CN114672364B - Conductive lubricating grease and preparation method thereof - Google Patents

Conductive lubricating grease and preparation method thereof Download PDF

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Publication number
CN114672364B
CN114672364B CN202210384439.3A CN202210384439A CN114672364B CN 114672364 B CN114672364 B CN 114672364B CN 202210384439 A CN202210384439 A CN 202210384439A CN 114672364 B CN114672364 B CN 114672364B
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oil
lubricating grease
ionic liquid
grease
soluble ionic
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CN114672364A (en
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周峰
于强亮
蔡美荣
于波
张朝阳
张明
梁依经
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Yantai Advanced Materials And Green Manufacturing Shandong Laboratory
Lanzhou Institute of Chemical Physics LICP of CAS
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Yantai Advanced Materials And Green Manufacturing Shandong Laboratory
Lanzhou Institute of Chemical Physics LICP of CAS
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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
    • C10M169/00—Lubricating compositions characterised by containing as components a mixture of at least two types of ingredient selected from base-materials, thickeners or additives, covered by the preceding groups, each of these compounds being essential
    • C10M169/06—Mixtures of thickeners and additives
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C209/00—Preparation of compounds containing amino groups bound to a carbon skeleton
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C209/00—Preparation of compounds containing amino groups bound to a carbon skeleton
    • C07C209/04—Preparation of compounds containing amino groups bound to a carbon skeleton by substitution of functional groups by amino groups
    • C07C209/06—Preparation of compounds containing amino groups bound to a carbon skeleton by substitution of functional groups by amino groups by substitution of halogen atoms
    • C07C209/12—Preparation of compounds containing amino groups bound to a carbon skeleton by substitution of functional groups by amino groups by substitution of halogen atoms with formation of quaternary ammonium compounds
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C303/00—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides
    • C07C303/32—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides of salts of sulfonic acids
    • 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
    • C10M115/00—Lubricating compositions characterised by the thickener being a non-macromolecular organic compound other than a carboxylic acid or salt thereof
    • C10M115/08—Lubricating compositions characterised by the thickener being a non-macromolecular organic compound other than a carboxylic acid or salt thereof 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
    • C10M2205/00—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions
    • C10M2205/02—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions containing acyclic monomers
    • C10M2205/028—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions containing acyclic monomers containing aliphatic monomers having more than four carbon atoms
    • C10M2205/0285—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions containing acyclic monomers containing aliphatic monomers having more than four carbon atoms used as base material
    • 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
    • C10M2215/00—Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
    • C10M2215/10—Amides of carbonic or haloformic acids
    • C10M2215/102—Ureas; Semicarbazides; Allophanates
    • C10M2215/1026—Ureas; Semicarbazides; Allophanates used as thickening material
    • 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
    • C10M2219/00—Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions
    • C10M2219/04—Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions containing sulfur-to-oxygen bonds, i.e. sulfones, sulfoxides
    • C10M2219/044—Sulfonic acids, Derivatives thereof, e.g. neutral salts
    • 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
    • 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
    • C10N2040/00—Specified use or application for which the lubricating composition is intended
    • C10N2040/14—Electric or magnetic purposes
    • C10N2040/16—Dielectric; Insulating oil or insulators
    • 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
    • C10N2050/00—Form in which the lubricant is applied to the material being lubricated
    • C10N2050/10—Semi-solids; greasy

Abstract

The invention provides conductive lubricating grease and a preparation method thereof, and belongs to the technical field of lubricating grease materials. The conductive lubricating grease provided by the invention comprises the following components in percentage by mass: 1-30% of oil-soluble ionic liquid; 5 to 15 percent of thickening agent; the balance of basic lubricating oil; the preparation raw materials of the thickening agent comprise polyisocyanate compounds and amine compounds. According to the invention, the oil-soluble ionic liquid is used as a component of the conductive lubricating grease, on one hand, anions and cations in the oil-soluble ionic liquid can move directionally under the action of an electric field, so that the lubricating grease is endowed with good conductivity; on the other hand, the oil-soluble ionic liquid has excellent tribological characteristics, and can further improve the extreme pressure anti-wear performance of the lubricating grease. The conductive lubricating grease provided by the invention has good conductivity and antifriction and abrasion resistance, and can play a role in continuous lubrication and conductivity in electric contact equipment.

Description

Conductive lubricating grease and preparation method thereof
Technical Field
The invention relates to the technical field of lubricating grease materials, and particularly relates to conductive lubricating grease and a preparation method thereof.
Background
The rapid development of modern industry accelerates the consumption of energy too rapidly, and friction can lead to wear of mechanical equipment and additional consumption of energy. The use of greases is the most effective means of reducing friction and wear, and they are used in a wide range of applications, almost covering industrial, aerospace, electronic information and various military equipment. However, under some special operating conditions, for example: the wire bayonet of the equipment such as the power converter equipment, the pantograph and the ultrahigh voltage transmission line needs lubricating grease to have good lubricating performance and good conductive performance.
At present, some conductive powder materials (such as silver powder, zinc powder, copper powder, carbon powder and the like) are mostly used for improving the conductivity of the lubricating grease, but the conductive materials usually need to be added with 60-70% of metal powder to ensure the conductivity of the lubricating grease. However, the addition of a large amount of the above conductive powder material often reduces the friction-reducing and wear-resisting properties of the grease.
Disclosure of Invention
In view of the above, the present invention aims to provide a conductive grease and a preparation method thereof, and the conductive grease provided by the present invention has good conductivity and friction reduction and wear resistance.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a conductive lubricating grease which comprises the following components in percentage by mass:
1-30% of oil-soluble ionic liquid;
5 to 15 percent of thickening agent;
the balance of basic lubricating oil;
the preparation raw materials of the thickening agent comprise polyisocyanate compounds and amine compounds.
Preferably, the oil-soluble ionic liquid has a structure shown in formula I:
Figure BDA0003593067890000021
preferably, the preparation method of the oil-soluble ionic liquid with the structure shown in the formula I comprises the following steps:
carrying out a first substitution reaction on trioctylamine and bromohexadecane to obtain a compound with a structure shown in a formula a;
Figure BDA0003593067890000022
and (3) carrying out a second substitution reaction on the compound with the structure shown in the formula a and docusate sodium to obtain the oil-soluble ionic liquid with the structure shown in the formula I.
Preferably, the temperature of the first substitution reaction is 60-70 ℃ and the time is 8-48 h.
Preferably, the temperature of the second substitution reaction is 50-70 ℃ and the time is 8-48 h.
Preferably, the polyisocyanate compound is toluene diisocyanate and/or diphenylmethane-4, 4' -diisocyanate, and the amine compound is one or more of octadecylamine, hexadecylamine and dodecylamine.
Preferably, the base lubricant is one of PAO-10, base oil 500SN, and base oil 5750.
The invention provides a preparation method of the conductive grease, which comprises the following steps:
mixing basic lubricating oil, oil-soluble ionic liquid, polyisocyanate compounds and amine compounds, and performing saponification reaction to obtain a saponification reactant;
and heating and refining the saponified reactant to obtain the conductive lubricating grease.
Preferably, the temperature of the saponification reaction is 50-80 ℃, and the holding time is 30-90 min.
Preferably, the temperature for heating and refining is 170-190 ℃, and the heat preservation time is 10-30 min.
The invention provides conductive lubricating grease which comprises the following components in percentage by mass: 1-30% of oil-soluble ionic liquid; 5 to 15 percent of thickening agent; the balance of basic lubricating oil; the preparation raw materials of the thickening agent comprise polyisocyanate compounds and amine compounds. According to the invention, the oil-soluble ionic liquid is used as one of the components of the conductive grease, on one hand, anions and cations in the oil-soluble ionic liquid can move directionally under the action of an electric field, so that the grease has good conductivity; on the other hand, the oil-soluble ionic liquid has excellent tribological characteristics, and can further improve the extreme pressure anti-wear performance of the lubricating grease. The conductive lubricating grease provided by the invention has good conductivity and antifriction and abrasion resistance, can play a role in continuous lubrication and conductivity in electrical contact equipment, and is expected to play a role in long-acting lubrication and continuous conductivity at metal conductor joints of power plants, transformer substations, distribution substations and high-voltage transmission lines. The results of the examples show that when the conductive grease provided by the invention is used as a steel/steel friction pair lubricant, under the condition of 25 ℃ and no current carrying, the average friction coefficient is 0.113385-0.139842, and the average wear volume is (0.43272-0.79808). Times.10-3mm3(ii) a Under the condition of 100 ℃ and current carrying 1A, the average friction coefficient is 0.124869-0.146351, and the average abrasion volume is (0.94614-1.05464) × 10-3mm3。
The invention provides a preparation method of the conductive lubricating grease, which comprises the steps of mixing basic lubricating oil, oil-soluble ionic liquid, polyisocyanate compounds and amine compounds, carrying out saponification reaction to obtain saponification reactants, and then heating, refining and grinding the saponification reactants in sequence to obtain the conductive lubricating grease. The preparation method provided by the invention is simple to operate and is suitable for industrial batch production.
Detailed Description
The invention provides conductive lubricating grease which comprises the following components in percentage by mass:
1-30% of oil-soluble ionic liquid;
5 to 15 percent of thickening agent;
the balance of basic lubricating oil;
the preparation raw materials of the thickening agent comprise polyisocyanate compounds and amine compounds.
The conductive grease provided by the invention comprises 1-30% of oil-soluble ionic liquid by mass percentage, preferably 5-25%, more preferably 10-20%, and further preferably 15-18%. In the present invention, the oil-soluble ionic liquid preferably has a structure represented by formula I:
Figure BDA0003593067890000041
in the present invention, the preparation method of the oil-soluble ionic liquid having the structure represented by formula I preferably includes the following steps:
carrying out a first substitution reaction on trioctylamine and bromohexadecane to obtain a compound with a structure shown in a formula a;
Figure BDA0003593067890000042
and (3) carrying out a second substitution reaction on the compound with the structure shown in the formula a and docusate sodium to obtain the oil-soluble ionic liquid with the structure shown in the formula I.
In the invention, trioctylamine and bromohexadecane are subjected to a first substitution reaction to obtain a compound with a structure shown in a formula a. In the present invention, the molar ratio of trioctylamine to bromohexadecane is preferably 1 to 1.2, more preferably 1.
In the present invention, the first substitution reaction is preferably carried out in a polar organic solvent, which is preferably acetonitrile.
In the present invention, the temperature of the first substitution reaction is preferably 60 to 70 ℃, more preferably 65 ℃; the time is preferably 8 to 48 hours, more preferably 12 to 24 hours.
In the present invention, after the first substitution reaction, the organic solvent in the product of the first substitution reaction is preferably distilled off.
The invention carries out a second substitution reaction on the compound with the structure shown in the formula a and docusate sodium to obtain the oil-soluble ionic liquid with the structure shown in the formula I. In the present invention, the molar ratio of trioctylamine to docusate sodium is preferably 1.
In the present invention, the second substitution reaction is preferably carried out in a polar organic solvent, which is preferably ethanol.
In the present invention, the temperature of the second substitution reaction is preferably 50 to 70 ℃, more preferably 60 ℃; the time is preferably 8 to 48 hours, more preferably 12 to 24 hours.
After the second substitution reaction, the present invention preferably performs a post-treatment on the obtained second substitution reaction solution, and the post-treatment preferably includes:
and (3) sequentially washing, drying and removing the organic solvent from the second substitution reaction liquid to obtain the oil-soluble ionic liquid pure product with the structure shown in the formula I.
The invention has no special requirement on the water washing mode, and the water washing mode known to the technical personnel in the field can be used.
After said washing, the present invention preferably dries the resulting organic phase. In the present invention, the drying method is preferably drying with anhydrous sodium sulfate.
In the present invention, the organic solvent is preferably removed by rotary evaporation.
In the invention, the preparation process of the oil-soluble ionic liquid with the structure shown in the formula I is shown in the formula A.
Figure BDA0003593067890000051
The conductive grease provided by the invention comprises 5-15% of thickening agent by mass percentage, preferably 8-12%, and more preferably 10%. In the invention, the thickening agent is obtained by reacting a polyisocyanate compound and an amine compound. In the invention, the polyisocyanate compound is toluene diisocyanate and/or diphenylmethane-4, 4' -diisocyanate, and the amine compound is one or more of octadecylamine, hexadecylamine and dodecylamine.
In the present invention, the molar ratio of the polyisocyanate compound to the amine compound is preferably 1.
The conductive lubricating grease provided by the invention comprises the balance of base lubricating oil in percentage by mass. In the present invention, the base lubricant is preferably one of PAO-10, base oil 500SN, and base oil 5750. In the present invention, the source of the base lubricant is preferably commercially available.
The invention provides a preparation method of the conductive grease, which comprises the following steps:
mixing basic lubricating oil, oil-soluble ionic liquid, polyisocyanate compounds and amine compounds, and performing saponification reaction to obtain a saponification reactant;
and heating and refining the saponified reactant to obtain the conductive lubricating grease.
The invention mixes basic lubricating oil, oil-soluble ionic liquid, polyisocyanate compound and amine compound to carry out saponification reaction, thus obtaining saponification reactant.
In the present invention, the mixing is preferably performed in the following manner: firstly, preheating basic lubricating oil to obtain saponification reaction temperature, and adding oil-soluble ionic liquid, polyisocyanate compounds and amine compounds under the condition of stirring.
In the present invention, the saponification reaction temperature is preferably 50 to 80 ℃, more preferably 60 to 70 ℃; the time is preferably 30 to 90min, more preferably 40 to 80min. In the invention, in the saponification reaction process, the polyisocyanate compound and the amine compound are subjected to substitution reaction to obtain the carbamido thickening agent.
After the saponification reaction, the present invention preferably removes unreacted amine compounds by mixing the saponification reaction with water.
The invention heats and refines the saponification reactant to obtain the conductive grease. In the invention, the temperature for heating and refining is preferably 170-190 ℃, and more preferably 180 ℃; the time is preferably 10 to 30min, more preferably 15 to 25min. In the present invention, during the heating refining process, the viscosity of the grease system rapidly decreases, changing from a grease-like state to a viscous liquid.
After the conductive grease is obtained, the present invention preferably performs grinding. In the present invention, the grease obtained is preferably cooled to room temperature in the present invention before said grinding. In the present invention, the grinding is preferably a three-roll mill grinding.
The conductive grease and the preparation method thereof provided by the present invention will be described in detail with reference to the following examples, which should not be construed as limiting the scope of the present invention.
Example 1
Preparation of blank grease a:
weighing 85g of PAO10, placing the PAO10 in a 250ml beaker, preheating the PAO10 for 30 minutes at 80 ℃ under mechanical stirring, respectively weighing 3.66g of toluene diisocyanate, adding the toluene diisocyanate into the preheated PAO10 base oil while stirring, weighing 11.34g of octadecylamine, slowly dropwise adding the octadecylamine into the stirred PAO10 base oil, stopping heating in the dropwise adding process, controlling the dropwise adding time to be 30 minutes, generating a large amount of bubbles in the dropwise adding process to prove that saponification reaction occurs, gradually converting a reaction system from transparent oily matters into white greasy matters in the saponification process, and after the dropwise adding is finished, continuously stirring the mixture for 30 minutes at 80 ℃ to complete the saponification reaction. And then, heating the saponification system, controlling the reaction temperature to be 170-190 ℃, and carrying out high-temperature refining for half an hour, wherein the viscosity of the lubricating grease system is rapidly reduced in the refining process, and the lubricating grease system is converted into viscous liquid from grease. After the refining is finished and the lubricating grease system is completely cooled, the blank lubricating grease is ground for a plurality of times by using a three-roll mill, the process lasts for 20 minutes, and finally the blank lubricating grease A is obtained.
Example 2
Preparation of conductive grease B:
weighing 80g of PAO10, placing the PAO10 in a 250mL beaker, preheating the PAO10 for 30 minutes at 80 ℃ under mechanical stirring, weighing 5g of oil-soluble ionic liquid with a structure shown in formula I and 3.66g of toluene diisocyanate, adding the mixture into the PAO10 base oil preheated in advance while stirring, weighing 11.34g of octadecylamine, slowly dropwise adding the octadecylamine into the stirred PAO10 base oil, stopping heating in the dropwise adding process, controlling the dropwise adding time to be 30 minutes, generating a large amount of bubbles in the dropwise adding process to prove that saponification reaction occurs, gradually converting a reaction system from transparent oily matter into white greasy matter in the saponification process, and continuously stirring the mixture for 30 minutes at 80 ℃ after the dropwise adding is finished to ensure that the saponification reaction is completely performed. And then, heating the saponification system, controlling the reaction temperature to be 170-190 ℃, and carrying out high-temperature refining for half an hour, wherein the viscosity of the lubricating grease system is rapidly reduced in the refining process, and the lubricating grease system is converted into viscous liquid from grease. After the refining is finished and the lubricating grease system is completely cooled, the blank lubricating grease is ground for a plurality of times by using a three-roll mill, the process lasts for 20 minutes, and finally the conductive lubricating grease B is obtained.
Example 3
Preparation of conductive grease C:
weighing 75g of PAO10, placing the PAO10 in a 250mL beaker, preheating the PAO10 for 30 minutes at 80 ℃ under mechanical stirring, respectively weighing 10g of oil-soluble ionic liquid with a structure shown in formula I and 3.66g of toluene diisocyanate, adding the mixture into preheated PAO10 base oil while stirring, weighing 11.34g of octadecylamine, slowly dropwise adding the octadecylamine into the stirred PAO10 base oil, stopping heating in the dropwise adding process, controlling the dropwise adding time to be 30 minutes, generating a large amount of bubbles in the dropwise adding process to prove that saponification reaction occurs, gradually converting a reaction system from transparent oily matter into white greasy matter in the saponification process, and continuously stirring the mixture for 30 minutes at 80 ℃ after the dropwise adding is finished so as to complete the saponification reaction. And then, heating the saponification system, controlling the reaction temperature to be 170-190 ℃, and carrying out high-temperature refining for half an hour, wherein the viscosity of the lubricating grease system is rapidly reduced in the refining process, and the lubricating grease system is converted into viscous liquid from grease. After the refining is finished and the grease system is completely cooled, the blank grease is ground for a plurality of times by using a three-roll mill, and the process lasts for 20 minutes, so that the conductive grease C is finally obtained.
Example 4
Preparation of conductive grease D:
weighing 55g of PAO10, placing the PAO10 in a 250ml beaker, preheating the PAO10 for 30 minutes at 80 ℃ under mechanical stirring, respectively weighing 30g of oil-soluble ionic liquid with a structure shown in formula I and 3.66g of toluene diisocyanate, adding the mixture into preheated PAO10 base oil while stirring, weighing 11.34g of octadecylamine, slowly dropwise adding the octadecylamine into the stirred PAO10 base oil, stopping heating in the dropwise adding process, controlling the dropwise adding time to be 30 minutes, generating a large amount of bubbles in the dropwise adding process to prove that saponification reaction occurs, gradually converting a reaction system from transparent oily matter into white greasy matter in the saponification process, and continuously stirring the mixture for 30 minutes at 80 ℃ after the dropwise adding is finished so as to complete the saponification reaction. And then, heating the saponification system, controlling the reaction temperature to be 170-190 ℃, and carrying out high-temperature refining for half an hour, wherein the viscosity of the lubricating grease system is rapidly reduced in the refining process, and the lubricating grease system is converted into viscous liquid from grease. After the refining is finished and the lubricating grease system is completely cooled, the blank lubricating grease is ground for a plurality of times by using a three-roll mill, the process lasts for 20 minutes, and finally the conductive lubricating grease D is obtained.
Comparative example 1
As comparative example 1, a commercially available conductive grease containing copper powder was used, the copper powder content being 70 wt%.
Comparative example 2
As comparative example 2, domestic power-rich electric composite grease DLZ-1G was used.
Performance testing
(1) The tribological properties of the greases of the examples and comparative examples were tested using an Optimol-SRV-IV type Friction wear tester under a load of 200N,25 ℃ and under a no-load condition. The friction pair contact mode of the Optimol-SRV-IV type friction wear testing machine is ball-disc point contact, the frequency is 25Hz, the amplitude is 1mm, the testing time is 30min, an upper test ball is a GCr15 (SAE 52100) steel ball with the diameter of 10 mm, and a lower test disc is a steel disc. The test results are shown in table 1.
TABLE 1 average coefficient of friction and average wear volume at 25 ℃ for example and comparative greases as a steel/steel friction secondary lubricant
Figure BDA0003593067890000081
Figure BDA0003593067890000091
As can be seen from table 1, the three conductive greases described herein all have superior lubricating properties than the blank grease under no current carrying conditions. The experimental result shows that compared with the blank lubricating grease, the antifriction and antiwear performances of the conductive lubricating grease are greatly improved.
(2) The tribology performance of the lubricating grease of the examples and the comparative example under the condition of the load of 200N,100 ℃ and the current carrying (1A) is tested by serially connecting a regulated power supply with an Optimol-SRV-IV type friction wear tester. The friction pair contact mode of the Optimol-SRV-IV type friction wear testing machine is ball-disc point contact, the frequency is 25Hz, the amplitude is 1mm, the testing time is 30min, an upper test ball is a GCr15 (SAE 52100) steel ball with the diameter of 10 mm, and a lower test disc is a steel disc. The results obtained are shown in Table 2.
TABLE 2 average coefficient of friction and average wear volume at 100 ℃ for example and comparative greases as a steel/steel friction secondary lubricant
Figure BDA0003593067890000092
As can be seen from table 2, the three conductive greases described herein all have superior lubricating properties under current carrying conditions compared to the blank grease. The experimental result shows that compared with the blank lubricating grease, the antifriction and antiwear performance of the conductive lubricating grease is also greatly improved under the current-carrying condition.
(3) Dropping Point, penetration of example and comparative greases
The greases of the examples and comparative examples were tested for dropping point and penetration, with test standards GB/T4929-85 and GB/T269-91, and the results are shown in Table 3.
TABLE 3 dropping Point, penetration of example and comparative greases
Figure BDA0003593067890000093
Figure BDA0003593067890000101
As can be seen from table 3, with the addition of the oil-soluble ionic liquid, the data of the dropping point and the penetration of the conductive grease is almost unchanged compared with the blank grease, so that it can be proved that with the addition of the oil-soluble ionic liquid, the structure and the physical and chemical properties of the grease are not greatly affected.
(4) Maximum seizure-free load Pb and sintering load Pd for example and comparative greases
An MS-10A four-ball friction wear testing machine produced by Xiamen skyscraper automation company is utilized to measure the extreme pressure performance of the lubricating grease (four-ball method) according to the national standard SH/T0202-92; SH/T0204-92, a method for measuring the antiwear performance of lubricating grease (four-ball method) tests the extreme pressure bearing capacity of lubricating grease of examples and comparative examples. The results obtained are shown in Table 4.
TABLE 4 PB and PD of the example and comparative greases
Figure BDA0003593067890000102
As can be seen from table 4, the extreme pressure load-carrying properties of the conductive grease were significantly improved as compared with the blank grease and the comparative example.
(5) The conductivity properties of the greases of examples and comparative examples were measured using an FT-304 series resistivity tester from Ningbor instruments, inc. and the results are shown in Table 5.
TABLE 5 conductivity of the greases of the examples and comparative examples
Figure BDA0003593067890000103
Figure BDA0003593067890000111
It can be seen from table 5 that, when the oil-soluble ionic liquid is added, the tribological performance of the blank grease is improved, and the conductivity of the blank grease is greatly improved, and when the addition amount is 5%, the conductivity of the blank grease is reduced by 4 orders of magnitude compared with that of the blank grease, and when the addition amount is increased to 30%, the conductivity of the blank grease is reduced by 6 orders of magnitude compared with that of the blank grease.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.

Claims (9)

1. The conductive lubricating grease comprises the following components in percentage by mass:
20-30% of oil-soluble ionic liquid;
5 to 15 percent of thickening agent;
the balance of basic lubricating oil;
the preparation raw materials of the thickening agent comprise polyisocyanate compounds and amine compounds;
the oil-soluble ionic liquid has a structure shown in formula I:
Figure FDA0003858423200000011
2. the conductive grease of claim 1, wherein the preparation method of the oil-soluble ionic liquid having the structure shown in formula I comprises the following steps:
carrying out a first substitution reaction on trioctylamine and bromohexadecane to obtain a compound with a structure shown in a formula a;
Figure FDA0003858423200000012
and (3) carrying out a second substitution reaction on the compound with the structure shown in the formula a and docusate sodium to obtain the oil-soluble ionic liquid with the structure shown in the formula I.
3. The conductive grease of claim 2, wherein the temperature of the first substitution reaction is 60 to 70 ℃ and the time is 8 to 48 hours.
4. The conductive grease of claim 2, wherein the temperature of the second substitution reaction is 50-70 ℃ and the time is 8-48 h.
5. The conductive grease of claim 1 wherein the polyisocyanate compound is toluene diisocyanate and/or diphenylmethane-4, 4' -diisocyanate and the amine compound is one or more of octadecylamine, hexadecylamine, and dodecylamine.
6. The electrically conductive grease of claim 1 wherein the base lubricant is one of PAO-10, base oil 500SN, and base oil 5750.
7. The process for preparing the conductive grease of any one of claims 1 to 6, comprising the steps of:
mixing basic lubricating oil, oil-soluble ionic liquid, polyisocyanate compounds and amine compounds, and performing saponification reaction to obtain a saponification reactant;
and heating and refining the saponification reactant to obtain the conductive grease.
8. The method according to claim 7, wherein the saponification reaction is carried out at a temperature of 50 to 80 ℃ for a holding time of 30 to 90min.
9. The preparation method according to claim 7, wherein the temperature for heating and refining is 170-190 ℃, and the holding time is 10-30 min.
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CA2495384A1 (en) * 2002-08-16 2004-02-26 Sachem, Inc. Ionic liquids containing a sulfonate anion
JP2007191523A (en) * 2006-01-17 2007-08-02 Nsk Ltd Grease composition
EP1970432A1 (en) * 2006-12-19 2008-09-17 Castrol Limited Lubricating oil compositions and uses
CN102337171A (en) * 2010-07-22 2012-02-01 中国科学院兰州化学物理研究所 Ionic liquid polyurea grease composition
CN105273799B (en) * 2015-12-02 2018-06-05 国家电网公司 A kind of electric force compounded grease and preparation method thereof
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