of viscosity in the temperature gradient to ensure the lubricating effect of the gearbox oil. Heating changes the physical properties of the gearbox oil, mostly the deformation of long chain structures. The gearbox oil molecules must be expanded and the molecular chains are opened in order to insert the graphene powder, and the applicant of the invention finds that the effect is optimal at 50-100 ℃; or for the uniformity of the temperature, physical stirring equipment is adopted, and the mixture is stirred for 30 minutes to 1 hour at a constant speed of about 30 to 200 rpm.
The product obtained by the method is also called graphene gear oil protective agent. The obtained graphene gear oil protective agent does not damage graphene powder and is uniformly dispersed; the gear box oil structure is not damaged at all, and the original function of the gear box oil can be maintained.
Through field tests for more than three years by a team, the graphene gear oil protective agent obtained by the invention can effectively repair the worn part of the engine in a physical mode and ensure the healthy operation of a transmission system of the vehicle engine. The service life of the vehicle gear transmission box is prolonged. And (4) integrating the experimental results to obtain the conclusion of the final test:
1. the generator gearbox operating noise is significantly reduced from 60 db to 52 db measured at a fixed location (using a TES-1350a 1351B noise meter sound tester noise meter high accuracy industrial decibel meter).
2. The engine is feeling smooth during shifting during operation.
3. The self-propelled vehicle is free of previous jerks and jerks of significant gear shifts during a launch operation.
1) The nano-graphene powder can increase the fine friction coefficient on the transmission gear, increase the lubricating effect between gears and reduce the gear abrasion.
2) The lubrication degree of the gear transmission machinery is improved, and the purpose of saving energy by 8-10% of gasoline consumption of an engine is achieved.
3) Because the gear box has good mechanical lubricity and reduced friction force, the automobile becomes lubricous during speed change, and the friction force of the gear is reduced to achieve the effects of noise reduction and shock absorption.
Drawings
Fig. 1 photo of graphene powder uniformly dispersed in gearbox oil.
Detailed Description
Reference will now be made in detail to embodiments of the present invention, examples of which are illustrated in the accompanying drawings, wherein like or similar reference numerals refer to the same or similar elements or elements having the same or similar function throughout. The embodiments described below with reference to the drawings are illustrative and intended to be illustrative of the invention and are not to be construed as limiting the invention. The examples do not specify particular techniques or conditions, and are performed according to the techniques or conditions described in the literature in the art or according to the product specifications. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products commercially available.
Parameters of the graphene powder used in the following examples:
layer number: 3-10 layers with volume density of 0.34-0.41g/cm3Average thickness of 4.2nm, transverse size of 10-80 μm, and carbon purity>80% free of functional groups, characterized by a Raman 2D peak width of 55-60/cm and a characteristic Raman I2D/IG ratio of 0.4-0.7.
Example 1: method for stably dispersing graphene powder in gearbox oil
Gear box oil pretreatment: stirring for 30 minutes to 1 hour at a constant speed of 30 to 60rpm by using stirring equipment to expand the molecules of the gearbox oil and open the molecular chains to obtain pretreated gearbox oil;
pretreatment of graphene powder: vibrating graphene powder for 20-40 minutes under the condition of modulating ultrasonic waves, gradually increasing the frequency at the speed of 20 Hz/minute to 240Hz, and staying at 240Hz to continue vibrating for 30-40 minutes; obtaining pretreated graphene powder;
mixing and stirring: mixing the obtained pretreated gearbox oil and pretreated graphene powder together, wherein the mass ratio of the pretreated gearbox oil to the pretreated graphene powder is 10:100, 20rpm and 100 ℃, stirring is carried out for 3 hours, so that the graphene powder is inserted into the long-chain molecules of the gearbox oil, a stable state is maintained, the molecules are mature, and insertion is completed. The photo of the obtained graphene gear oil protective agent observed by a microscope with a magnification of 100 is shown in fig. 1. As can be seen from fig. 1, the obtained graphene gear oil protective agent is uniformly dispersed without agglomeration, which indicates that the graphene powder is stably dispersed in the gear oil.
The obtained graphene gear oil protective agent is added into a gearbox, and the running noise of the generator gearbox is obviously reduced to a fixed position (a noise meter uses a TES-1350A 1351B noise meter sound tester noise meter high-precision industrial decibel meter) and the measured noise is reduced from 60 decibels to 52 decibels. While the engine is shifting gears during operation with a smooth feel. The self-propelled vehicle is free of previous jerks and jerks of significant gear shifts during a launch operation.
Example 2: method for stably dispersing graphene powder in gearbox oil
Gear box oil pretreatment: heating at 60 ℃ to expand the molecules of the gearbox oil and open molecular chains to obtain pretreated gearbox oil;
pretreatment of graphene powder: vibrating graphene powder for 20-40 minutes under the condition of modulating ultrasonic waves, gradually increasing the frequency to 15 Hz/minute, increasing the frequency to 230Hz, staying at 230Hz, and continuing to vibrate for 30-40 minutes to obtain pretreated graphene powder;
mixing and stirring: mixing the obtained pretreated gear box oil and the pretreated graphene powder together, wherein the mass ratio of the pretreated gear box oil to the pretreated graphene powder is 3:100, 30rpm and 80 ℃, stirring at a low speed for 4 hours to enable the graphene powder to be inserted into long-chain molecules of the gear box oil, maintaining a stable state to enable the molecules to be mature, and completing insertion to obtain the graphene gear oil protective agent.
The obtained graphene gear oil protective agent is added into a gearbox, and the running noise of the generator gearbox is obviously reduced to a fixed position (a noise meter uses a TES-1350A 1351B noise meter sound tester noise meter high-precision industrial decibel meter) and the measured noise is reduced to 51 decibels from 60 decibels. While the engine is shifting gears during operation with a smooth feel. The self-propelled vehicle is free of previous jerks and jerks of significant gear shifts during a launch operation.
Example 3: method for stably dispersing graphene powder in gearbox oil
Gear box oil pretreatment: heating at 100 ℃ to expand the molecules of the gearbox oil and open molecular chains to obtain pretreated gearbox oil;
pretreatment of graphene powder: vibrating graphene powder for 20-40 minutes under the condition of modulating ultrasonic waves, gradually increasing the frequency to 25 Hz/minute, increasing the frequency to 250Hz, staying at 250Hz, and continuing to vibrate for 30-40 minutes to obtain pretreated graphene powder;
mixing and stirring: mixing the obtained pretreated gear box oil and the pretreated graphene powder together, wherein the mass ratio of the pretreated gear box oil to the pretreated graphene powder is 0.1:100, 40rpm and 90 ℃, slowly stirring for 5 hours, inserting the graphene powder into long-chain molecules of the gear box oil, maintaining a stable state to ensure that the molecules are mature, and completing insertion to obtain the graphene gear oil protective agent.
The obtained graphene gear oil protective agent is added into a gearbox, and the running noise of the generator gearbox is obviously reduced to a fixed position (a noise meter uses a TES-1350A 1351B noise meter sound tester noise meter high-precision industrial decibel meter) and the measured noise is reduced from 60 decibels to 53 decibels. While the engine is shifting gears during operation with a smooth feel. The self-propelled vehicle is free of previous jerks and jerks of significant gear shifts during a launch operation.
Example 4: method for stably dispersing graphene powder in gearbox oil
Gear box oil pretreatment: heating at 80 ℃ to expand the gearbox oil molecules and open molecular chains to obtain pretreated gearbox oil;
pretreatment of graphene powder: vibrating graphene powder for 20-40 minutes under the condition of modulating ultrasonic waves, gradually increasing the frequency to 20 Hz/minute, increasing the frequency to 240Hz, staying at 240Hz, and continuing to vibrate for 30-40 minutes to obtain pretreated graphene powder;
mixing and stirring: mixing the obtained pretreated gear box oil and the pretreated graphene powder together, wherein the mass ratio of the pretreated gear box oil to the pretreated graphene powder is 50:100, 20rpm and 80 ℃, stirring at a low speed for 6 hours to enable the graphene powder to be inserted into long-chain molecules of the gear box oil, maintaining a stable state to enable the molecules to be mature, and completing insertion to obtain the graphene gear oil protective agent.
The obtained graphene gear oil protective agent is added into a gearbox, and the running noise of the generator gearbox is obviously reduced to a fixed position (a noise meter uses a TES-1350A 1351B noise meter sound tester noise meter high-precision industrial decibel meter) and the measured noise is reduced from 60 decibels to 52 decibels. While the engine is shifting gears during operation with a smooth feel. The self-propelled vehicle is free of previous jerks and jerks of significant gear shifts during a launch operation.
Example 5: method for stably dispersing graphene powder in gearbox oil
Gear box oil pretreatment: heating at 50 ℃ to expand the molecules of the gearbox oil and open molecular chains to obtain pretreated gearbox oil;
pretreatment of graphene powder: vibrating graphene powder for 20-40 minutes under the condition of modulating ultrasonic waves, gradually increasing the frequency to 20 Hz/minute, increasing the frequency to 240Hz, staying at 240Hz, and continuing to vibrate for 30-40 minutes to obtain pretreated graphene powder;
mixing and stirring: mixing the obtained pretreated gear box oil and the pretreated graphene powder together, wherein the mass ratio of the pretreated gear box oil to the pretreated graphene powder is 7:100, 20rpm and 80 ℃, stirring at a low speed for 6 hours to enable the graphene powder to be inserted into long-chain molecules of the gear box oil, maintaining a stable state to enable the molecules to be mature, and completing insertion to obtain the graphene gear oil protective agent.
The obtained graphene gear oil protective agent is added into a gearbox, and the running noise of the generator gearbox is obviously reduced to a fixed position (a noise meter uses a TES-1350A 1351B noise meter sound tester noise meter high-precision industrial decibel meter) and the measured noise is reduced from 60 decibels to 53 decibels. While the engine is shifting gears during operation with a smooth feel. The self-propelled vehicle is free of previous jerks and jerks of significant gear shifts during a launch operation.
Although embodiments of the present invention have been shown and described above, it is understood that the above embodiments are exemplary and should not be construed as limiting the present invention, and that variations, modifications, substitutions and alterations can be made in the above embodiments by those of ordinary skill in the art without departing from the principle and spirit of the present invention.