CN114907909A - Lithium-based lubricating grease with alkyl tetrahydronaphthalene compound as blending oil and preparation method thereof - Google Patents
Lithium-based lubricating grease with alkyl tetrahydronaphthalene compound as blending oil and preparation method thereof Download PDFInfo
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- CN114907909A CN114907909A CN202210698759.6A CN202210698759A CN114907909A CN 114907909 A CN114907909 A CN 114907909A CN 202210698759 A CN202210698759 A CN 202210698759A CN 114907909 A CN114907909 A CN 114907909A
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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
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- 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
- C10M2203/06—Well-defined aromatic compounds
- C10M2203/065—Well-defined aromatic compounds used as base material
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- 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
- C10M2207/02—Hydroxy compounds
- C10M2207/023—Hydroxy compounds having hydroxy groups bound to carbon atoms of six-membered aromatic rings
- C10M2207/025—Hydroxy compounds having hydroxy groups bound to carbon atoms of six-membered aromatic rings with condensed rings
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- 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
- C10M2207/02—Hydroxy compounds
- C10M2207/023—Hydroxy compounds having hydroxy groups bound to carbon atoms of six-membered aromatic rings
- C10M2207/026—Hydroxy compounds having hydroxy groups bound to carbon atoms of six-membered aromatic rings with tertiary alkyl groups
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- 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
- C10M2207/121—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of seven or less carbon atoms
- C10M2207/123—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of seven or less carbon atoms polycarboxylic
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- 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
- C10M2207/126—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 monocarboxylic
- C10M2207/1265—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 monocarboxylic used as thickening agent
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- 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
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- 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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- C10M2215/00—Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
- C10M2215/02—Amines, e.g. polyalkylene polyamines; Quaternary amines
- C10M2215/06—Amines, e.g. polyalkylene polyamines; Quaternary amines having amino groups bound to carbon atoms of six-membered aromatic rings
- C10M2215/064—Di- and triaryl amines
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- C10M2215/00—Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
- C10M2215/22—Heterocyclic nitrogen compounds
- C10M2215/223—Five-membered rings containing nitrogen and carbon only
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- C10M2219/00—Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions
- C10M2219/02—Sulfur-containing compounds obtained by sulfurisation with sulfur or sulfur-containing compounds
- C10M2219/022—Sulfur-containing compounds obtained by sulfurisation with sulfur or sulfur-containing compounds of hydrocarbons, e.g. olefines
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- 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
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- C10M2219/00—Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions
- C10M2219/10—Heterocyclic compounds containing sulfur, selenium or tellurium compounds in the ring
- C10M2219/104—Heterocyclic compounds containing sulfur, selenium or tellurium compounds in the ring containing sulfur and carbon with nitrogen or oxygen in the ring
- C10M2219/108—Phenothiazine
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- C10M2223/00—Organic non-macromolecular compounds containing phosphorus as ingredients in lubricant compositions
- C10M2223/02—Organic non-macromolecular compounds containing phosphorus as ingredients in lubricant compositions having no phosphorus-to-carbon bonds
- C10M2223/04—Phosphate esters
- C10M2223/045—Metal containing thio derivatives
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- 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
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- C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
- C10N2030/08—Resistance to extreme temperature
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- C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
- C10N2030/10—Inhibition of oxidation, e.g. anti-oxidants
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- C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
- C10N2030/12—Inhibition of corrosion, e.g. anti-rust agents or anti-corrosives
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- C10N2050/00—Form in which the lubricant is applied to the material being lubricated
- C10N2050/10—Semi-solids; greasy
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Abstract
The invention provides lithium-based lubricating grease taking an alkyl tetrahydronaphthalene compound as blending oil and a preparation method thereof, belonging to the technical field of lubricating grease. The lithium-based lubricating grease disclosed by the invention comprises the following components in parts by mass: 40.0-55.0 parts of basic lithium grease, 0-5.0 parts of antioxidant, 0-5.0 parts of antirust agent and 1.0-10.0 parts of extreme pressure agent. Wherein the basic lithium-based grease is prepared from base oil compounded by alkyl tetrahydronaphthalene compound and poly alpha olefin. The alkyl tetrahydronaphthalene compound selected by the invention has good compatibility with the thickening agent and the additive, and the selected poly-alpha-olefin has excellent viscosity-temperature performance and high-temperature usability. The lithium-based lubricating grease obtained by compounding the two base oils has good friction performance and bearing and wear-resisting performance.
Description
Technical Field
The invention relates to the technical field of lubricating grease, in particular to lithium-based lubricating grease taking an alkyl tetrahydronaphthalene compound as blending oil and a preparation method thereof.
Background
The lubricating grease is a highly structured grease-like semisolid consisting of three parts, namely lubricating base oil, a thickening agent and an additive. Lubricating base oils have a significant impact on various properties of greases. The paraffinic oils among the mineral oils are the main base oils for preparing the grease, and polyalphaolefin synthetic oils (PAOs) as typical paraffinic oils make a great contribution in synthesizing lithium-based grease. The lithium-based lubricating grease is high-temperature multi-effect lubricating grease, has wide application fields, has certain defects in the aspect of bearing performance and the like, and needs to be added with organic or solid additives in the basic lithium-based lubricating grease for improving the lubricating property, the extreme pressure resistance, the oxygen resistance and the like of the lubricating grease. Lithium-based greases synthesized by PAOs have excellent low-temperature and high-temperature service properties, and because base oils, thickeners, additives and the like have poor solubility, relatively more thickeners and additives need to be used to improve the properties. However, since the production cost of raw materials such as thickeners and additives required for synthetic fats is increased, it is important to reduce the amount of both.
The PAO oil and the polar oil are blended, so that the defects of PAOs can be better improved, and the solubility of the PAO oil and the thickening agent and additives is increased. Research has been reported, and the structural strength and the bearing performance of the lubricating grease can be obviously improved by mixing PAOs with ester oil as the co-base oil to prepare the lithium-base lubricating grease. The structure of high polarity ester oils is very different from PAOs, leading to the problem that these two oils may have poor compatibility, thereby affecting the lubricating properties. Research has shown that ester oils with high polarity compete with additives for friction pair surfaces, reducing the efficacy of the additives. Meanwhile, esters are easily hydrolyzed in the presence of water, and easily cause pollution.
The series alkyl tetrahydronaphthalene oil products obtained by alkylation reaction of coal chemical raw material tetrahydronaphthalene and Fischer-Tropsch synthesized olefins with different chain lengths are aromatic compounds with special structures, contain a saturated ring, and can reduce the toxicity of naphthalene and products thereof. The alkyl tetrahydronaphthalene has the characteristics of high density, low pour point, good solubility, low viscosity, good thermal stability and the like, has a molecular structure and performance similar to those of petroleum-based naphthenic base oil, can supplement or replace the existing resource-type naphthenic lubricating base oil, and relieves the problem of resource shortage of the naphthenic base oil. However, at present, the use of alkyltetralins as common base oils for lithium-based greases has not been reported.
Disclosure of Invention
The invention aims to provide lithium-based lubricating grease taking alkyl tetrahydronaphthalene compound as blending oil and a preparation method thereof, and solves the technical problem that alkyl tetrahydronaphthalene is not taken as the blending oil of the lithium-based lubricating grease in the prior art.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides lithium-based lubricating grease taking an alkyl tetrahydronaphthalene compound as blending oil, which comprises the following components in parts by weight:
the basic lithium grease comprises the following components in parts by weight:
65.0-80.0 parts of base oil, 5.0-16.0 parts of fatty acid and 0.5-2.5 parts of lithium hydroxide;
the base oil comprises an alkyl tetrahydronaphthalene compound and poly-alpha-olefin synthetic oil in a mass ratio of 1: 1-9.
Further, the fatty acid comprises 12-hydroxystearic acid and/or stearic acid.
Further, the alkyl tetralin compound comprises one or more of hexyl tetralin, octyl tetralin, decyl tetralin, dodecyl tetralin, tetradecyl tetralin and hexadecyl tetralin, and the poly-alpha-olefin synthetic oil comprises one or more of PAO6, PAO8 and PAO 10.
Further, the antioxidant comprises one or more of 2, 6-di-tert-butyl-p-cresol, beta-naphthol, phenothiazine and diphenylamine; the antirust agent comprises one or more of barium petroleum sulfonate, barium dinonylnaphthalene sulfonate, zinc dinonylnaphthalene sulfonate, alkenyl succinic acid, dodecenylbutanediamine and benzotriazole.
Further, the extreme pressure agent comprises one or more of zinc dialkyl dithiophosphate, molybdenum dialkyl dithiophosphate and sulfurized isobutylene.
The invention provides a preparation method of lithium grease taking alkyl tetrahydronaphthalene compound as blending oil, which comprises the following steps:
1) mixing part of fatty acid with the first part of base oil, and then adding a lithium hydroxide aqueous solution for saponification to obtain mixed oil;
2) reacting the mixed oil with the rest fatty acid to obtain a reactant;
3) liquefying the reactant and a second part of base oil, cooling to be turbid, adding the rest part of base oil, cooling to room temperature, and homogenizing to obtain the basic lithium-based grease;
4) and mixing the basic lithium grease with other components and then carrying out homogenization treatment to obtain the lithium grease.
Furthermore, the partial fatty acid accounts for 88-96% of the total mass of the fatty acid; the first part of base oil accounts for 65-68% of the total mass of the base oil; the second part of base oil accounts for 15-18% of the total mass of the base oil.
Further, mixing the partial fatty acid and the first part of base oil at the temperature of 70-90 ℃ until the fatty acid is dissolved;
the temperature of the saponification treatment is 110-130 ℃, and the time of the saponification treatment is 0.5-3 h;
the mass concentration of the lithium hydroxide aqueous solution is 0.5-1.5 g/mL.
Further, the temperature of the reaction of the mixed oil and the rest fatty acid is 145-150 ℃, and the reaction time is 20-40 min; in the step 3), the temperature of the liquefaction reaction is 190-215 ℃, and the time of the liquefaction reaction is 8-12 min.
Further, the mixing temperature in the step 4) is between room temperature and 100 ℃, and the mixing time is 0.5 to 3 hours;
the homogenization treatment is grinding, and the grinding time is 0.5-2 h.
The invention has the beneficial effects that:
(1) the invention discloses a lithium-based lubricating grease prepared by blending an alkyl tetrahydronaphthalene compound and poly-alpha olefin synthetic oil as base oil for the first time, and the prepared lithium-based lubricating grease has good bearing and wear-resistant capabilities and is suitable for various severe working conditions.
(2) The invention adopts alkyl tetralin series compounds synthesized by coal-based raw materials to replace naphthenic base oil obtained by a petroleum route for oil product compounding, solves the problem of naphthenic base oil resource shortage, and has obvious resource advantages.
(3) The invention takes the alkyl tetrahydronaphthalene compound as the blend oil, improves the compatibility of the poly-alpha olefin synthetic oil with the thickening agent and the additive, can obviously reduce the use amount of the thickening agent and the additive, and saves the industrial application cost.
Detailed Description
The invention provides lithium-based lubricating grease taking an alkyl tetrahydronaphthalene compound as blending oil, which comprises the following components in parts by weight:
the basic lithium grease comprises the following components in parts by weight:
65.0-80.0 parts of base oil, 5.0-16.0 parts of fatty acid and 0.5-2.5 parts of lithium hydroxide;
the base oil comprises an alkyl tetrahydronaphthalene compound and poly-alpha-olefin synthetic oil in a mass ratio of 1: 1-9.
In the present invention, the content of the basic lithium grease is 40.0 to 55.0 parts by mass, preferably 43.0 to 52.0 parts by mass, and more preferably 46.0 to 49.0 parts by mass.
In the present invention, the basic lithium grease preferably comprises the following components in parts by mass:
66.0-78.0 parts of base oil, 8.0-12.0 parts of fatty acid and 1.0-2.0 parts of lithium hydroxide; more preferably: 70.0-73.0 parts of base oil, 10.0 parts of fatty acid and 1.5 parts of lithium hydroxide.
In the invention, the base oil comprises an alkyl tetrahydronaphthalene compound and a poly-alpha olefin synthetic oil in a mass ratio of 1: 1-9, preferably 1: 2-8, and more preferably 1: 3 to 6.
In the present invention, the fatty acid comprises 12-hydroxystearic acid and/or stearic acid, preferably stearic acid.
In the present invention, the alkyl tetralin compound includes one or more of hexyl tetralin, octyl tetralin, decyl tetralin, dodecyl tetralin, tetradecyl tetralin and hexadecyl tetralin, preferably one or more of hexyl tetralin, octyl tetralin, decyl tetralin and dodecyl tetralin, and more preferably hexyl tetralin and/or octyl tetralin.
In the invention, the viscosity of the alkyl tetrahydronaphthalene compound at 40 ℃ is 20-80 mm 2 Preferably 30 to 60 mm/s 2 (ii) s, more preferably 40mm 2 /s。
In the invention, the pour point of the alkyl tetrahydronaphthalene compound is less than or equal to-25 ℃, and the aniline point is less than or equal to 130 ℃; preferably, the pour point is less than or equal to-35 ℃, and the aniline point is less than or equal to 100 ℃.
In the present invention, the polyalphaolefin synthetic oil comprises one or more of PAO6, PAO8 and PAO10, preferably PAO6 and/or PAO 8.
In the present invention, the content of the antioxidant is 0 to 5.0 parts by mass, preferably 1.0 to 4.0 parts by mass, and more preferably 2.0 to 3.0 parts by mass.
In the invention, the antioxidant comprises one or more of 2, 6-di-tert-butyl-p-cresol, beta-naphthol, phenothiazine and diphenylamine, and preferably 2, 6-di-tert-butyl-p-cresol.
In the present invention, the content of the rust inhibitor is 0 to 5.0 parts by mass, preferably 1.0 to 4.0 parts by mass, and more preferably 2.0 to 3.0 parts by mass.
In the invention, the antirust agent comprises one or more of barium petroleum sulfonate, barium dinonylnaphthalene sulfonate, zinc dinonylnaphthalene sulfonate, alkenyl succinic acid, dodecenylbutanediamine and benzotriazole, and preferably alkenyl succinic acid.
In the present invention, the content of the extreme pressure agent is 1.0 to 10.0 parts by mass, preferably 2.0 to 8.0 parts by mass, and more preferably 4.0 to 6.0 parts by mass.
In the invention, the extreme pressure agent comprises one or more of zinc dialkyl dithiophosphate, molybdenum dialkyl dithiophosphate and sulfurized isobutylene, and is preferably sulfurized isobutylene.
The invention provides a preparation method of lithium grease taking alkyl tetrahydronaphthalene compound as blending oil, which comprises the following steps:
1) mixing part of fatty acid with the first part of base oil, and then adding a lithium hydroxide aqueous solution for saponification treatment to obtain mixed oil;
2) reacting the mixed oil with the rest part of fatty acid to obtain a reactant;
3) liquefying the reactant and a second part of base oil, cooling to be turbid, adding the rest part of base oil, cooling to room temperature, and homogenizing to obtain a base lithium base grease;
4) and mixing the basic lithium grease with other components and then carrying out homogenization treatment to obtain the lithium grease.
In the present invention, the fatty acid portion accounts for 88 to 96%, preferably 90 to 94%, and more preferably 92% of the total mass of the fatty acids.
In the invention, the first part of base oil accounts for 65-68% of the total mass of the base oil, and is preferably 66.7%.
In the invention, the second part of base oil accounts for 15-18% of the total mass of the base oil, and preferably 16.7%.
In the invention, the temperature for mixing the partial fatty acid and the first partial base oil is 70-90 ℃, and the mixing temperature is preferably 80 ℃ until the fatty acid is dissolved.
In the invention, the temperature of the saponification treatment is 110-130 ℃, and the time of the saponification treatment is 0.5-3 h; preferably, the saponification treatment temperature is 115-125 ℃, and the saponification treatment time is 1-2 h; further preferably, the temperature of the saponification treatment is 120 ℃ and the time of the saponification treatment is 1.5 hours.
In the present invention, the mass concentration of the lithium hydroxide aqueous solution is 0.5 to 1.5g/mL, preferably 0.8 to 1.2g/mL, and more preferably 1.0 to 1.2 g/mL.
In the invention, the temperature for the reaction of the mixed oil and the rest fatty acid is 145-150 ℃, and the reaction time is 20-40 min; preferably, the reaction temperature is 148 ℃ and the reaction time is 30 min.
In the invention, in the step 3), the temperature of the liquefaction reaction is 190-215 ℃, and the time of the liquefaction reaction is 8-12 min; preferably, the temperature of the liquefaction reaction is 200-205 ℃, and the time of the liquefaction reaction is 10 min.
In the invention, the mixing temperature in the step 4) is room temperature to 100 ℃, and the mixing time is 0.5 to 3 hours; preferably, the mixing temperature is 40-80 ℃, and the mixing time is 1-2 h; further preferably, the mixing temperature is 50-60 ℃, and the mixing time is 1.5 h.
In the present invention, the homogenization treatment is grinding, preferably in a three-roll mill; the grinding time is 0.5-2 h, preferably 1-1.5 h.
The technical solutions provided by the present invention are described in detail below with reference to examples, but they should not be construed as limiting the scope of the present invention.
Example 1
A homogeneous base oil was prepared by mixing 12.0g of hexyltetralin with 68.0g of PAO8 for 10min with stirring. Wherein the viscosity of the hexyltetralin at 40 ℃ is 28.3mm 2 The pour point was-42 ℃ and the aniline point 37.8 ℃.
Adding 5.3g of 12-hydroxystearic acid and 1.3g of stearic acid into 48.8g of base oil, heating to 80 ℃, adding 1.1mL of lithium hydroxide aqueous solution (containing 1.1g of lithium hydroxide) after the fatty acid is dissolved, mixing and stirring, maintaining the temperature at 120 ℃, saponifying for 2 hours, and completely dehydrating the soap base; then heating to 145 ℃, adding 0.8g of stearic acid with the pH value regulated and controlled, and continuing to react for 30min at constant temperature; adding 12.2g of base oil, rapidly heating to 190 ℃ of liquid crystal temperature, and keeping the liquid state for 10 min; cooling to turbidity, adding 12.2g of base oil, continuously stirring, cooling to room temperature, and uniformly grinding by a three-roller machine to obtain the base lithium grease, thus obtaining the finished product lithium grease.
49.0g of the obtained basic lithium grease and 1.0g of sulfurized isobutylene are stirred at 80 ℃ for 0.5h to be uniformly mixed, cooled to room temperature, and then ground and homogenized by a three-roller machine for 0.5h to obtain the lithium grease.
Comparative example 1
Adding 5.3g of 12-hydroxystearic acid and 1.3g of stearic acid into 48.8g of PAO8 base oil, heating to 80 ℃, adding 1.1mL of lithium hydroxide aqueous solution (containing 1.1g of lithium hydroxide) after the fatty acid is dissolved, mixing and stirring, maintaining the temperature at 120 ℃, saponifying for 2 hours, and completely dehydrating the soap base; then heating to 145 ℃, adding 0.8g of stearic acid with the pH value regulated and controlled, and continuing to react for 30min at constant temperature; adding 12.2g of PAO8 base oil, rapidly heating to liquid crystal temperature of 202 ℃, and keeping the liquid state for 10 min; cooling to turbidity, adding 12.2g of PAO8 base oil, continuously stirring, and after cooling to room temperature, uniformly grinding by a three-roller machine to obtain the basic lithium grease.
49.0g of the obtained basic lithium grease and 1.0g of sulfurized isobutylene are stirred at 100 ℃ for 2 hours, the mixture is uniformly mixed, and the mixture is ground and homogenized by a three-roller machine for 0.5 hour after being cooled to room temperature, so that the lithium grease is prepared.
The extreme pressure properties (50Hz, 80 ℃) of the lithium-based grease were evaluated using an SRV friction and wear tester as shown in Table 1 below. The result shows that the lithium-based lubricating grease synthesized by the oil product compounded by adding the extreme pressure agent sulfurized isobutylene with the same content, alkyl tetralin and PAO8 has obviously improved bearing capacity (running load) and more excellent bearing and wear resistance compared with the pure PAO8 lithium-based lubricating grease.
Table 1 performance test of lithium-based grease obtained in example 1 and comparative example 1
Running load | 200N | 300N | 400N |
Comparative example 1 | 4.29 | — | — |
Example 1 | 4.60 | 5.91 | 6.17 |
Example 2
A homogeneous base oil was prepared by mixing 16.0g of octyl tetralin with 64.0g of PAO8 for 10min with stirring. Wherein the viscosity of the octyl tetrahydronaphthalene at 40 ℃ is 35.9mm 2 The pour point was-38 ℃ and the aniline point was 49.8 ℃.
Adding 6.7g of stearic acid into 48.8g of base oil, heating to 80 ℃, adding 1.2mL of lithium hydroxide aqueous solution (containing 1.2g of lithium hydroxide) after the stearic acid is dissolved, mixing and stirring, maintaining the temperature at 110 ℃, and saponifying for 1.5h to completely dehydrate a soap base; then heating to 145 ℃, adding 0.8g of stearic acid with the pH value regulated and controlled, and continuing to react for 30min at constant temperature; adding 12.2g of base oil, rapidly heating to liquid crystal temperature of 196 ℃, and keeping the liquid state for 10 min; and cooling to turbidity, adding 12.2g of base oil, continuously stirring, and after cooling to room temperature, uniformly grinding by using a three-roller machine to obtain the lithium-based lubricating grease.
42.0g of the basic lithium grease, 2.4g of 2, 6-di-tert-butyl-p-cresol, 2.4g of benzotriazole and 3.2g of zinc dialkyldithiophosphate obtained above are stirred at 30 ℃ for 1 hour to be uniformly mixed, cooled to room temperature, and then ground and homogenized by a three-roll mill for 0.5 hour to obtain the lithium-based lubricating grease.
Comparative example 2
Adding 6.7g of stearic acid into 48.8g of PAO8 base oil, heating to 80 ℃, adding 1.2mL of lithium hydroxide aqueous solution (containing 1.2g of lithium hydroxide) after the stearic acid is dissolved, mixing and stirring, maintaining the temperature at 110 ℃, and saponifying for 1.5h to completely dehydrate a soap base; then heating to 145 ℃, adding 0.8g of stearic acid with the pH value regulated and controlled, and continuing to react for 30min at constant temperature; adding 12.2g of PAO8 base oil, rapidly heating to liquid crystal temperature of 206 deg.C, and keeping liquefied for 10 min; cooling to turbidity, adding 12.2g of PAO8 base oil, continuously stirring, and after cooling to room temperature, uniformly grinding by a three-roller machine to obtain the basic lithium grease.
42.0g of the basic lithium grease, 2.4g of 2, 6-di-tert-butyl-p-cresol, 2.4g of benzotriazole and 3.2g of zinc dialkyl dithiophosphate are stirred for 1 hour at 30 ℃, mixed uniformly, cooled to room temperature and then ground and homogenized for 0.5 hour by a three-roll mill to prepare the lithium-based lubricating grease.
The basic physical and chemical properties of the two lithium greases were compared and the extreme pressure properties were evaluated, and the results are shown in table 2 below. The result shows that the lithium-based lubricating grease synthesized by the oil product after the antioxidant, the antirust agent and the extreme pressure agent with the same content are added and the alkyl tetralin and the PAO8 are compounded has obviously improved thermal oxidation stability bearing capacity (running load) compared with the pure PAO8 lithium-based lubricating grease, shows more excellent oxidation stability and bearing wear resistance, and is beneficial to being used under severe conditions.
Table 2 performance test of lithium grease obtained in example 2 and comparative example 2
Example 3
A homogeneous base oil was prepared by mixing 16.0g of decyltetrahydronaphthalene with 64.0g of PAO8 for 10min with stirring. Wherein decyl tetrahydroThe viscosity of naphthalene at 40 ℃ is 46.8mm 2 The pour point was-38 ℃ and the aniline point 59.4 ℃.
Adding 6.7g of stearic acid into 48.8g of base oil, heating to 80 ℃, adding 1.2mL of lithium hydroxide aqueous solution (containing 1.2g of lithium hydroxide) after the stearic acid is dissolved, mixing and stirring, maintaining the temperature at 110 ℃, and saponifying for 1.5h to completely dehydrate a soap base; then heating to 145 ℃, adding 0.8g of stearic acid with the pH value regulated and controlled, and continuing to react for 30min at constant temperature; adding 12.2g of base oil, rapidly heating to liquid crystal temperature of 196 ℃, and keeping the liquid state for 10 min; cooling to turbidity, adding 12.2g of base oil, continuously stirring, and after cooling to room temperature, uniformly grinding by a three-roller machine to obtain the basic lithium grease.
43.5g of the basic lithium grease obtained above, 2.1g of beta-naphthol, 1.5g of dodecenyl butanediamine and 2.9g of molybdenum dialkyl dithiophosphate are stirred at room temperature for 1 hour, mixed uniformly, cooled to room temperature and then ground and homogenized by a three-roll mill for 0.5 hour to obtain the lithium grease.
Example 4
20.0g of dodecyltetralin and 60.0g of PAO6 synthetic oil are stirred and mixed for 10min to prepare the uniform base oil. Wherein the viscosity of the dodecyl tetrahydronaphthalene at 40 ℃ is 57.6mm 2 The pour point was-34 ℃ and the aniline point 80.6 ℃.
Adding 6.3g of 12-hydroxystearic acid and 1.6g of stearic acid into 48.0g of base oil, heating to 84 ℃, adding 1.3mL of lithium hydroxide aqueous solution (containing 1.3g of lithium hydroxide) after the fatty acid is dissolved, mixing and stirring, maintaining the temperature at 115 ℃, and saponifying for 1.5h to completely dehydrate a soap base; then heating to 150 ℃, adding 0.5g of stearic acid with the pH value regulated and controlled, and continuing to react for 30min at constant temperature; adding 12.0g of base oil, rapidly heating to 200 deg.C, and keeping liquefied for 10 min; cooling to turbidity, adding 12.0g of base oil, continuously stirring, and after cooling to room temperature, uniformly grinding by a three-roller machine to obtain the basic lithium grease.
Stirring the obtained basic lithium grease 46.5g, alkenyl succinic acid 1.5g and sulfurized isobutylene 2.0g at room temperature for 0.5h, uniformly mixing, cooling to room temperature, and grinding and homogenizing by a three-roller machine for 1h to obtain the lithium-based lubricating grease.
Example 5
A homogeneous base oil was prepared by mixing 24.0g tetradecyltetrahydronaphthalene with 56.0g PAO6 for 10min with stirring. Wherein the viscosity of the tetradecyl tetrahydronaphthalene at 40 ℃ is 61.5mm 2 The pour point was-32 ℃ and the aniline point was 92.2 ℃.
Adding 9.8g of 12-hydroxystearic acid into 46.7g of base oil, heating to 80 ℃, adding 1.6mL of lithium hydroxide aqueous solution (containing 1.6g of lithium hydroxide) after the 12-hydroxystearic acid is dissolved, mixing and stirring, maintaining the temperature at 115 ℃, saponifying for 2h, and completely dehydrating the soap base; then heating to 146 ℃, adding 0.8g of stearic acid with the pH value regulated and controlled, and continuing to react for 30min at constant temperature; adding 11.7g of base oil, rapidly heating to the liquid crystal temperature of 198 ℃, and keeping the liquid state for 10 min; cooling to turbidity, adding 11.7g of base oil, continuously stirring, and after cooling to room temperature, uniformly grinding by a three-roller machine to obtain the basic lithium grease.
47.5g of the basic lithium grease, 0.05g of diphenylamine, 0.05g of benzotriazole and 2.4g of zinc dialkyl dithiophosphate are stirred at room temperature for 0.5h to be uniformly mixed, cooled to room temperature and then ground by a three-roll mill for homogenization for 0.5h to prepare the lithium grease.
Example 6
A homogeneous base oil was prepared by mixing 32.0g of hexadecyltetralin with 48.0g of PAO6 for 10min with stirring. Wherein the viscosity of the hexadecyl tetrahydronaphthalene at 40 ℃ is 71.8mm 2 The pour point was-28 ℃ and the aniline point 93.8 ℃.
Adding 9.4g of 12-hydroxystearic acid and 2.4g of stearic acid into 45.3g of base oil, heating to 80 ℃, adding 1.9mL of lithium hydroxide aqueous solution (containing 1.9g of lithium hydroxide) after the fatty acid is dissolved, mixing and stirring, maintaining the temperature at 120 ℃, saponifying for 2 hours, and completely dehydrating the soap base; then heating to 145 ℃, adding 0.6g of stearic acid with the pH value regulated and controlled, and continuing to react for 30min at constant temperature; adding 11.3g of base oil, rapidly heating to the liquid crystal temperature of 203 ℃, and keeping the liquid state for 10 min; cooling to turbidity, adding 11.3g of base oil, continuously stirring, and after cooling to room temperature, uniformly grinding by a three-roller machine to obtain the basic lithium grease.
48.0g of the basic lithium grease obtained above, 0.05g of 2, 6-di-tert-butyl-p-cresol, 0.05g of barium dinonylnaphthalene sulfonate and 1.9g of molybdenum dialkyldithiophosphate are stirred at 100 ℃ for 2 hours, mixed uniformly, cooled to room temperature and then ground and homogenized by a three-roll mill for 0.5 hour to obtain the lithium grease.
The basic physical and chemical property comparison and the evaluation of extreme pressure performance of the lithium-based lubricating grease prepared in the embodiments 3 to 6 are shown in the following table 3, and the results show that the lithium-based lubricating grease synthesized by different alkyl tetralin and poly alpha olefin compound oils has good colloid stability, thermal oxidation stability and bearing capacity.
TABLE 3 Performance testing of lithium-based greases obtained in examples 3 to 6
From the above examples, the present invention provides a lithium grease using an alkyl tetralin compound as a blending oil and a method for preparing the same. The alkyl tetrahydronaphthalene compound selected by the invention has good compatibility with the thickening agent and the additive, and the selected poly-alpha-olefin has excellent viscosity-temperature performance and high-temperature usability. The lithium base grease obtained by compounding the two base oils has good friction performance and bearing and wear-resisting performance.
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. The lithium-based lubricating grease taking the alkyl tetrahydronaphthalene compound as the blending oil is characterized by comprising the following components in parts by mass:
the basic lithium grease comprises the following components in parts by weight:
65.0-80.0 parts of base oil, 5.0-16.0 parts of fatty acid and 0.5-2.5 parts of lithium hydroxide;
the base oil comprises an alkyl tetrahydronaphthalene compound and poly-alpha-olefin synthetic oil in a mass ratio of 1: 1-9.
2. The lithium-based grease using an alkyltetralin compound as a blending oil according to claim 1, wherein the fatty acid comprises 12-hydroxystearic acid and/or stearic acid.
3. The lithium-based grease using an alkyltetralin compound as a blending oil according to claim 2, wherein the alkyltetralin compound comprises one or more of hexyltetralin, octyltetralin, decyltetralin, dodecyltetralin, tetradecyltetralin, and hexadecyltetralin, and the polyalphaolefin synthetic oil comprises one or more of PAO6, PAO8, and PAO 10.
4. The lithium-based grease using an alkyl tetrahydronaphthalene compound as a blending oil according to any one of claims 1 to 3, wherein the antioxidant comprises one or more of 2, 6-di-tert-butyl-p-cresol, beta-naphthol, phenothiazine and diphenylamine; the antirust agent comprises one or more of barium petroleum sulfonate, barium dinonylnaphthalene sulfonate, zinc dinonylnaphthalene sulfonate, alkenyl succinic acid, dodecenylbutanediamine and benzotriazole.
5. The lithium-based grease using an alkyltetralin compound as a co-mixed oil according to claim 4, wherein the extreme pressure agent comprises one or more of zinc dialkyldithiophosphate, molybdenum dialkyldithiophosphate, and sulfurized isobutylene.
6. The method for preparing the lithium-based grease using the alkyl tetrahydronaphthalene compound as the blending oil according to any one of claims 1 to 5, comprising the steps of:
1) mixing part of fatty acid with the first part of base oil, and then adding a lithium hydroxide aqueous solution for saponification to obtain mixed oil;
2) reacting the mixed oil with the rest fatty acid to obtain a reactant;
3) liquefying the reactant and a second part of base oil, cooling to be turbid, adding the rest part of base oil, cooling to room temperature, and homogenizing to obtain a base lithium base grease;
4) and mixing the basic lithium grease with other components and then carrying out homogenization treatment to obtain the lithium grease.
7. The preparation method according to claim 6, wherein the partial fatty acid accounts for 88-96% of the total mass of the fatty acid; the first part of base oil accounts for 65-68% of the total mass of the base oil; the second part of base oil accounts for 15-18% of the total mass of the base oil.
8. The method according to claim 6 or 7, wherein the temperature for mixing the partial fatty acid with the first part of base oil is 70 to 90 ℃ until the fatty acid is dissolved;
the temperature of the saponification treatment is 110-130 ℃, and the time of the saponification treatment is 0.5-3 h;
the mass concentration of the lithium hydroxide aqueous solution is 0.5-1.5 g/mL.
9. The preparation method according to claim 8, wherein the temperature of the reaction of the mixed oil and the rest of the fatty acid is 145-150 ℃, and the reaction time is 20-40 min; in the step 3), the temperature of the liquefaction reaction is 190-215 ℃, and the time of the liquefaction reaction is 8-12 min.
10. The preparation method according to claim 7 or 9, wherein the mixing temperature in the step 4) is room temperature to 100 ℃, and the mixing time is 0.5 to 3 hours;
the homogenization treatment is grinding, and the grinding time is 0.5-2 h.
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