CN111423916A - CTAB modified nano molybdenum disulfide, preparation method and application thereof, lithium-based lubricating grease and preparation method thereof - Google Patents

CTAB modified nano molybdenum disulfide, preparation method and application thereof, lithium-based lubricating grease and preparation method thereof Download PDF

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CN111423916A
CN111423916A CN202010338176.3A CN202010338176A CN111423916A CN 111423916 A CN111423916 A CN 111423916A CN 202010338176 A CN202010338176 A CN 202010338176A CN 111423916 A CN111423916 A CN 111423916A
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molybdenum disulfide
ctab
nano molybdenum
lubricating grease
lithium
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熊胜锋
储修祥
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Zhejiang A&F University ZAFU
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Zhejiang A&F University ZAFU
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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
    • C10M141/00—Lubricating compositions characterised by the additive being a mixture of two or more compounds covered by more than one of the main groups C10M125/00 - C10M139/00, each of these compounds being essential
    • C10M141/06—Lubricating compositions characterised by the additive being a mixture of two or more compounds covered by more than one of the main groups C10M125/00 - C10M139/00, each of these compounds being essential at least one of them being an organic nitrogen-containing compound
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G39/00—Compounds of molybdenum
    • C01G39/06—Sulfides
    • 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
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/06—Metal compounds
    • C10M2201/065—Sulfides; Selenides; Tellurides
    • C10M2201/066—Molybdenum sulfide
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/14—Inorganic compounds or elements as ingredients in lubricant compositions inorganic compounds surface treated with organic compounds
    • 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
    • C10M2203/00—Organic non-macromolecular hydrocarbon compounds and hydrocarbon fractions as ingredients in lubricant compositions
    • C10M2203/10—Petroleum or coal fractions, e.g. tars, solvents, bitumen
    • C10M2203/102—Aliphatic fractions
    • C10M2203/1025—Aliphatic fractions 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
    • C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/10—Carboxylix acids; Neutral salts thereof
    • C10M2207/12—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms
    • C10M2207/125—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids
    • C10M2207/128—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids containing hydroxy groups; Ethers thereof
    • C10M2207/1285—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids containing hydroxy groups; Ethers thereof used as thickening agents
    • 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
    • C10M2215/02—Amines, e.g. polyalkylene polyamines; Quaternary amines
    • C10M2215/04—Amines, e.g. polyalkylene polyamines; Quaternary amines having amino groups bound to acyclic or cycloaliphatic carbon atoms

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Abstract

The invention provides CTAB modified nano molybdenum disulfide, a preparation method and application thereof, lithium-based lubricating grease and a preparation method thereof, and belongs to the technical field of lubricating grease. The invention takes CTAB (cetyl trimethyl ammonium bromide) as a surface modifier to modify nano molybdenum disulfide, a CTAB molecular layer is formed on the surface of the nano molybdenum disulfide, and the polar end of the CTAB molecular layer and nano MoS2Combined while the non-polar end canThe lubricating grease is stably dispersed in the lubricating grease in a similar and compatible manner with the oil phase, so that the lubricating grease can be more stably kept in a dispersed state, the surface energy of the nano molybdenum disulfide is reduced, and the comprehensive performance of the lubricating grease is effectively improved.

Description

CTAB modified nano molybdenum disulfide, preparation method and application thereof, lithium-based lubricating grease and preparation method thereof
Technical Field
The invention relates to the technical field of lubricating grease, and particularly relates to CTAB modified nano molybdenum disulfide, a preparation method and application thereof, lithium-based lubricating grease and a preparation method thereof.
Background
Molybdenum disulfide (MOS)2) The graphene-like composite material is a typical layered hexagonal metal compound, has a unique sandwich structure and typical graphene-like two-dimensional material characteristics, and has good lubricating, catalytic and electrochemical properties. MoS2The extreme pressure antiwear additive as lubricating grease is widely applied, and the nano MOS2Also has been widely studied for anti-wear extreme pressure properties. But nanoscale MOS2The lubricating grease has small volume, large specific surface area and high specific surface energy, and is easy to agglomerate to form larger particles, thereby influencing the service performance of the lubricating grease.
The prior art generally carries out surface modification on nano molybdenum disulfide to improve the dispersibility of the nano molybdenum disulfide in lubricating grease, such as modifying the nano molybdenum disulfide by using laurylamidopropyl amine oxide. However, the existing surface modification technology can only improve the dispersion stability of the nano molybdenum disulfide, and cannot further improve other properties of the lubricating grease.
Disclosure of Invention
The invention aims to provide CTAB modified nano molybdenum disulfide, a preparation method and application thereof, and lithium-based lubricating grease and a preparation method thereof.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a preparation method of CTAB modified nano molybdenum disulfide, which comprises the following steps:
mixing nano molybdenum disulfide, CTAB and ethanol to obtain a raw material mixed solution;
and carrying out reflux reaction on the raw material mixed solution for 22-26 h, and then standing for reaction for 22-26 h to obtain the CTAB modified nano molybdenum disulfide.
Preferably, the mass ratio of the nano molybdenum disulfide to CTAB is 1 (3-5).
Preferably, the temperature of the reflux reaction is 75-85 ℃, and the standing reaction is carried out at room temperature.
Preferably, after the standing reaction is completed, the method further comprises post-treatment, wherein the post-treatment comprises the following steps: carrying out solid-liquid separation on the reaction liquid obtained by the standing reaction to obtain a solid; the solid was hot washed with alternating petroleum ether and ethanol and then dried.
The invention also provides the CTAB modified nano molybdenum disulfide obtained by the preparation method in the technical scheme.
The invention also provides application of the CTAB modified nano molybdenum disulfide as a lubricating grease additive.
The lithium-based lubricating grease comprises the following main raw materials in parts by mass: 90-100 parts of dodecahydroxy stearic acid, 750-900 parts of base oil, 13-17 parts of lithium hydroxide and 15-22 parts of lubricating grease additive, wherein the lubricating grease additive is the CTAB modified nano molybdenum disulfide in the technical scheme.
The invention also provides a preparation method of the lithium-based lubricating grease, which comprises the following steps:
dissolving dodecahydroxy stearic acid in part of base oil to obtain a base oil solution of dodecahydroxy stearic acid;
dissolving lithium hydroxide in water to obtain a lithium hydroxide aqueous solution;
mixing the base oil solution of the dodecahydroxy stearic acid with a lithium hydroxide aqueous solution, and performing saponification reaction to obtain thickened lubricating oil;
sequentially dehydrating and refining the thickened lubricating oil to obtain anhydrous thickened lubricating oil;
and mixing the anhydrous thickened lubricating oil with the rest base oil and the lubricating grease additive, and then grinding to obtain the lithium-based lubricating grease.
Preferably, the part of the base oil accounts for 2/3 of the total amount of the base oil, and the saponification reaction is carried out at the temperature of 90-125 ℃ for 0.8-1.2 h.
Preferably, the dehydration temperature is 140-160 ℃, and the time is 15-30 min; the refining temperature is 190-210 ℃, and the refining time is 9-12 min.
The invention provides a preparation method of CTAB modified nano molybdenum disulfide, which comprises the following steps: mixing nano molybdenum disulfide, CTAB and ethanol to obtain a raw material mixed solution; and carrying out reflux reaction on the raw material mixed solution for 22-26 h, and then standing for reaction for 22-26 h to obtain the CTAB modified nano molybdenum disulfide. The invention takes CTAB (cetyl trimethyl ammonium bromide) as a surface modifier to modify nano molybdenum disulfide, a CTAB molecular layer is formed on the surface of the nano molybdenum disulfide, and the polar end of the CTAB molecular layer and nano MoS2And the nonpolar end can be stably dispersed in the lubricating grease in a similar and compatible manner with the oil phase, so that the nonpolar end can be more stably kept in a dispersed state in the lubricating grease, the surface energy of the nano molybdenum disulfide is reduced, and the comprehensive performance of the lubricating grease is effectively improved.
Drawings
FIG. 1 is an SEM image of CTAB modified nano molybdenum disulfide obtained in example 1;
FIG. 2 is an infrared spectrum of the lithium-based grease obtained in comparative example 2;
FIG. 3 is an infrared spectrum of the lithium-based grease obtained in comparative example 1;
FIG. 4 is an infrared spectrum of the lithium grease obtained in example 1.
Detailed Description
The invention provides a preparation method of CTAB modified nano molybdenum disulfide, which comprises the following steps:
mixing nano molybdenum disulfide, CTAB and ethanol to obtain a raw material mixed solution;
and carrying out reflux reaction on the raw material mixed solution for 22-26 h, and then standing for reaction for 22-26 h to obtain the CTAB modified nano molybdenum disulfide.
The method mixes the nano molybdenum disulfide, CTAB and ethanol to obtain a raw material mixed solution.
The specification of the nano molybdenum disulfide is not particularly limited, commercially available nano molybdenum disulfide can be adopted, and in the embodiment of the invention, the average sheet diameter of the nano molybdenum disulfide is preferably 500nm, and the thickness of the nano molybdenum disulfide is preferably 80 nm.
In the invention, the mass ratio of the nano molybdenum disulfide to CTAB is preferably 1 (3-5), and more preferably 1: 5.
In the invention, the ethanol is preferably absolute ethanol, the dosage of the ethanol is not particularly limited, and the conventional solvent dosage is adopted, and in the embodiment of the invention, the dosage ratio of the molybdenum disulfide to the ethanol is preferably 1g (40-50) m L, and more preferably 1g:45m L.
The invention has no special limitation on the mixing sequence of the nano molybdenum disulfide, CTAB and ethanol, and can obtain the raw material mixed solution which is uniformly mixed. In an embodiment of the present invention, the mixing preferably comprises the steps of:
dispersing nano molybdenum disulfide in partial ethanol to obtain nano molybdenum disulfide dispersion liquid;
dissolving CTAB in the residual ethanol to obtain CTAB solution;
mixing the CTAB solution with the nano molybdenum disulfide dispersion.
The invention has no special limit on the amount of the partial ethanol, can ensure that the nano molybdenum disulfide is uniformly dispersed, and the CTAB can be completely dissolved in the residual ethanol.
In the embodiment of the invention, the mixing process of the CTAB solution and the nano molybdenum disulfide dispersion liquid is preferably carried out by heating the nano molybdenum disulfide dispersion liquid to the temperature of reflux reaction and then adding the CTAB solution, wherein the adding rate of the CTAB solution is preferably 8-12 m L/min, and more preferably 10m L/min.
After the raw material mixed solution is obtained, the raw material mixed solution is subjected to reflux reaction for 22-26 hours, and then is subjected to standing reaction for 22-26 hours to obtain the CTAB modified nano molybdenum disulfide.
In the invention, the temperature of the reflux reaction is preferably 75-85 ℃, more preferably 80 ℃, and the time is preferably 24 h; in the reflux reaction process, stirring is preferably maintained, and the rotating speed of the stirring is preferably 60-75 rpm, more preferably 70 rpm; the standing reaction is preferably carried out at room temperature (i.e., without additional heating or cooling), and the time for the standing reaction is preferably 24 hours.
In the present invention, after the standing reaction is completed, the method preferably further comprises a post-treatment, and the post-treatment preferably comprises the following steps: carrying out solid-liquid separation on the reaction liquid obtained by the standing reaction to obtain a solid; the solid was hot washed with alternating petroleum ether and ethanol and then dried. The solid-liquid separation mode is not particularly limited, and a conventional solid-liquid separation mode, such as filtration, is adopted; the temperature of the petroleum ether used for hot washing is preferably 40-50 ℃, more preferably 45 ℃, and the temperature of the ethanol used for hot washing is preferably 65-70 ℃, more preferably 70 ℃; the number of times of hot washing is not particularly limited, and CTAB can be removed, and in the embodiment of the invention, the number of times of alternately hot washing by petroleum ether and ethanol is preferably 3-5 times. The drying mode and parameters are not particularly limited in the invention, and a constant weight product can be obtained, in the embodiment of the invention, the drying is preferably vacuum drying, and the drying temperature is preferably 80 ℃.
The invention also provides the CTAB modified nano molybdenum disulfide obtained by the preparation method in the technical scheme.
The invention also provides the application of the CTAB modified nano molybdenum disulfide as a lubricating grease additive in the technical scheme; the grease additive is preferably a lithium-based grease additive.
The invention provides lithium-based lubricating grease which comprises the following main raw materials in parts by mass: 90-100 parts of dodecahydroxy stearic acid, 750-900 parts of base oil, 13-17 parts of lithium hydroxide and 15-22 parts of lubricating grease additive, wherein the lubricating grease additive is the CTAB modified nano molybdenum disulfide in the technical scheme. The raw material of the lithium-based lubricating grease provided by the invention also comprises water for dissolving lithium hydroxide, and the amount of the water is not particularly limited in the invention and can be removed in the preparation process.
In the present invention, the lithium-based grease preferably comprises the following main raw materials in parts by mass: 100 parts of dodecahydroxy stearic acid, 865 parts of base oil, 15 parts of lithium hydroxide and 20 parts of a lubricating grease additive.
The type of the base oil is not particularly limited, in the embodiment of the invention, the base is preferably 500N base oil, and the kinematic viscosity of the 500N base oil at 40 ℃ is preferably 95-100 mm2S, more preferably 98.0mm2/s。
The invention also provides a preparation method of the lithium-based lubricating grease, which comprises the following steps:
dissolving dodecahydroxy stearic acid in part of base oil to obtain a base oil solution of dodecahydroxy stearic acid;
dissolving lithium hydroxide in water to obtain a lithium hydroxide aqueous solution;
mixing the base oil solution of the dodecahydroxy stearic acid with a lithium hydroxide aqueous solution, and performing saponification reaction to obtain thickened lubricating oil;
sequentially dehydrating and refining the thickened lubricating oil to obtain anhydrous thickened lubricating oil;
and mixing the anhydrous thickened lubricating oil with the rest base oil and the lubricating grease additive, and then grinding to obtain the lithium-based lubricating grease.
The invention dissolves the dodecahydroxy stearic acid in part of base oil to obtain the base oil solution of the dodecahydroxy stearic acid.
In the present invention, the portion of the base oil is preferably 2/3 based on the total amount of base oil.
In the present invention, the above-mentioned dissolving method is not particularly limited, and it is sufficient if the dodecahydroxystearic acid is completely dissolved, and in the present embodiment, it is preferable to mix the dodecahydroxystearic acid and a part of the base oil and heat the mixture to a saponification reaction temperature so that the dodecahydroxystearic acid is completely dissolved and prepare for the saponification reaction.
The invention dissolves lithium hydroxide in water to obtain the lithium hydroxide aqueous solution.
In the present invention, the lithium hydroxide is dissolved in water without any particular limitation, and the lithium hydroxide may be dissolved, and in the embodiment of the present invention, the lithium hydroxide is preferably dissolved by heating at a temperature of preferably 75 to 85 ℃, more preferably 80 ℃, and the concentration of the lithium hydroxide aqueous solution is preferably 12 to 13g/100m L, more preferably 12.8g/100m L.
The order of preparation of the base oil solution of dodecahydroxystearic acid and the aqueous solution of lithium hydroxide is not particularly limited.
After the base oil solution of the dodecahydroxystearic acid and the lithium hydroxide aqueous solution are obtained, the base oil solution of the dodecahydroxystearic acid and the lithium hydroxide aqueous solution are mixed for saponification reaction to obtain the thickened lubricating oil.
In the present invention, after the base oil solution of dodecahydroxystearic acid and the aqueous solution of lithium hydroxide are mixed, the dodecahydroxystearic acid and the lithium hydroxide are saponified to generate lithium dodecahydroxystearate, a large amount of heat is generated, and water is boiled to generate a large amount of foam, so that it is preferable to maintain stirring at a rotation speed of 80 to 110rpm, more preferably 110rpm, during the saponification reaction to reduce the foam.
In the present invention, the order of mixing the base oil solution of dodecahydroxystearic acid and the aqueous solution of lithium hydroxide is preferably such that the aqueous solution of lithium hydroxide is slowly added to the base oil solution of dodecahydroxystearic acid, to the extent that no boiling phenomenon occurs.
In the invention, the temperature of the saponification reaction is preferably 90-125 ℃, more preferably 115 ℃, and the time of the saponification reaction is preferably based on the alkali of the reaction liquid of the saponification reaction; in the embodiment of the invention, preferably, when the time of the saponification reaction is 1h, the acid-base degree of the reaction solution is detected, the saponification reaction is completed when the reaction solution is detected to be alkalescent, namely, the pH value is 8-10, the next step is carried out, if the reaction solution is detected to be acidic, the saponification reaction is continued, and a proper amount of sodium hydroxide solution can be added dropwise.
The temperature and time for dehydration are not particularly limited, and water can be removed, in the embodiment of the invention, the temperature for dehydration is preferably 140-160 ℃, more preferably 150 ℃, and the time is preferably 15-30 min, more preferably 30 min.
In the invention, the refining temperature is preferably 190-210 ℃, more preferably 200 ℃, and the time is preferably 9-12 min, more preferably 10 min. In the present invention, the refining enables better blending of the base oil with lithium dodecahydroxystearate, resulting in the formation of stable soap fibers.
After the anhydrous thickened lubricating oil is obtained, the anhydrous thickened lubricating oil is mixed with the rest base oil and the lubricating grease additive, and then the mixture is ground to obtain the lithium-based lubricating grease.
In the invention, after the anhydrous thickened lubricating oil is mixed with the rest base oil and the lubricating grease additive, the temperature is preferably reduced to 57-63 ℃, more preferably to 60 ℃, and then grinding is carried out, wherein the grinding at the preferred temperature can better fuse the rest base oil and the lubricating grease additive in a soap fiber framework; the cooling rate is not particularly limited, and a person skilled in the art can control the cooling rate according to needs, for example, when short soap fibers and lubricating grease with a large cone penetration are required to be obtained, rapid cooling is preferably adopted, and the cooling rate is preferably 10-15 ℃/min, and more preferably 10 ℃/min; the grinding equipment is preferably a three-roll mill, and the grinding parameters comprise: the rough roll milling gap is preferably 0.09-0.39 mm, more preferably 0.09mm, and the fine roll milling gap is preferably 0.05-0.09 mm, more preferably 0.05mm, and the milling can obtain uniform and smooth grease.
The CTAB modified nano molybdenum disulfide, the preparation method and the application thereof, the lithium grease and the preparation method thereof provided by the present invention are described in detail below with reference to the examples, but they should not be construed as limiting the scope of the present invention.
Example 1
Dissolving 100g of CTAB in 500m L anhydrous ethanol to obtain a CTAB solution;
mixing 20g of nano molybdenum disulfide (average sheet diameter is 500nm and average thickness is 80nm) with 400m L absolute ethyl alcohol, heating to 80 ℃, slowly adding 500m L CTAB solution at the rate of 10m L/min, stirring and refluxing for 24h at the rotating speed of 70rpm, standing for 24h at room temperature, carrying out suction filtration, alternately washing the solid obtained by suction filtration with 45 ℃ petroleum ether and 70 ℃ ethanol for 4 times, and carrying out vacuum drying at 80 ℃ to constant weight to obtain CTAB modified nano molybdenum disulfide;
576.7g of 500N base oil (kinematic viscosity at 40 ℃ 98.0 mm)2The method comprises the steps of/s) mixing with 100g of dodecahydroxystearic acid, stirring and heating to 115 ℃, dissolving the dodecahydroxystearic acid to obtain a base oil solution of the dodecahydroxystearic acid, mixing 15g of lithium hydroxide with 150m L of water, stirring in a water bath kettle at 80 ℃ until the lithium hydroxide is completely dissolved to obtain a lithium hydroxide aqueous solution, slowly adding the lithium hydroxide aqueous solution into the base oil solution of the dodecahydroxystearic acid at the temperature of 115 ℃, stirring and reacting for 1 hour at the rotation speed of 110rpm, detecting the pH value of a reaction solution to obtain weak alkalinity (the pH value is 8-10), heating to 150 ℃, dehydrating for 30min, heating to 200 ℃, refining at constant temperature for 10min to obtain anhydrous thickened lubricating oil, mixing the anhydrous thickened lubricating oil with 288.3g of 500N base oil and 20g of CTAB modified nano molybdenum disulfide, stirring uniformly, rapidly cooling to 60 ℃ at the cooling rate of 10 ℃/min, placing in a three-roll mill to obtain the lithium-based lubricating grease with the gap of 0.09mm for coarse roll and the gap of 0.05mm for fine roll.
Example 2
Dissolving 45g CTAB in 225m L anhydrous ethanol to obtain CTAB solution;
mixing 15g of nano molybdenum disulfide (average sheet diameter is 500nm and average thickness is 80nm) with 350m L absolute ethyl alcohol, heating to 80 ℃, slowly adding 225m L CTAB solution at the rate of 10m L/min, stirring and refluxing for 24h at the rotating speed of 70rpm, standing for 24h at room temperature, carrying out suction filtration, alternately washing the solid obtained by suction filtration with 45 ℃ petroleum ether and 70 ℃ ethanol for 4 times, and carrying out vacuum drying at 80 ℃ to constant weight to obtain CTAB modified nano molybdenum disulfide;
587g of 500N base oil (kinematic viscosity at 40 ℃ 98.0 mm)2/s) with 90g of dodecahydroxystearic acid, stirring and heating to 115 ℃, and dissolving the dodecahydroxystearic acid to obtain a base oil solution of dodecahydroxystearic acidThe preparation method comprises the steps of mixing 14g of lithium hydroxide and 140m of L water, stirring the mixture in a water bath kettle at 80 ℃ until the lithium hydroxide is completely dissolved to obtain a lithium hydroxide aqueous solution, slowly adding the lithium hydroxide aqueous solution into a base oil solution of dodecahydroxystearic acid at 115 ℃, stirring the mixture at a rotation speed of 110rpm for reaction for 1 hour, detecting the pH value of the reaction solution to obtain a weak alkaline condition (the pH value is 8-10), heating the mixture to 150 ℃ for dehydration for 30 minutes, heating the mixture to 200 ℃, refining the mixture at a constant temperature for 10 minutes to obtain anhydrous lubricating oil, mixing the anhydrous thickened lubricating oil with 294g of 500N base oil and 15g of CTAB modified nano molybdenum disulfide, stirring the mixture uniformly, rapidly cooling the mixture to 60 ℃ at a cooling rate of 10 ℃/min, placing the mixture in a three-roll mill, and grinding the mixture under the conditions that the gap between a rough roll mill is 0.09mm and the gap between a fine roll mill is 0.05mm to obtain the lithium-based.
Example 3
Dissolving 80g CTAB in 400m L anhydrous ethanol to obtain CTAB solution;
mixing 20g of nano molybdenum disulfide (average sheet diameter is 500nm and average thickness is 80nm) with 400m L absolute ethyl alcohol, heating to 80 ℃, slowly adding 400m L CTAB solution at the rate of 10m L/min, stirring and refluxing for 24h at the rotating speed of 70rpm, standing for 24h at room temperature, carrying out suction filtration, alternately washing the solid obtained by suction filtration with 45 ℃ petroleum ether and 70 ℃ ethanol for 4 times, and carrying out vacuum drying at 80 ℃ to constant weight to obtain CTAB modified nano molybdenum disulfide;
580g of 500N base oil (kinematic viscosity at 40 ℃ C. of 98.0 mm)2/s) mixing with 95g of dodecahydroxystearic acid, stirring and heating to 115 ℃, dissolving the dodecahydroxystearic acid to obtain a base oil solution of the dodecahydroxystearic acid, mixing 14g of lithium hydroxide with 140m L of water, stirring in a water bath kettle at 80 ℃ until the lithium hydroxide is completely dissolved to obtain a lithium hydroxide aqueous solution, slowly adding the lithium hydroxide aqueous solution into the base oil solution of the dodecahydroxystearic acid at the temperature of 115 ℃, stirring and reacting for 1 hour under the rotation speed of 110rpm, detecting the pH value of a reaction solution to obtain a weak alkaline pH value (8-10), heating to 150 ℃, dehydrating for 30min, heating to 200 ℃, refining at a constant temperature for 10min to obtain anhydrous thickened lubricating oil, mixing the anhydrous thickened lubricating oil with 291g of 500N base oil and 20g of CTAB modified nano molybdenum disulfideMixing, stirring uniformly, rapidly cooling to 60 ℃ at a cooling rate of 10 ℃/min, and then placing in a three-roller machine for grinding under the conditions that the coarse roller grinding gap is 0.09mm and the fine roller grinding gap is 0.05mm to obtain the lithium-based lubricating grease.
Comparative example 1
The lithium grease was prepared according to the method of example 1, except that the nano molybdenum disulfide was used as the grease additive without modifying the nano molybdenum disulfide, and the other parameters were the same as those of example 1.
Comparative example 2
A lithium grease was prepared as in example 1, except that CTAB-modified nano molybdenum disulfide was not added, and the other parameters were the same as in example 1.
The SEM image of the CTAB modified nano molybdenum disulfide obtained in example 1 is shown in fig. 1, and as can be seen from fig. 1, the gray flake part is nano molybdenum disulfide, the flocculent CTAB bonded to the flake surface, the CTAB molecular structure is tightly adhered to the nano molybdenum disulfide flake layer, and the nonpolar carbon chain forms a non-smooth and flat external structure. From the analysis, CTAB is uniformly covered on the surface of the nano molybdenum disulfide after being treated, the steric hindrance generated by the nonpolar group of the CTAB slows down the tendency of mutual attraction and agglomeration of the nano molybdenum disulfide, and meanwhile, the CTAB interacts with lithium soap, so that the nano molybdenum disulfide can be kept stable in a lubricating grease system, and the dispersion stability of the lubricating grease is improved.
The infrared spectra of the lithium-based greases obtained in example 1 and comparative examples 1 to 2 were measured, and the results are shown in FIGS. 2 to 4. FIG. 2 shows the infrared characteristic peak of the mineral oil of the lithium-based grease obtained in comparative example 2, i.e., the lithium-based grease without additive, at 1337cm-1At 1559cm-1The characteristic peak of (A) is the asymmetric absorption peak of O-L i of lithium fatty acid, and is located at 1455cm-1FIG. 3 shows the symmetric absorption peak of O-L i of lithium fatty acid, and FIG. 3 shows the characteristic peak of MO-O of nano-molybdenum disulfide as additive at 532cm for the lithium grease obtained in comparative example 1, i.e. the lithium grease using nano-molybdenum disulfide as additive-1(ii) a FIG. 4 shows the lithium grease obtained in example 1, in which CTAB modified nano-molybdenum disulfide is addedThe lithium-based lubricating grease is 1020-1360 cm-1A characteristic peak of C-N appears between, 532cm-1The characteristic peak of the molybdenum disulfide disappears, which shows that CTAB is combined with molybdenum disulfide, and the thickness is 1810-1790 cm-1A new absorption peak appears, and the absorption peak belongs to an N-H bending vibration characteristic absorption peak and is 1400-700 cm-1The characteristic peak disappears, which shows that the surface of the molybdenum disulfide particles has new groups, and the organic modifier CTAB successfully carries out surface modification on the molybdenum disulfide, so that the overall surface energy is reduced. The nano molybdenum disulfide surface atoms have lone pair electrons, free cationic groups in a lubricating grease system are easily attracted, and the molybdenum disulfide with negative charges is combined with positive charge groups in CTAB molecules, so that the CTAB molecules are surrounded around the nano molybdenum disulfide, and the nano molybdenum disulfide is wrapped to reduce the surface energy of the nano molybdenum disulfide, thereby keeping the structure stable and preventing the nano molybdenum disulfide from agglomerating to achieve the effect of dispersing the nano molybdenum disulfide.
The lithium-based greases obtained in examples 1 to 3 and comparative examples 1 to 2 were tested for their properties, and the results are shown in Table 1. From table 1, in the aspect of working penetration, the addition of the nano molybdenum disulfide has no influence on the consistency and the grease forming performance of the lithium-based lubricating grease basically, but the difference of the penetration after the addition of the CTAB modified nano molybdenum disulfide is smaller, which indicates that the nano molybdenum disulfide modified by the CTAB is used as an additive to enable the nano molybdenum disulfide to be distributed in a grease framework better and reduce the adverse influence on the performance of the lithium-based lubricating grease; the drop point performance comparison shows that the drop point of the lithium-based lubricating grease can be improved by adding the nano molybdenum disulfide additive, and the drop point is higher after adding the CTAB modified nano molybdenum disulfide, so that the colloidal structure of the lithium-based soap fiber grease is more stable, and free oil can be better fixed in a soap fiber framework; the PB and PD performance comparison shows that the addition of the nano molybdenum disulfide additive can not improve the wear resistance and extreme pressure performance of the lithium-based lubricating grease, and the modified molybdenum disulfide can improve the PB (maximum seizure-free load) and PD (sintering load) of the lithium-based lubricating grease; the result of steel mesh branch oil performance can know, adds nanometer molybdenum disulfide and can reduce the oil content, adds the modified nanometer molybdenum disulfide of CTAB and can further reduce the oil content, explains that the modified nanometer molybdenum disulfide of CTAB can improve the solid oily ability of lithium base lubricating grease, and the fibrous structure of lubricating grease is more firm, can be with the locking that the oil content is tight in the fibrous framework. Therefore, the CTAB modification can not only improve the dispersion stability of the nano molybdenum disulfide, but also improve the comprehensive performance of the lithium-based lubricating grease.
TABLE 1 Performance results for lithium-based greases obtained in examples 1 to 3 and comparative examples 1 to 2
Figure BDA0002467378200000111
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 (10)

1. A preparation method of CTAB modified nano molybdenum disulfide is characterized by comprising the following steps:
mixing nano molybdenum disulfide, CTAB and ethanol to obtain a raw material mixed solution;
and carrying out reflux reaction on the raw material mixed solution for 22-26 h, and then standing for reaction for 22-26 h to obtain the CTAB modified nano molybdenum disulfide.
2. The preparation method of claim 1, wherein the mass ratio of the nano molybdenum disulfide to CTAB is 1 (3-5).
3. The method according to claim 1, wherein the reflux reaction is carried out at 75 to 85 ℃ and the standing reaction is carried out at room temperature.
4. The preparation method according to any one of claims 1 to 3, wherein after the standing reaction is completed, the method further comprises a post-treatment, and the post-treatment comprises the following steps: carrying out solid-liquid separation on the reaction liquid obtained by the standing reaction to obtain a solid; the solid was hot washed with alternating petroleum ether and ethanol and then dried.
5. The CTAB modified nano molybdenum disulfide obtained by the preparation method of any one of claims 1 to 4.
6. Use of the CTAB modified nano molybdenum disulphide as claimed in claim 5 as a grease additive.
7. The lithium-based lubricating grease comprises the following main raw materials in parts by mass: 90-100 parts of dodecahydroxy stearic acid, 750-900 parts of base oil, 13-17 parts of lithium hydroxide and 15-22 parts of lubricating grease additive, wherein the lubricating grease additive is the CTAB modified nano molybdenum disulfide as claimed in claim 5.
8. The method of preparing a lithium grease according to claim 7 comprising the steps of:
dissolving dodecahydroxy stearic acid in part of base oil to obtain a base oil solution of dodecahydroxy stearic acid;
dissolving lithium hydroxide in water to obtain a lithium hydroxide aqueous solution;
mixing the base oil solution of the dodecahydroxy stearic acid with a lithium hydroxide aqueous solution, and performing saponification reaction to obtain thickened lubricating oil;
sequentially dehydrating and refining the thickened lubricating oil to obtain anhydrous thickened lubricating oil;
and mixing the anhydrous thickened lubricating oil with the rest base oil and the lubricating grease additive, and then grinding to obtain the lithium-based lubricating grease.
9. The method according to claim 8, wherein the part of the base oil accounts for 2/3 of the total amount of the base oil, and the saponification reaction is carried out at 90-125 ℃ for 0.8-1.2 h.
10. The preparation method according to claim 8, wherein the dehydration temperature is 140-160 ℃ and the dehydration time is 15-30 min; the refining temperature is 190-210 ℃, and the refining time is 9-12 min.
CN202010338176.3A 2020-04-26 2020-04-26 CTAB modified nano molybdenum disulfide, preparation method and application thereof, lithium-based lubricating grease and preparation method thereof Pending CN111423916A (en)

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Application publication date: 20200717