CN107828473B - High-low temperature resistant long-life extreme pressure lubricating grease and preparation method thereof - Google Patents
High-low temperature resistant long-life extreme pressure lubricating grease and preparation method thereof Download PDFInfo
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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
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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
- C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
- C10M2201/06—Metal compounds
- C10M2201/062—Oxides; Hydroxides; Carbonates or bicarbonates
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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
- 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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- 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
- C10M2205/0206—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions containing acyclic monomers used as base material
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- 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
- C10M2207/127—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 polycarboxylic
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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
- 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
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- 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
- C10M2215/22—Heterocyclic nitrogen compounds
- C10M2215/223—Five-membered rings containing nitrogen and carbon only
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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
- 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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- 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
- C10M2219/06—Thio-acids; Thiocyanates; Derivatives thereof
- C10M2219/062—Thio-acids; Thiocyanates; Derivatives thereof having carbon-to-sulfur double bonds
- C10M2219/066—Thiocarbamic type compounds
- C10M2219/068—Thiocarbamate metal salts
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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
- 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
- C10M2219/106—Thiadiazoles
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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
- 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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- 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
- C10N2030/08—Resistance to extreme temperature
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- 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
- C10N2030/26—Waterproofing or water resistance
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- 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 discloses a high-low temperature resistant and long-life extreme pressure lubricating grease and a preparation method thereof, wherein the lubricating grease comprises the following components in percentage by weight: 80-85% of mixed base oil, 9-16% of thickening agent, 0.5-1.5% of structure improving agent, 1.0-3.0% of extreme pressure antiwear agent, 0.5-1.5% of metal deactivator, 0.05-1.5% of antirust agent and 0.3-1.5% of antioxidant; wherein the mixed base oil contains alkyl naphthalene, and the weight percentage of the alkyl naphthalene in the mixed base oil is 10-30%. The invention has the advantages that the product has excellent high-temperature performance, water resistance, extreme pressure resistance and friction resistance, stable structure, safe and environment-friendly production and simple process, and is suitable for various lubricating occasions requiring high and low temperature resistance and extreme pressure wear resistance, such as automobile hub bearings, constant velocity universal joints, high temperature bearings and other fields.
Description
Technical Field
The invention belongs to the field of lubricating grease, and particularly relates to high-low temperature resistant long-life extreme pressure lubricating grease and a preparation method thereof.
Background
In the current situation of global economic slowdown, it is desirable for both the equipment owners and operators to reduce the maintenance costs of the equipment, which has led to a greater demand for long life greases with long grease change periods that perform well under high temperature, low temperature, heavy load, etc. The high dropping point lubricating grease mainly comprises composite calcium lubricating grease, composite lithium-based lubricating grease, composite aluminum-based lubricating grease, composite calcium sulfonate-based lubricating grease, polyurea-based lubricating grease and bentonite lubricating grease, wherein the composite lithium-based lubricating grease has the advantages of safe and environment-friendly production process, relatively high degree of production process technology, good compatibility with additives, wide application and the like and is widely concerned. According to survey statistics, the yield of the lithium complex grease in China in 2015 reaches 6.42 ten thousand tons, accounts for 16.62 percent of the annual grease yield, is the high dropping point grease with the highest proportion, and other high dropping point greases such as polyurea grease and calcium complex sulfonate grease account for only 5.08 percent and 1.42 percent. Therefore, the application prospect and the demand of the composite lithium-based lubricating grease are getting larger and larger. However, most of the base oil adopted by the composite lithium-based lubricating grease produced in China at present is I-type mineral base oil, the oxidation resistance and low temperature resistance of the product are poor, the use temperature can only reach-20-150 ℃, the service life is short, and the requirements of high and low temperature resistance, extreme pressure antifriction property and long service life of the lubricating grease provided by the development of modern vehicles and equipment technologies cannot be met.
Currently, polyurea thickening agents are mostly adopted in China to produce high-temperature-resistant long-life lubricating grease, for example, CN101649243B introduces a high-temperature and low-temperature lubricating grease and a preparation method thereof, polyurea lubricating grease prepared by taking octadecylamine, cyclohexylamine and diphenylmethane diisocyanate as raw materials is used, but the toxicity of the production raw materials is high, the production raw materials are not safe and environment-friendly, and the product can be hardened at high temperature. CN105087108A discloses a high and low temperature resistant lubricating grease and a preparation method thereof, which is prepared by taking composite calcium sulfonate soap as thickening poly-alpha olefin and adding additives such as extreme pressure, oxidation and the like, and not only has complex preparation process and poor product stability, but also has the problem that the product is easy to harden after being placed for a long time. CN102286306A also provides a high-temperature water-resistant long-life composite lithium-calcium-based lubricating grease and a preparation method thereof, the composite calcium sulfonate soap and the composite lithium-calcium soap are mixed to be used as a thickening agent, the production process is complex, the dropping point of the prepared product is lower than 300 ℃, and meanwhile, the addition of the composite calcium sulfonate soap can influence the low-temperature performance of the product and can not well meet the low-temperature use requirement. In addition, the low-temperature lubricating grease reported in other related patents is mostly prepared by thickening poly-alpha-olefin or ester oil with lithium soap or composite lithium soap, and has the problems of poor compatibility of prefabricated soap or lubricating grease with additives and the like, and accordingly, the production difficulty is increased or the product performance is reduced.
Therefore, a better solution is needed to solve the problems of the prior art, so as to meet the requirements of modern industrial development on grease with high and low temperature resistance, high extreme pressure and long service life.
Disclosure of Invention
The purpose of the invention is as follows: the first purpose of the invention is to provide the extreme pressure grease with high and low temperature resistance and long service life, which can improve the compatibility of base oil and complex lithium soap or complex lithium calcium soap; the second purpose of the invention is to provide a preparation method of the lubricating grease.
The technical scheme is as follows: the extreme pressure lubricating grease with high and low temperature resistance and long service life comprises the following components in percentage by weight: 80-85% of mixed base oil, 9-16% of thickening agent, 0.5-1.5% of structure improving agent, 1.0-3.0% of extreme pressure antiwear agent, 0.5-1.5% of metal deactivator, 0.05-1.5% of antirust agent and 0.3-1.5% of antioxidant; the mixed base oil contains alkyl naphthalene, and the weight percentage of the alkyl naphthalene in the mixed base oil is 10-30%.
Wherein the content of the first and second substances,the mixed base oil contains at least one of hydrogenated base oil and poly-alpha-olefin oil, and the kinematic viscosity of the mixed base oil at 40 ℃ is 60-150 mm2(ii) a viscosity index of not less than 120. The alkyl naphthalene is mixed with the hydrogenated base oil or the poly-alpha olefin oil, so that the compatibility of the base oil and the composite lithium soap can be improved, the structural stability of the lubricating grease is ensured, the application effect of various polar additives in the fully-synthesized composite lithium base grease is enhanced, the use amount of the additives is reduced, and the problems of poor structural stability and poor compatibility with the additives in the traditional preparation of the composite lithium base grease by adopting synthetic oil are solved. In addition, the addition of alkyl naphthalene can further improve the high-temperature oxidation resistance, low-temperature fluidity and compatibility with rubber sealing materials of the lubricating grease.
The extreme pressure antiwear agent adopted by the invention is at least one of zinc dialkyl dithiophosphate, molybdenum dialkyl dithiocarbamate and aminothioester; the metal deactivator adopted by the invention is a thiadiazole derivative or a benzotriazole derivative. The excellent wear resistance (but serious corrosion to copper) of molybdenum dialkyl dithiocarbamate and the excellent extreme pressure performance expressed by the synergistic effect of molybdenum dialkyl dithiocarbamate and thiadiazole derivatives are utilized, so that the lubricating grease is ensured to have better extreme pressure performance and wear resistance on the premise of lower additive addition, the sintering load of the prepared fully-synthetic composite lithium-based grease/composite lithium-calcium-based grease reaches more than 400kg, and the diameter of a wear scar is less than 0.45 mm. Meanwhile, the thiadiazole derivative is used as a metal deactivator to inhibit the corrosion problem caused by the molybdenum salt antiwear agent, thereby achieving double effects.
The structure improver adopted by the invention is a hydroxylated C3-C20 olefin multi-block copolymer, and is used for improving the fiber structure of the lubricating grease; preferably, the texture improving agent is Lubrizol 2002D. The water resistance of the composite lithium is effectively improved by utilizing the interaction of hydrogen bonds formed between the composite lithium soap and a composite lithium soap fiber structure, and the low-temperature performance of the composite lithium soap is not influenced.
The thickening agent adopted by the invention is a composite lithium soap or a composite lithium calcium soap, wherein in the raw material of the thickening agent, the molar ratio of 12-hydroxystearic acid to sebacic acid is 1: 0.4-1: 0.8; preferably, the molar ratio of the 12-hydroxystearic acid to the sebacic acid is 1: 0.5-1: 0.6. The antirust agent is at least one of benzotriazole, barium dinonylnaphthalene sulfonate and calcium petroleum sulfonate. The antioxidant is at least one of amine antioxidant and phenol antioxidant, wherein the amine antioxidant is preferably octyl/butyl diphenylamine, and the phenol antioxidant is preferably 2, 6-di-tert-butyl-p-cresol.
The invention also provides a preparation method of the extreme pressure lubricating grease with high and low temperature resistance and long service life, which comprises the following steps: weighing the components according to the weight percentage, and preparing the mixed base oil and the thickening agent, wherein the structural improvement agent is added in the saponification stage of preparing the thickening agent, the temperature is raised to 210-220 ℃, then the temperature is reduced to below 90 ℃, the rest components are added, and the finished product is obtained by uniformly stirring, mixing and grinding for dispersion.
During the preparation process of the thickening agent, sequentially adding part of the mixed base oil, the thickening agent raw material 12-hydroxystearic acid and sebacic acid into a reaction kettle, mixing, stirring and heating to 80-85 ℃, then adding another thickening agent raw material lithium hydroxide oil solution or adding a calcium hydroxide emulsion, then adding a lithium hydroxide oil solution, and after the addition is finished, carrying out heat preservation reaction at 95-105 ℃ for 60-90 minutes; heating to 130-140 ℃, dehydrating and preserving heat for 30-40 minutes, adding an antioxidant and a structure improving agent, and continuously heating to the maximum temperature of 210-220 ℃; then adding the rest mixed base oil and cooling to below 90 ℃.
Since the water resistance of the lithium complex grease is inferior to that of other thickening agents such as calcium complex grease, the conventional method for improving the water resistance is to add a tackifier such as polyisobutylene, but the low-temperature performance of the grease is greatly affected by adding the polyisobutylene, and the water resistance is not greatly improved. According to the invention, the special structure improver is added in the saponification stage, and the polarity of the structure improver and the hydrogen bond formed between the soap fiber structure molecules are utilized, so that the composite lithium grease can maintain excellent low-temperature characteristics and simultaneously improve the water scouring resistance.
Has the advantages that: compared with the prior art, the invention has the advantages that: (1) the lubricating grease disclosed by the invention has good high and low temperature resistance, extreme pressure abrasion resistance and water resistance and long service life, can meet the lubricating requirements of equipment and bearings under various heavy load working conditions at the temperature of-40-180 ℃, is suitable for the fields of automobile hub bearings, constant velocity universal joints, high temperature bearings and the like, and is particularly suitable for lubricating all bearings of electric automobiles. (2) According to the invention, a special structure improver is selected, and the water resistance of the composite lithium is effectively improved by utilizing the interaction of hydrogen bonds formed between the special structure improver and the composite lithium soap fiber structure, and the low-temperature performance of the composite lithium is not influenced. (3) The production process is simple, safe and environment-friendly, and is favorable for large-scale production.
Detailed Description
The technical solution of the present invention is further explained below.
The lithium hydroxide oil solutions used in the following examples were prepared: anhydrous lithium hydroxide purchased in the market is ground into powder with the diameter of 8 mu m by a ball mill, and then micron-sized lithium hydroxide is dispersed in base oil 150SN by a high-speed dispersion machine, and the content of the lithium hydroxide in the prepared lithium hydroxide oil solution is 36.5 percent. Other raw materials are all conventional raw materials purchased from commercial places unless otherwise specified.
Example 1
Mixing poly alpha olefin oil PAO1092.88kg and alkyl naphthalene Synestic 1230.96kg as mixed base oil (the kinematic viscosity of the mixed base oil at 40 ℃ is 78 mm)2In s, viscosity index of 123). Adding 82.2kg of mixed base oil, 10.5kg of 12-hydroxystearic acid and 3.54kg of sebacic acid into a saponification reaction kettle in sequence, starting stirring and heating to 82 ℃, then adding 4.92kg of lithium hydroxide oil solution, carrying out saponification reaction at 95-105 ℃ for 90 minutes after the addition is finished, then heating to 135 ℃ and carrying out heat preservation for 30 minutes, adding Irganox L570.45kg of antioxidant and 0.75kg of structure improver Lubrizol2002D 0.75, continuing heating to 215 ℃ and carrying out heat preservation for 5 minutes, finally transferring the materials to a blending kettle, adding 41.64kg of the rest mixed base oil and cooling, and adding 1.5kg of molybdenum dialkyl dithiocarbamate, 1.5kg of zinc dialkyl dithiophosphate, 1.5kg of thiadiazole derivative and 1.5kg of barium dinonylnaphthalene sulfonate into the mixture after the temperature is reduced to 90 ℃, and grinding and dispersing the mixture by a three-roll grinder after the mixture is uniformly stirred and mixed to obtain a finished product. The measurement data of example 1 are shown in Table 1.
Example 2
Poly-alpha olefin oil PAO4037.8kg, PAO1070.33kg and alkyl naphthalene Synessic 1212.01kg are mixed as mixed base oil (the kinematic viscosity at 40 ℃ of the mixed base oil is 115 mm)2In/s, viscosity index 138). Adding 80kg of mixed base oil, 13.5kg of 12-hydroxystearic acid and 4.55kg of sebacic acid into a saponification reaction kettle in sequence, starting stirring and heating to 82 ℃, then adding 0.80kg of calcium hydroxide emulsion and 4.86kg of lithium hydroxide oil solution in sequence, carrying out saponification reaction at 105 ℃ for 75 minutes after the addition is finished, then heating to 140 ℃ and keeping the temperature for 40 minutes, adding Irganox L570.075kg of antioxidant and 0.75kg of structure improver Lubrizol2002D, continuing heating to 220 ℃ and keeping the temperature for 5 minutes, finally transferring the materials to a blending kettle, adding 40.14kg of the rest mixed base oil and cooling, adding 3kg of molybdenum dialkyl dithiophosphate, 1.5kg of zinc dialkyl dithiophosphate, 0.75kg of thiadiazole derivative and 0.075kg of benzotriazole in sequence when the temperature is reduced to 90 ℃, stirring and mixing uniformly, and then grinding and dispersing by a three-roll grinder to obtain the finished product. The measurement data of example 2 are shown in Table 1.
Example 3
Mixing poly alpha olefin oil PAO 10103.29kg and alkyl naphthalene SynNaph2319.4kg as mixed base oil (the kinematic viscosity of the mixed base oil is 80mm at 40℃)2In s, viscosity index 129). Adding 86kg of mixed base oil, 10.5kg of 12-hydroxystearic acid and 4.23kg of sebacic acid into a saponification reaction kettle in sequence, stirring and heating to 82 ℃, adding 5.08kg of lithium hydroxide oil solution, performing saponification reaction at 95-105 ℃ for 90 minutes after the addition is finished, heating to 135 ℃ and keeping the temperature for 30 minutes, adding Irganox L1350.25kg, Irganox L570.5kg and a structure improver Lubrizol2002D 1.5kg, continuing heating to 210 ℃ and keeping the temperature for 5 minutes, transferring the material to a blending kettle, adding 36.69kg of the rest mixed base oil, cooling, adding 2.25kg of molybdenum dialkyl dithiocarbamate, 1.5kg of thiadiazole derivative and 1.5kg of barium dinonylnaphthalene sulfonate in sequence when the temperature is reduced to 90 ℃, stirring and mixing uniformly, and grinding and dispersing by a three-roll grinder to obtain the finished product. The measurement data of example 3 are shown in Table 1.
Example 4
Taking hydrogenated base oil GTL25088.44kg and alkyl naphthalene SynNaph2334.25kg as mixed base oil (mixed base oil with kinematic viscosity of 65mm at 40 deg.C)2In s, viscosity index of 142). Adding 86kg of mixed base oil, 10.5kg of 12-hydroxystearic acid and 4.23kg of sebacic acid into a saponification reaction kettle in sequence, stirring and heating to 82 ℃, adding 5.08kg of lithium hydroxide oil solution, performing saponification reaction at 95-105 ℃ for 90 minutes after the addition is finished, heating to 135 ℃ and keeping the temperature for 30 minutes, adding Irganox L1350.25kg, Irganox L570.5kg and a structure improver Lubrizol2002D 1.5kg, continuing heating to 210 ℃ and keeping the temperature for 5 minutes, transferring the material to a blending kettle, adding 36.69kg of the rest mixed base oil, cooling, adding 2.25kg of molybdenum dialkyl dithiocarbamate, 1.5kg of thiadiazole derivative and 1.5kg of barium dinonylnaphthalene sulfonate in sequence when the temperature is reduced to 90 ℃, stirring and mixing uniformly, and grinding and dispersing by a three-roll grinder to obtain the finished product. The data of the example four are shown in Table 1.
Example 5
Mixing hydrogenated base oil GTL25061.92kg, PAO4026.52kg and alkyl naphthalene SynNaph2334.25kg to obtain mixed base oil (the kinematic viscosity of the mixed base oil is 100mm at 40 ℃)2In s, viscosity index 145). Adding 86kg of mixed base oil, 10.5kg of 12-hydroxystearic acid and 4.23kg of sebacic acid into a saponification reaction kettle in sequence, stirring and heating to 82 ℃, adding 5.08kg of lithium hydroxide oil solution, performing saponification reaction at 95-105 ℃ for 90 minutes after the addition is finished, heating to 135 ℃ and keeping the temperature for 30 minutes, adding Irganox L1350.25kg, Irganox L570.5kg and a structure improver Lubrizol2002D 1.5kg, continuing heating to 210 ℃ and keeping the temperature for 5 minutes, transferring the material to a blending kettle, adding 36.69kg of the rest mixed base oil, cooling, adding 2.25kg of molybdenum dialkyl dithiocarbamate, 1.5kg of thiadiazole derivative and 1.5kg of barium dinonylnaphthalene sulfonate in sequence when the temperature is reduced to 90 ℃, stirring and mixing uniformly, and grinding and dispersing by a three-roll grinder to obtain the finished product. The data for the measurement of example five are shown in table 1.
Example 6
3 sets of parallel experiments were designed, the basic procedure being the same as in example 1, except for the content of each component of the mixed base oil, as shown in Table 2. The physical and chemical property test data of the prepared lubricating grease are shown in table 1.
Table 2 base oil component content of three parallel runs in example 6
Example 7
Mixing poly-alpha olefin oil PAO1086.84kg and alkyl naphthalene Synestic 1235.5 kg as mixed base oil (the kinematic viscosity of the mixed base oil at 40 ℃ is 78 mm)2In s, viscosity index of 123). Adding 82.2kg of mixed base oil, 10.5kg of 12-hydroxystearic acid and 3.54kg of sebacic acid into a saponification reaction kettle in sequence, starting stirring and heating to 82 ℃, then adding 4.92kg of lithium hydroxide oil solution, carrying out saponification reaction at 95-105 ℃ for 90 minutes after the addition is finished, then heating to 135 ℃ and carrying out heat preservation for 30 minutes, adding Irganox L570.45kg of antioxidant and Lubrizol2002 D2.25kg of structure improver, continuing heating to 215 ℃ and carrying out heat preservation for 5 minutes, finally transferring the materials to a blending kettle, adding 40.14kg of the rest mixed base oil, cooling, and adding 1.5kg of molybdenum dialkyl dithiocarbamate, 1.5kg of zinc dialkyl dithiophosphate, 1.5kg of thiadiazole derivative and 1.5kg of barium dinonylnaphthalene sulfonate into the mixture after the temperature is reduced to 90 ℃, stirring and mixing uniformly, and then grinding and dispersing the mixture by a three-roll grinder to obtain the finished product. The measurement data of example seven are shown in Table 1.
Comparative example 1
Mixing poly-alpha olefin oil PAO1087.59kg and alkyl naphthalene Synessic 1237 kg to obtain mixed base oil (the kinematic viscosity of the mixed base oil at 40 ℃ is 78 mm)2In s, viscosity index of 123). Sequentially adding 82.2kg of mixed base oil, 10.5kg of 12-hydroxystearic acid and 3.54kg of sebacic acid into a saponification reaction kettle, stirring and heating to 82 ℃, then adding 4.92kg of lithium hydroxide oil solution, performing saponification reaction at 95-105 ℃ for 90 minutes after the addition is finished, heating to 135 ℃ and keeping the temperature for 30 minutes, addingAdding an antioxidant Irganox L570.45kg, continuously heating to 215 ℃ and preserving heat for 5 minutes, finally transferring the materials to a blending kettle, adding 42.39kg of the rest mixed base oil, cooling, sequentially adding 1.5kg of molybdenum dialkyl dithiocarbamate, 1.5kg of zinc dialkyl dithiophosphate, 1.5kg of thiadiazole derivative and 1.5kg of barium dinonyl naphthalene sulfonate when the temperature is reduced to below 90 ℃, uniformly stirring and mixing, and grinding and dispersing by a three-roll grinder to obtain the finished product. The measurement data of comparative example 1 is shown in Table 1.
Comparative example 2
Mixing poly-alpha-olefin oil PAO1086.64kg and alkyl naphthalene Synestic 1237.2kg as mixed base oil (the kinematic viscosity of the mixed base oil at 40 ℃ is 78 mm)2In s, viscosity index of 123). Adding 82.2kg of mixed base oil, 10.5kg of 12-hydroxystearic acid and 3.54kg of sebacic acid into a saponification reaction kettle in sequence, starting stirring and heating to 82 ℃, then adding 4.92kg of lithium hydroxide oil solution, carrying out saponification reaction at 95-105 ℃ for 90 minutes after the addition is finished, then heating to 135 ℃ and carrying out heat preservation for 30 minutes, adding Irganox L570.45kg of antioxidant, continuing heating to 215 ℃ and carrying out heat preservation for 5 minutes, finally transferring the materials to a blending kettle, adding 41.64kg of the rest mixed base oil, cooling, sequentially adding 0.75kg of structure improving agent Lubrizol2002D, 1.5kg of molybdenum dialkyl dithiocarbamate, 1.5kg of zinc dialkyl dithiophosphate, 1.5kg of thiadiazole derivative and 1.5kg of barium dinonylnaphthalene sulfonate when the temperature is reduced to 90 ℃, stirring and uniformly mixing, and then grinding and dispersing by a three-roll grinder to obtain the finished product. The measurement data of comparative example 2 is shown in Table 1.
Comparative example 3
Mixing poly-alpha-olefin oil PAO4039.64kg and PAO1080.5kg as mixed base oil (the kinematic viscosity of the mixed base oil at 40 ℃ is 115 mm)2In s, viscosity index 147). Adding 80kg of mixed base oil, 13.5kg of 12-hydroxystearic acid and 4.55kg of sebacic acid into a saponification reaction kettle in sequence, starting stirring and heating to 82 ℃, then adding 0.80kg of calcium hydroxide emulsion and 4.86kg of lithium hydroxide oil solution in sequence, carrying out saponification reaction at 105 ℃ for 75 minutes after the addition is finished, heating to 140 ℃ and keeping the temperature for 40 minutes, adding 0.75kg of antioxidant Irganox L570.075kg and structure improver Lubrizol2002D, continuously heating to 220 ℃ and keeping the temperatureAnd (3) heating for 5 minutes, finally transferring the materials to a blending kettle, adding 40.14kg of the rest mixed base oil, cooling, sequentially adding 3kg of molybdenum dialkyl dithiophosphate, 1.5kg of zinc dialkyl dithiophosphate, 0.75kg of thiadiazole derivative and 0.075kg of benzotriazole when the temperature is reduced to below 90 ℃, uniformly stirring and mixing, and grinding and dispersing by a three-roll grinder to obtain a finished product. The measurement data of comparative example 3 are shown in Table 1.
Comparative example 4
Poly-alpha-olefin oil PAO4037.8kg, PAO1076.34kg and alkyl naphthalene Synessitic 126.0 kg are mixed as mixed base oil (the kinematic viscosity at 40 ℃ of the mixed base oil is 110 mm)2In/s, viscosity index 136). Adding 80kg of mixed base oil, 13.5kg of 12-hydroxystearic acid and 4.55kg of sebacic acid into a saponification reaction kettle in sequence, starting stirring and heating to 82 ℃, then adding 0.80kg of calcium hydroxide emulsion and 4.86kg of lithium hydroxide oil solution in sequence, carrying out saponification reaction at 105 ℃ for 75 minutes after the addition is finished, then heating to 140 ℃ and keeping the temperature for 40 minutes, adding Irganox L570.075kg of antioxidant and 0.75kg of structure improver Lubrizol2002D, continuing heating to 220 ℃ and keeping the temperature for 5 minutes, finally transferring the materials to a blending kettle, adding 40.14kg of the rest mixed base oil and cooling, adding 3kg of molybdenum dialkyl dithiophosphate, 1.5kg of zinc dialkyl dithiophosphate, 0.75kg of thiadiazole derivative and 0.075kg of benzotriazole in sequence when the temperature is reduced to 90 ℃, stirring and mixing uniformly, and then grinding and dispersing by a three-roll grinder to obtain the finished product. The measurement data of comparative example 4 is shown in Table 1.
Comparative example 5
The polyalphaolefin oil PAO4037.8kg, PAO1040.29kg and alkyl naphthalene Synessic 1242.05kg are mixed to be used as mixed base oil (the kinematic viscosity of the mixed base oil at 40 ℃ is 124 mm)2In s, viscosity index 127). Adding 80kg of mixed base oil, 13.5kg of 12-hydroxystearic acid and 4.55kg of sebacic acid into a saponification reaction kettle in sequence, starting stirring and heating to 82 ℃, then adding 0.80kg of calcium hydroxide emulsion and 4.86kg of lithium hydroxide oil solution in sequence, carrying out saponification reaction at 105 ℃ for 75 minutes after the addition is finished, heating to 140 ℃ and keeping the temperature for 40 minutes, adding 0.75kg of antioxidant Irganox L570.075kg and structure improver Lubrizol2002D, continuing heating to 220 ℃ and keeping the temperatureAnd 5 minutes, finally transferring the materials to a blending kettle, adding 40.14kg of the rest mixed base oil, cooling, sequentially adding 3kg of molybdenum dialkyl dithiophosphate, 1.5kg of zinc dialkyl dithiophosphate, 0.75kg of thiadiazole derivative and 0.075kg of benzotriazole when the temperature is reduced to below 90 ℃, uniformly stirring and mixing, and grinding and dispersing by a three-roll grinder to obtain a finished product. The measurement data of comparative example 5 is shown in Table 1.
Table 1 physical and chemical property test data of grease of each example
As can be seen from the data in table 1, compared with the example (such as example 2) in which the alkyl naphthalene is added, the performance index of comparative example 3 without the alkyl naphthalene is reduced in the drop point, the steel mesh oil separation, the water leaching loss, the extreme pressure performance, and the like, because the polyalphaolefin oil has a weak polarity and a poor compatibility with the complex lithium soap thickener and the additive, the dispersion state of the thickener in the mixed base oil is unstable, and the mixed base oil is easily separated from the fibrous structure of the thickener soap when high temperature is encountered. The alkyl naphthalene has stronger polarity and can form intermolecular hydrogen bonds with the thickening agent, so that the base oil is effectively fixed in the skeleton of the thickening agent, and the alkyl naphthalene has strong dissolving capacity on the additive and can enhance the structural stability and the sensitivity on the additive of the lubricating grease. Thus, the addition of alkylnaphthalenes is an innovation of the present invention.
In comparative examples 4 and 5, the weight ratio of alkyl naphthalene to the mixed base oil was 5% and 35%, respectively, and when the weight ratio of alkyl naphthalene to the mixed base oil was 5%, there was a certain improvement in the performance of the grease, but the effect was not so significant; when the alkyl naphthalene accounts for 35% by weight of the mixed base oil, the performance of the grease is substantially equivalent to that of the grease containing 30% of alkyl naphthalene, but the low-temperature performance is deteriorated because the viscosity index of alkyl naphthalene is smaller than that of PAO, and the low-temperature performance is poor, and the low-temperature performance of the grease is poor due to the excessively high addition amount. Therefore, the preferred weight percentage of the alkyl naphthalene in the mixed base oil is 10-30%, and the prepared lubricating grease has better comprehensive performance; wherein, when the alkyl naphthalene accounts for 30 percent of the mixed base oil by weight, the performance is optimal.
In contrast, in comparative example 1, the structure improver is not added, and compared with the example (such as example 7) in which the structure improver is added, the prepared grease is inferior in water resistance, because the complex lithium soap thickener has hydrophilicity, and is liable to cause poor structural stability and loss when meeting water, and the addition of the structure improver can prevent the water from damaging the soap fiber structure of the grease and improve the water resistance of the grease.
The structure improver of comparative example 2 was added in the last step of the preparation process, and compared with the example (e.g., example 1) in which the structure improver was added in the saponification stage, the prepared grease was not significant in improving water resistance and did not have a great effect in improving the structural stability of the grease, because the structure improver was simply dispersed in the grease without entering the interior of the soap fiber structure and did not form a hydrogen bond with the complex lithium soap fiber structure when the structure improver was added in the last step, thereby achieving both effective improvement of the water resistance of the complex lithium and contribution to reduction of oil separation and improvement of mechanical stability. Therefore, in the preparation step of the invention, the structure improver is added in the saponification stage, so that the prepared lubricating grease has excellent performance.
Example 8
The basic procedure is the same as in example 1, except that: 95.625kg of poly-alpha-olefin oil PAO10 and 31.875kg of alkyl naphthalene Synesstic12 are mixed to be used as mixed base oil, 8.84kg of 12-hydroxystearic acid, 2.54kg of sebacic acid and 3.92kg of lithium hydroxide oil solution.
Example 9
The basic procedure is the same as in example 1, except that: 98.34kg of poly-alpha-olefin oil PAO10 and 30.96kg of alkyl naphthalene Synessic 12 were mixed as a mixed base oil, 8.04kg of 12-hydroxystearic acid, 2.04kg of sebacic acid, and 3.42kg of lithium hydroxide oil solution.
Example 10
The basic procedure is the same as in example 1, except that: 87.84kg of poly-alpha-olefin oil PAO10 and 30.96kg of alkyl naphthalene Synessic 12 are mixed to be used as mixed base oil, 12.54kg of 12-hydroxystearic acid, 5.04kg of sebacic acid and 6.42kg of lithium hydroxide oil solution.
Example 11
The basic procedure is the same as in example 1, except that: 93.88kg of polyalphaolefin oil PAO10 and 31.46kg of alkyl naphthalene synchronous 12 were mixed as a mixed base oil without adding zinc dialkyl dithiophosphate.
Example 12
The basic procedure is the same as in example 1, except that: 92.13kg of poly-alpha-olefin oil PAO10 and 30.96kg of alkyl naphthalene Synesstic12 are mixed to be used as mixed base oil, 2.25kg of benzotriazole derivatives are added, and thiadiazole derivatives are not added.
Example 13
The basic procedure is the same as in example 1, except that: 92.13kg of poly-alpha-olefin oil PAO10 and 30.96kg of alkyl naphthalene Synesstic12 are mixed to be used as mixed base oil, 2.25kg of calcium petroleum sulfonate is added, and barium dinonyl naphthalene sulfonate is not added.
Example 14
The basic procedure is the same as in example 1, except that: mixing poly alpha olefin oil PAO1091.08kg and alkyl naphthalene Synessitic1230.96kg as mixed base oil, and adding antioxidant Irganox L572.25kg.
Example 15
The basic procedure is the same as in example 1, except that: 82.2kg of mixed base oil, 10.5kg of 12-hydroxystearic acid and 3.54kg of sebacic acid are sequentially added into a saponification reaction kettle, stirring is started, the temperature is raised to 80 ℃, then 4.92kg of lithium hydroxide oil solution is added, saponification reaction is carried out for 60 minutes at the temperature of 95-105 ℃ after the addition is finished, and then the temperature is raised to 130 ℃ and is kept for 40 minutes.
Example 16
The basic procedure is the same as in example 1, except that: 82.2kg of mixed base oil, 10.5kg of 12-hydroxystearic acid and 3.54kg of sebacic acid are sequentially added into a saponification reaction kettle, and stirring is started and the temperature is raised to 85 ℃.
The lubricating grease prepared in the examples 8 to 16 is tested, and the detection result shows that all performances of the prepared lubricating grease reach the standard. The lubricating grease prepared by the invention has high dropping point, excellent high and low temperature properties, excellent mechanical stability and good extreme pressure wear resistance, is suitable for various lubricating occasions requiring high and low temperature resistance and extreme pressure wear resistance, such as the fields of automobile hub bearings, constant velocity universal joints, high temperature bearings and the like, and can prolong the grease replacement period.
Claims (1)
1. A preparation method of extreme pressure grease with high and low temperature resistance and long service life is characterized by comprising the following steps: mixing poly alpha olefin oil PAO 1086.84 kg and alkyl naphthalene Synessitic1235.5 kg as mixed base oil, wherein the kinematic viscosity of the mixed base oil at 40 ℃ is 78mm2s, viscosity index is 123, 82.2kg of mixed base oil, 10.5kg of 12-hydroxystearic acid and 3.54kg of sebacic acid are sequentially added into a saponification reaction kettle, stirring is started, the temperature is raised to 82 ℃, then adding 4.92kg of lithium hydroxide oil solution, carrying out saponification reaction for 90 minutes at 95-105 ℃ after the addition is finished, heating to 135 ℃ and preserving heat for 30 minutes, adding an antioxidant Irganox L570.45 kg and a structure improving agent Lubrizol2002D 2.25kg, continuously heating to 215 ℃ and preserving heat for 5 minutes, finally transferring the materials to a blending kettle, adding the rest mixed base oil 40.14kg and reducing the temperature, sequentially adding molybdenum dialkyl dithiocarbamate 1.5kg, zinc dialkyl dithiophosphate 1.5kg, thiadiazole derivative 1.5kg and barium dinonylnaphthalene sulfonate 1.5kg when the temperature is reduced to 90 ℃, uniformly stirring and mixing, and grinding and dispersing by a three-roll grinder to obtain the finished product.
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| CN108485760B (en) * | 2018-04-27 | 2020-07-03 | 中国石油化工股份有限公司 | Lubricating grease composition and preparation method thereof |
| US20190382680A1 (en) * | 2018-06-18 | 2019-12-19 | Exxonmobil Research And Engineering Company | Formulation approach to extend the high temperature performance of lithium complex greases |
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| CN111979024A (en) * | 2020-08-20 | 2020-11-24 | 中国石油化工股份有限公司 | Light hammer lubricating grease composition and preparation method and application thereof |
| CN114369487A (en) * | 2022-01-14 | 2022-04-19 | 中海油气(泰州)石化有限公司 | High-temperature-resistant long-life lubricating grease and preparation method thereof |
| CN115491244A (en) * | 2022-10-07 | 2022-12-20 | 东莞市摩得力润滑材料有限公司 | Shock-absorbing wear-resistant high-temperature lubricating grease composition and preparation method thereof |
| CN115851340B (en) * | 2022-11-10 | 2024-02-09 | 江苏龙蟠科技股份有限公司 | Preparation method of high-dropping-point single-lithium soap lubricating grease |
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