CN115960655A - Lubricating oil additive for mechanical system and preparation method and application thereof - Google Patents
Lubricating oil additive for mechanical system and preparation method and application thereof Download PDFInfo
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- CN115960655A CN115960655A CN202211663026.5A CN202211663026A CN115960655A CN 115960655 A CN115960655 A CN 115960655A CN 202211663026 A CN202211663026 A CN 202211663026A CN 115960655 A CN115960655 A CN 115960655A
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- 230000000996 additive effect Effects 0.000 title claims abstract description 30
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- 238000002360 preparation method Methods 0.000 title claims abstract description 7
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- OYHQOLUKZRVURQ-NTGFUMLPSA-N (9Z,12Z)-9,10,12,13-tetratritiooctadeca-9,12-dienoic acid Chemical compound C(CCCCCCC\C(=C(/C\C(=C(/CCCCC)\[3H])\[3H])\[3H])\[3H])(=O)O OYHQOLUKZRVURQ-NTGFUMLPSA-N 0.000 claims description 3
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Abstract
The invention relates to a preparation method of a lubricating oil additive for a mechanical system, which comprises the following steps: (1) Weighing graphite-phase carbon nitride, adding a solvent, and performing ultrasonic dispersion to obtain a graphite-phase carbon nitride solution; (2) Adding a modifier, DMAP (dimethyl formamide) and DCC (dimethyl dichloroisocyanurate) into the graphite-phase carbon nitride solution obtained in the step (1), stirring, and heating and refluxing in an inert atmosphere for reaction; (3) After the reaction is finished, centrifuging to take out precipitate, washing with absolute ethyl alcohol and petroleum ether, and drying to obtain the product. The invention also provides a lubricating oil additive product prepared by the method and application. The lubricating oil additive provided by the invention can promote the repair nano material with a similar structure to be uniformly dispersed, reduce the existence of an agglomerated structure, effectively fill surface scratches and reduce mechanical damage, and realize the effects of friction reduction and wear resistance under the synergistic action of the nano material and the agglomerated structure.
Description
Technical Field
The invention relates to the technical field of lubricating oil, in particular to a lubricating oil additive for a mechanical system and a preparation method and application thereof.
Background
From a tribological point of view, friction wear directly results in energy loss of the mechanical equipment, leading to component failure and serious mechanical accidents, and lubrication is considered to be one of the most effective methods to reduce friction and control wear. With the extreme and harsh development of the working conditions and environment of mechanical systems, the lubricant additive has been widely applied to many types of machinery, and graphene, hexagonal boron nitride, metals (such as Cu, co and Ni) and metal oxides (such as Al) are used 2 O 3 ZnO and TiO 2 ) When the nano material is added into the lubricating oil, a friction chemical reaction oil film is formed on a friction contact surface to reduce friction and abrasion, and the wear resistance, the friction reduction and the lubricating performance of the lubricating oil can be obviously improved. Against this background, in order to minimize the negative effects of friction and wear in mechanical systems, extensive research is still being conducted on lubricants to develop a high performance industrial lubricating oil to meet the requirements of antifriction and antiwear properties under severe conditions and environments, which is always the core task in both academic and industrial fields. The proper amount of the additive can obviously improve the friction characteristic of the base oil, plays a key role in making up for the defects of the traditional lubricating oil, and especially has important significance in ensuring the longest service cycle of a mechanical system, reducing the operation cost and realizing the strategic goals of 'double carbon'.
At present, graphite-phase carbon nitride is used as a novel material consisting of carbon and nitrogen, is mainly applied to the fields of visible light photocatalysis, solar energy conversion, adsorption and the like, has the advantages of low cost, easiness in preparation, reliable thermal stability, environmental friendliness and the like, and can theoretically replace the traditional additive. In particular, the van der waals force between graphite-phase carbon nitride layers is weak, and the graphite-phase carbon nitride layers are easy to shear, so that the graphite-phase carbon nitride lubricating oil can be used as a lubricating oil additive in the friction field to improve the tribological performance, and has a good development prospect. Unfortunately, however, graphite-phase carbon nitrides have extremely high activity and surface energy, meaning that they have poor dispersibility in base oils, resulting in the presence of their multilayer agglomerated structures, so there has been little research currently directed to the use of graphite-phase carbon nitrides as base oil additives.
Therefore, the invention is especially provided.
Disclosure of Invention
In order to solve the technical problems in the prior art, the invention provides a lubricating oil additive for a mechanical system and a preparation method thereof.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
in a first aspect, the present invention provides a method for preparing a lubricating oil additive for a mechanical system, comprising the steps of:
(1) Weighing graphite-phase carbon nitride, adding a solvent, and performing ultrasonic dispersion to obtain a graphite-phase carbon nitride solution;
(2) Adding a modifier, DMAP (dimethyl formamide) and DCC (dimethyl dichloroisocyanurate) into the graphite-phase carbon nitride solution obtained in the step (1), stirring, and heating and refluxing in an inert atmosphere for reaction;
(3) After the reaction is finished, centrifuging to take out precipitate, washing with absolute ethyl alcohol and petroleum ether, and drying to obtain the product.
Preferably or alternatively, the concentration of graphite phase carbon nitride in the graphite phase carbon nitride solution is from 0.005 to 0.05g/mL.
Preferably or alternatively, the solvent is any one of deionized water, ethyl acetate, absolute ethyl alcohol, toluene and isopropanol.
Preferably or alternatively, the modifier comprises any one of oleic acid, linoleic acid, stearic acid, palmitic acid.
Preferably or alternatively, the mass ratio of the modifier, DMAP, DCC and graphite phase carbon nitride added in the step (2) is 30-40.
Preferably or alternatively, the heating reflux reaction in the step (2) is carried out at the temperature of 60-120 ℃ for 8-15h.
Preferably or optionally, in the step (3), the rotation speed of the centrifugation is 6000 to 12000rpm, and the centrifugation time is 5 to 10min.
Preferably or alternatively, in the step (3), the drying manner is any one of vacuum freeze drying, low-temperature vacuum drying, forced air drying and spray drying.
In a second aspect, the invention provides a lubricating oil additive for a mechanical system, prepared by the method.
In a third aspect, the invention also provides the use of the above lubricating oil additive in 150BS base oil.
Advantageous effects
Compared with the prior art, the invention has the beneficial effects that:
the graphite-phase carbon nitride lubricating oil additive is prepared by adopting a condensation reflux method, is easy to adsorb on the surface of a friction pair of a mechanical system, forms a lubricating oil film for preventing the surfaces from being in direct contact, and has better antifriction and antiwear effects. The method and the process are simple and efficient, the operation is convenient, and the industrial production is easy to realize;
further, the lubricant can be fully mixed with 150BS regenerated base oil through formula design and process adjustment, the problem of agglomeration caused by dispersion in the base oil is solved, the tribological performance of the 150BS regenerated base oil can be obviously improved, and the service life of a mechanical system is prolonged;
furthermore, the lubricating oil additive prepared by the invention does not contain elements such as sulfur, phosphorus, chlorine and the like, is environment-friendly, conforms to the low-carbon environment-friendly concept, and has great application potential as a high-efficiency lubricating oil additive.
Drawings
FIG. 1 is an SEM photograph of the surface of a friction pair of a four-ball friction test of example 1 group in example 1;
FIG. 2 is an SEM photograph of the surface of a friction pair of a four-ball friction test in example 2 of example 1;
FIG. 3 is an SEM photograph of the surfaces of friction pairs of a four-ball friction test in example 3 of example 1;
FIG. 4 is an SEM photograph of the surface of a friction pair of a four-ball friction test in example 4 of example 1;
FIG. 5 is an SEM photograph of the surface of a friction pair in a four-ball friction test of an air-white control group in example 1 of the effect of the present invention;
FIG. 6 is an SEM photograph of the surface of a friction pair of a four-ball friction test of comparative example 1 in example 1 of the effect of the present invention;
FIG. 7 is a result of testing the average friction coefficient in effect example 2 of the present invention;
fig. 8 is a result of measuring the diameter of the abrasion marks in example 2 of the effect of the present invention.
Detailed Description
In order to facilitate understanding of the present invention, the present invention will be described more fully and in detail with reference to the accompanying drawings and preferred experimental examples, but the scope of the present invention is not limited to the following specific examples.
Unless otherwise defined, all terms of art used hereinafter have the same meaning as commonly understood by one of ordinary skill in the art. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to limit the scope of the present invention.
Unless otherwise specifically stated, various raw materials, reagents, instruments, equipment and the like used in the present invention are commercially available or can be prepared by existing methods.
The graphite-phase carbon nitride used in the examples of the present invention was prepared as follows:
weighing 10g of melamine, placing the melamine in a 50mL corundum crucible with a cover, placing the crucible in a muffle furnace, heating to 550 ℃ at the heating rate of 5 ℃/min, calcining for 4 hours, naturally cooling to room temperature, and grinding to obtain yellow block-shaped powder; spreading a certain amount of yellow powder on a combustion ship, heating to 550 ℃ at the heating rate of 2 ℃/min, calcining for 2 hours, cooling, taking out, grinding, alternately washing for 3 times by using deionized water and absolute ethyl alcohol, and drying at 60 ℃ for 8 hours to obtain lamellar graphite-phase carbon nitride.
Example 1
The embodiment of the invention provides a lubricating oil additive for a mechanical system.
0.1g of graphite-phase carbon nitride is taken to be put into a 100mL flask, 20mL of ethyl acetate is added, and ultrasonic treatment with the frequency of 20-30 kHz is carried out for 5-30 min to ensure that the graphite-phase carbon nitride is uniformly dispersed.
4mL of palmitic acid, 0.16g of DMAP (4-dimethylaminopyridine) and 0.27g of DCC (N, N' -dicyclohexylcarbodiimide) were added thereto, and the mixture was refluxed at 90 ℃ for 10 hours under a nitrogen atmosphere with continuous stirring.
After the reaction is finished, centrifuging at 6000rpm for 10min, taking out precipitate, washing with absolute ethyl alcohol and petroleum ether for 3 times respectively, and drying in an oven at 100 ℃ overnight to obtain the product.
Example 2
The embodiment of the invention provides a lubricating oil additive for a mechanical system.
0.2g of graphite phase carbon nitride is put into a 100mL flask, 20mL of deionized water is added, and the graphite phase carbon nitride is uniformly dispersed by ultrasonic treatment with the frequency of 20-30 kHz for 5-30 min.
4mL of linoleic acid, 0.16g of DMAP and 0.27g of DCC were added, and the system was refluxed at 80 ℃ for 8 hours under a nitrogen atmosphere with continuous stirring.
After the reaction is finished, centrifuging at 6000rpm for 10min, taking out precipitate, washing 3 times by using absolute ethyl alcohol and petroleum ether respectively, and drying in an oven at 60 ℃ overnight to obtain the product.
Example 3
The embodiment of the invention provides a lubricating oil additive for a mechanical system.
0.2g of graphite-phase carbon nitride is put into a 100mL flask, 20mL of toluene is added, and ultrasonic treatment with the frequency of 20-30 kHz is carried out for 5-30 min to uniformly disperse the graphite-phase carbon nitride.
4mL of oleic acid, 0.16g of DMAP and 0.27g of DCC were added, the mixture was stirred continuously, and the system was refluxed at 110 ℃ for 12 hours under a nitrogen atmosphere.
After the reaction is finished, centrifuging at 6000rpm for 10min, taking out precipitate, washing with absolute ethyl alcohol and petroleum ether respectively for 3 times, and drying in an oven at 80 ℃ overnight to obtain the product.
Example 4
The embodiment of the invention provides a lubricating oil additive for a mechanical system.
0.2g of graphite phase carbon nitride is taken to be put into a 100mL flask, 20mL of absolute ethyl alcohol is added, and the graphite phase carbon nitride is uniformly dispersed by ultrasonic treatment with the frequency of 20-30 kHz for 5-30 min.
4mL of stearic acid, 0.16g of DMAP and 0.27g of DCC were added, and the system was refluxed at 80 ℃ for 15 hours under a nitrogen atmosphere with continuous stirring.
After the reaction is finished, centrifuging for 6min at 6000rpm, taking out precipitate, washing 3 times respectively by absolute ethyl alcohol and petroleum ether, and placing at-20 ℃ for vacuum freeze drying overnight to obtain the product.
Comparative example 1
The present comparative example provides a lubricating oil additive for use in a mechanical system.
0.1g of graphite-phase carbon nitride is taken to be put into a 100mL flask, 20mL of isopropanol is added, and the graphite-phase carbon nitride is uniformly dispersed by ultrasonic treatment for 5-30 min at the frequency of 20-30 kHz.
4mL of myristic acid, 0.16g of DMAP and 0.27g of DCC were added, and the system was refluxed at 80 ℃ for 10 hours under a nitrogen atmosphere with continuous stirring.
After the reaction is finished, centrifuging at 6000rpm for 5min, taking out precipitate, washing with absolute ethyl alcohol and petroleum ether for 3 times respectively, and drying in an oven at 80 ℃ overnight to obtain the product.
Effect example 1
The additive products prepared in examples 1-4 and comparative example 1 were added to 150BS base oil at 0.03wt% and magnetically stirred for 0.5h, ultrasonically dispersed for 0.5h to uniformly disperse the additive in the base oil, and each product was subjected to a four-ball friction test using 150BS base oil without additive as a blank.
The four-ball friction testing machine is a four-ball friction testing machine of MRS-10W type produced by Jinan Chenda testing machine manufacturing Limited.
The test parameters are as follows: the load is 392N, the oil temperature is 75 ℃, the test time is 30min, and the rotating speed is 1200r/min.
The steel balls used in the test are GCr15 steel balls (phi =12.7mm, 60-65 HRC) produced by Shanghai Steel ball factory Co., ltd, and the steel balls need to be ultrasonically cleaned in petroleum ether and absolute ethyl alcohol before and after the friction test.
After the test, the diameter of the abrasion mark was measured by a microcomputer universal tool microscope of model 19JPC-V manufactured by the same marine optical instrument factory, and the surface of the friction pair was observed by a field emission scanning electron microscope.
SEM photographs of the friction pair surfaces of each group after the four-ball test are shown in fig. 1 to 6.
As can be seen from FIGS. 1-6, the additive products of examples 1-4 have better wear of the friction pair than the blank and comparative example 1, and especially example 3 has the best friction reducing and wear resisting effects.
Effect example 2
The tribological properties of each sample oil prepared in effect example 1 were measured using the same equipment as in effect example 1, with the test parameters: the load is 392N, the oil temperature is 75 ℃, the test time is 30min, and the rotating speed is 1200r/min. The results are shown in FIGS. 7-8.
As can be seen from fig. 7-8, the additive products of examples 1-4 exhibited better tribological performance than the blank and comparative example 1, and in particular example 3 exhibited the best tribological performance, with a 27.7% and 9.2% reduction in the average coefficient of friction and the scrub spot diameter, respectively, as compared to the blank control.
According to the invention, the lubricating oil additive is prepared by using the graphite-phase carbon nitride as a main raw material, the graphite-phase carbon nitride has a lamellar structure similar to graphene, and the graphite-phase carbon nitride can better generate electrostatic adsorption in a friction process, so that a thin protective oil film is easier to form, and the contact surface of a friction pair is smoother. Through further formula design and process adjustment, the modified graphite-phase carbon nitride is subjected to modification by adopting the long-chain alkyl acid, and the selection and use of the activating agents DMAP and DCC are matched, so that the lamellar spacing of the modified graphite-phase carbon nitride is enlarged, the interaction of Van der Waals force is hindered, the repair nano-materials with similar structures can be promoted to be uniformly dispersed, the existence of an agglomerated structure is reduced, meanwhile, the surface scratches can be effectively filled, the mechanical damage is reduced, and the friction-reducing and wear-resisting effects are jointly realized through the synergistic effect of the long-chain alkyl acid and the DCC.
In the actual operation, the solvent is selected according to the subsequent reaction temperature so that the boiling point of the solvent is as close as possible to the reaction temperature.
As a possible modification, the choice of solvent and reaction temperature can be made according to the following table.
| Solvent(s) | Boiling point of | Reaction temperature |
| Acetic acid ethyl ester | 77℃ | 90℃ |
| Deionized water | 100℃ | 80℃ |
| Toluene | 110.6℃ | 110℃ |
| Anhydrous ethanol | 78.4℃ | 80℃ |
| Isopropanol (I-propanol) | 82.5℃ | 80℃ |
Finally, it should be noted that: the above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (10)
1. A preparation method of a lubricating oil additive for a mechanical system is characterized by comprising the following steps:
(1) Weighing graphite-phase carbon nitride, adding a solvent, and performing ultrasonic dispersion to obtain a graphite-phase carbon nitride solution;
(2) Adding a modifier, DMAP (dimethyl formamide) and DCC (dimethyl dichloroisocyanurate) into the graphite-phase carbon nitride solution obtained in the step (1), stirring, and heating and refluxing in an inert atmosphere for reaction;
(3) After the reaction is finished, centrifuging to take out precipitate, washing with absolute ethyl alcohol and petroleum ether, and drying to obtain the product.
2. The production method according to claim 1, wherein the concentration of the graphite phase carbon nitride in the graphite phase carbon nitride solution is 0.005 to 0.05g/mL.
3. The method according to claim 1, wherein the solvent is any one of deionized water, ethyl acetate, absolute ethyl alcohol, toluene, and isopropyl alcohol.
4. The method of claim 1, wherein the modifier comprises any one of oleic acid, linoleic acid, stearic acid, and palmitic acid.
5. The method according to claim 4, wherein the mass ratio of the modifier, DMAP, DCC and graphite-phase carbon nitride added in step (2) is 30-40.
6. The method according to claim 1, wherein the heating reflux reaction in the step (2) is carried out at a temperature of 60 to 120 ℃ for a reaction time of 8 to 15 hours.
7. The method according to claim 1, wherein in the step (3), the rotation speed of the centrifugation is 6000 to 12000rpm, and the centrifugation time is 5 to 10min.
8. The method according to claim 1, wherein the drying method in the step (3) is any one of vacuum freeze drying, low-temperature vacuum drying, forced air drying and spray drying.
9. A lubricating oil additive for mechanical systems, prepared by the method of any one of claims 1 to 8.
10. Use of the lubricating oil additive of claim 9 in a 150BS base oil.
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