CN111961518B - Composite calcium sulfonate-based lubricating grease for open gears and preparation method and application thereof - Google Patents
Composite calcium sulfonate-based lubricating grease for open gears and preparation method and application thereof Download PDFInfo
- Publication number
- CN111961518B CN111961518B CN202010902519.4A CN202010902519A CN111961518B CN 111961518 B CN111961518 B CN 111961518B CN 202010902519 A CN202010902519 A CN 202010902519A CN 111961518 B CN111961518 B CN 111961518B
- Authority
- CN
- China
- Prior art keywords
- calcium
- sulfonate
- calcium sulfonate
- lubricating grease
- open gear
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Classifications
-
- 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
-
- 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
- C10M177/00—Special methods of preparation of lubricating compositions; Chemical modification by after-treatment of components or of the whole of a lubricating composition, not covered by other classes
-
- 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
- C10M2201/04—Elements
- C10M2201/041—Carbon; Graphite; Carbon black
-
- 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
- C10M2203/1006—Petroleum or coal fractions, e.g. tars, solvents, bitumen 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
- 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
- C10M2205/022—Ethene
-
- 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
- C10M2205/022—Ethene
- C10M2205/0225—Ethene 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
- 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
- C10M2205/024—Propene
-
- 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
- C10M2205/024—Propene
- C10M2205/0245—Propene used as base material
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2215/00—Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
- C10M2215/02—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
-
- 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
- C10M2219/02—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
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2219/00—Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions
- C10M2219/04—Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions containing sulfur-to-oxygen bonds, i.e. sulfones, sulfoxides
- C10M2219/044—Sulfonic acids, Derivatives thereof, e.g. neutral salts
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- 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
- C10M2219/0445—Sulfonic acids, Derivatives thereof, e.g. neutral salts 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
- 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
- C10M2219/046—Overbasedsulfonic acid salts
- C10M2219/0466—Overbasedsulfonic acid salts used as thickening agents
Abstract
The invention provides a composite calcium sulfonate-based lubricating grease for an open gear, and a preparation method and application thereof, and belongs to the technical field of lubricating grease preparation. The invention provides a composite calcium sulfonate-based lubricating grease for an open gear, which comprises the following components in percentage by mass: 67-72% of base oil, 11-15% of composite calcium sulfonate thickening agent, 4.5-6.0% of extreme pressure antiwear additive, 1.5-3% of ethylene propylene rubber, 0.4-0.5% of diphenylamine and 10-12% of graphite, wherein the sum of the mass percentages of the components is 100%; the extreme pressure antiwear additive comprises sulfurized olefin and calcium petroleum sulfonate; the compound calcium sulfonate is prepared from the following raw materials by phase inversion reaction: high base number calcium petroleum sulfonate, isopropanol, calcium carbonate, glacial acetic acid and dodecyl benzene sulfonic acid. The compound calcium sulfonate-based lubricating grease for the open gear has excellent extreme pressure performance and temperature resistance.
Description
Technical Field
The invention belongs to the technical field of lubricating grease preparation, and particularly relates to a calcium sulfonate complex type lubricating grease for an open gear, and a preparation method and application thereof.
Background
The tooth surface processing precision of the open gear is relatively low, the roughness is large, the open gear is in a heavy load and continuous working state for a long time, in addition, the working environment is severe, the gear lubricant is often in a working condition of large load or impact load, the gear lubricant lacks sealing protection, external media such as dust, impurities and water easily pollute the tooth surface of the engaged gear, and the open gear lubricant is required to have excellent performances of friction reduction, wear resistance, pitting corrosion resistance and extreme pressure resistance, and simultaneously has the characteristics of low toxicity, no smell and environmental friendliness.
Lithium-based and aluminum complex-based greases are generally used in current conventional open gear greases, and these greases have the disadvantages of poor extreme pressure resistance and poor temperature resistance. For example, chinese invention CN103045334A discloses an open gear grease, which comprises the following components: 50-90 parts of base oil and 4-10 parts of thickening agent; 1-3 parts by weight of an antioxidant; 1-5 parts of an extreme pressure antiwear agent; 1-5 parts of a solid antiwear agent; 10-20 parts of adhesive. The open gear lubricating grease provided by the invention has the advantages of simple components and low cost, and also has strong adhesion capability, excellent lubricity and good oil saving property, but has poor extreme pressure property, small (four-ball method) sintering load (PD value) of 6100-7000N (622-714 kg), poor temperature resistance and a dropping point of 164-173 ℃.
Disclosure of Invention
In view of the above, the present invention aims to provide a composite calcium sulfonate-based lubricating grease for an open gear, a preparation method thereof and an application thereof. The compound calcium sulfonate-based lubricating grease for the open gear has excellent extreme pressure resistance and temperature resistance, has high sintering load (PD value), and can bear heavy load.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a composite calcium sulfonate-based lubricating grease for an open gear, which comprises the following components in percentage by mass:
67-72% of base oil, 11-15% of composite calcium sulfonate thickening agent, 4.5-6.0% of extreme pressure antiwear additive, 1.5-3% of ethylene propylene rubber, 0.4-0.5% of diphenylamine and 10-12% of graphite, wherein the sum of the mass percentages of the components is 100%;
the extreme pressure antiwear additive comprises sulfurized olefin and calcium petroleum sulfonate, wherein the mass ratio of the sulfurized olefin to the calcium petroleum sulfonate is (3-4): 1.0 to 1.5; the sulfur content of the sulfurized olefin is 35-36 wt%; the calcium content of the petroleum calcium sulfonate is 14.5-16.5 wt%;
the composite calcium sulfonate thickener is prepared from the following raw materials through phase inversion reaction: high base number calcium petroleum sulfonate, isopropanol, calcium carbonate, glacial acetic acid and dodecylbenzene sulfonic acid;
the mass ratio of the high-base number petroleum calcium sulfonate to the isopropanol to the calcium carbonate to the glacial acetic acid to the dodecylbenzene sulfonic acid is 10-13.5: 0.3-0.4: 0.2-0.3: 0.15-0.25: 0.3 to 0.4; the base number of the high-base-number calcium petroleum sulfonate is 395-430.
Preferably, the viscosity of the base oil at 40 ℃ is 3000-4000 cst, the pour point is lower than-15 ℃, and the flash point is higher than 280 ℃.
Preferably, the base oil is a mixture of 150BS bright stock and polyethylene propylene synthetic oil, and the mass ratio of the 150BS bright stock to the polyethylene propylene synthetic oil is 4-6: 5 to 6.
Preferably, the 150BS bright stock has the viscosity of 28-32 cst at 100 ℃, the pour point of less than-15 ℃ and the flash point of more than 280 ℃.
Preferably, the polyethylene propylene synthetic oil has a viscosity of 2000cst at 100 ℃, a pour point below-10 ℃ and a flash point above 280 ℃.
Preferably, the particle size of the graphite is 10-13 μm.
Preferably, the particle size of the lubricating grease for the compound calcium sulfonate-based open gear is 120-150 meshes.
The invention also provides a preparation method of the lubricating grease for the compound calcium sulfonate-based open gear, which comprises the following steps:
mixing the composite calcium sulfonate thickener with part of base oil, and carrying out phase inversion reaction to obtain a phase inversion reaction product;
mixing the phase inversion reaction product, the ethylene propylene rubber and the residual base oil to obtain a mixed material;
and filtering the mixed material, carrying out first cooling, shearing reflux and second cooling in sequence, and mixing with diphenylamine, sulfurized olefin, calcium petroleum sulfonate and graphite to obtain the composite calcium sulfonate-based lubricating grease for the open gear.
Preferably, the temperature of the reflux shearing is 130-140 ℃, the pressure is 0.5-0.7 MPa, and the time is 30-90 min.
The invention also provides application of the lubricating grease for the compound calcium sulfonate-based open gear in the technical scheme or the lubricating grease for the compound calcium sulfonate-based open gear prepared by the preparation method in lubrication of an open gear machine, a crusher, a vibrating screen, a tooth type coupler and a chain, and leakage prevention and sealing of a heavy-load gear box.
The invention provides a composite calcium sulfonate-based lubricating grease for an open gear, which comprises the following components in percentage by mass: 67-72% of base oil, 11-15% of composite calcium sulfonate thickening agent, 4.5-6.0% of extreme pressure antiwear additive, 1.5-3% of ethylene propylene rubber, 0.4-0.5% of diphenylamine and 10-12% of graphite, wherein the sum of the mass percentages of the components is 100%; the extreme pressure antiwear additive comprises sulfurized olefin and calcium petroleum sulfonate, wherein the mass ratio of the sulfurized olefin to the calcium petroleum sulfonate is (3-4): 1.0 to 1.5; the sulfur content of the sulfurized olefin is 35-36 wt%; the calcium content of the petroleum calcium sulfonate is 14.5-16.5 wt%; the composite calcium sulfonate thickener is prepared from the following raw materials through phase inversion reaction: high base number calcium petroleum sulfonate, isopropanol, calcium carbonate, glacial acetic acid and dodecylbenzene sulfonic acid; the mass ratio of the high-base number petroleum calcium sulfonate to the isopropanol to the calcium carbonate to the glacial acetic acid to the dodecylbenzene sulfonic acid is 10-13.5: 0.3-0.4: 0.2-0.3: 0.15-0.25: 0.3 to 0.4; the base number of the high-base-number calcium petroleum sulfonate is 395-430. In the invention, sulfurized olefin with high sulfur content and calcium petroleum sulfonate with high calcium content have excellent extreme pressure performance, and the extreme pressure performance of the sulfurized olefin with high sulfur content and the calcium petroleum sulfonate with high calcium content are complementary by a specific proportion; the composite calcium sulfonate has good extreme pressure resistance and dropping point characteristics, and is matched with base oil, ethylene propylene rubber, diphenylamine and graphite with specific dosage, so that the sintering load (PD value) and the dropping point value of the lubricating grease are greatly improved.
Meanwhile, the composite calcium sulfonate-based lubricating grease for the open gear has excellent extreme pressure anti-wear performance, water resistance, rust resistance, mechanical stability and impact load resistance, and can be used for lubricating open gear machines, crushers, vibrating screens, tooth type couplings and chains in large-amount water showering, high-temperature, low-speed and heavy-load environments in cement, mines, electric power and metallurgical industries, and preventing leakage and sealing of heavy-load gear boxes.
Detailed Description
The invention provides a composite calcium sulfonate-based lubricating grease for an open gear, which comprises the following components in percentage by mass:
67-72% of base oil, 11-15% of composite calcium sulfonate thickening agent, 4.5-6.0% of extreme pressure antiwear additive, 1.5-3% of ethylene propylene rubber, 0.4-0.5% of diphenylamine and 10-12% of graphite, wherein the sum of the mass percentages of the components is 100%.
In the invention, the particle size of the composite calcium sulfonate-based lubricating grease for the open gear is preferably 120-150 meshes.
In the present invention, unless otherwise specified, the starting materials used are all those conventionally available commercially in the art or prepared by methods well known to those skilled in the art.
The composite calcium sulfonate based lubricating grease for the open gear comprises 67-72% of base oil by mass percentage, and preferably 69-71%. In the invention, the viscosity of the base oil at 40 ℃ is preferably 3000-4000 cst; the pour point of the base oil is preferably below-15 ℃; the flash point of the base oil is preferably above 280 ℃. In the invention, the base oil preferably comprises 150BS bright stock and polyethylene propylene synthetic oil, and the mass ratio of the 150BS bright stock to the polyethylene propylene synthetic oil is preferably 4-6: 5 to 6, and more preferably 4.5 to 5.5:5.2 to 5.8. In the invention, the viscosity of the 150BS bright stock at 100 ℃ is 28-32 cst; the 150BS bright stock has a pour point of less than-15 ℃; flash point 280 of the 150BS bright stock. In the invention, the polyethylene propylene synthetic oil is 1-propylene and ethylene polymer synthetic oil, and the viscosity of the polyethylene propylene synthetic oil at 100 ℃ is 2000 cst; the pour point of the polyethylene propylene synthetic oil is lower than-10 ℃; the polyethylene propylene synthetic oil has a flash point of 280. In the present invention, the 150BS bright stock is preferably purchased from oil companies. In the present invention, the polyethylene propylene synthetic oil is preferably HC 2000; the polyethylene propylene synthetic oil is preferably purchased from petroleum companies. In the invention, the base oil has higher viscosity and large oil film thickness, and can bear higher bearing capacity.
The lubricating grease for the compound calcium sulfonate-based open gear comprises, by mass, 11-15% of a compound calcium sulfonate thickening agent, and preferably 12-14%. In the invention, the composite calcium sulfonate thickener is prepared by carrying out phase inversion reaction on the following raw materials: high base number calcium petroleum sulfonate, isopropanol, calcium carbonate, glacial acetic acid and dodecyl benzene sulfonic acid. In the specific embodiment of the present invention, the composite calcium sulfonate thickener is preferably prepared by subjecting high base number calcium petroleum sulfonate, isopropanol, calcium carbonate, glacial acetic acid, and dodecylbenzene sulfonic acid to a phase inversion reaction in the presence of a base oil, that is, a preparation process of a phase inversion reaction product obtained by the preparation method according to the following technical scheme, and the specific process is as follows: mixing part of base oil and high-base number calcium petroleum sulfonate in a reaction kettle, mixing with an isopropanol aqueous solution and calcium carbonate at 65-70 ℃, mixing with a glacial acetic acid aqueous solution at 75 ℃ for the third time, performing a first phase inversion reaction, mixing with dodecylbenzene sulfonic acid at 80-85 ℃ for the fourth time after the reaction is performed for 5-10 min, performing a second phase inversion reaction at 90-100 ℃, and reacting for 30-40 min to obtain a phase inversion reaction product.
In the invention, the mixing mode of the dodecylbenzene sulfonic acid is preferably linear mixing, and the linear mixing speed is preferably 2-2.5 kg/min.
In the present invention, the first mixing, the second mixing, the third mixing and the fourth mixing are independently preferably mechanically agitated; the rotation speed of the mechanical stirring is preferably 30-50 rpm independently.
The second phase inversion reaction is preferably carried out until the material is thickened to be in a semi-solid state and smooth, so that a phase inversion reaction product is obtained.
In the invention, the mass ratio of the high-base number petroleum calcium sulfonate, the isopropanol, the calcium carbonate, the glacial acetic acid and the dodecylbenzene sulfonic acid is 10-13.5: 0.3-0.4: 0.2-0.3: 0.15-0.25: 0.3 to 0.4, preferably 10.5 to 13: 0.33 to 0.37: 0.22-0.27: 0.17-0.23: 0.33 to 0.37. In the invention, the base number of the high-base-number petroleum calcium sulfonate is 395-430, and the calcium content of the high-base-number petroleum calcium sulfonate is preferably 15-16 wt%; the high base number calcium petroleum sulfonate is preferably T106D. In the invention, the particle size of the nano calcium carbonate is preferably 10-13 μm. In the invention, the mass percentage of the isopropanol in the isopropanol aqueous solution is preferably 30 wt%; the mass percentage of the glacial acetic acid in the glacial acetic acid aqueous solution is preferably 20 wt%.
The lubricating grease for the compound calcium sulfonate-based open gear comprises, by mass, 4.5-6.0% of extreme pressure antiwear additive, preferably 4.5-5.0%. In the present invention, the extreme pressure antiwear additive includes sulfurized olefin and calcium petroleum sulfonate; the mass ratio of the sulfurized olefin to the petroleum calcium sulfonate is 3-4: 1.0 to 1.5, preferably 3 to 4:1.2 to 1.4. In the present invention, the sulfur content of the sulfurized olefin is 35 to 36 wt%; the calcium content of the petroleum calcium sulfonate is 15-16 wt%. In the invention, sulfurized olefin with high sulfur content and calcium petroleum sulfonate with high calcium content have excellent extreme pressure performance, and the extreme pressure performance of the sulfurized olefin with high sulfur content and the calcium petroleum sulfonate with high calcium content are supplemented by a specific proportion. In the present invention, the sulfurized olefin and calcium petroleum sulfonate are both preferably purchased from lubosun additives, the sulfurized olefin is preferably 5340 sulfurized olefin; the calcium petroleum sulfonate is preferably 75GR calcium petroleum sulfonate, so that the extreme pressure performance is excellent, and the corrosion resistance of the composite calcium sulfonate-based lubricating grease for the open gear can be improved.
The composite calcium sulfonate-based lubricating grease for the open gear comprises 1.5-3% of ethylene propylene rubber by mass percentage, and preferably 1.5-2.5%. In the invention, the ethylene-propylene rubber has excellent temperature resistance and mechanical stability.
The composite calcium sulfonate-based lubricating grease for the open gear comprises 0.4-0.5% of diphenylamine by mass percentage, and preferably 0.42-0.47%. In the present invention, diphenylamine has excellent oxidation resistance.
The composite calcium sulfonate based lubricating grease for the open gear comprises 0.3-0.5% of methylbenzotrinitrogen in percentage by mass
Preferably 0.35 to 0.45%. In the present invention, the methylbenzotrinitrogen
Preferably liquid methylbenzotriazone
Lubricating grease beneficial to uniform dispersion in composite calcium sulfonate-based open gearIn (1). In the present invention, methylbenzotrinitrogens
The antirust performance of the composite calcium sulfonate-based lubricating grease for the open gear on nonferrous metals can be improved.
The composite calcium sulfonate-based lubricating grease for the open gear comprises, by mass, 10-12% of graphite, and preferably 10.2-10.7%. In the present invention, the particle size of the graphite is preferably 10 to 13 μm. In the invention, the superfine graphite powder can enable the composite calcium sulfonate-based lubricating grease for the open gear to be used under the conditions of high temperature, high pressure, high load and impact load.
The invention also provides a preparation method of the lubricating grease for the compound calcium sulfonate-based open gear, which comprises the following steps:
mixing the composite calcium sulfonate thickener with part of base oil, and carrying out phase inversion reaction to obtain a phase inversion reaction product;
mixing the phase inversion reaction product, the ethylene propylene rubber and the residual base oil to obtain a mixed material;
and filtering the mixed material, carrying out first cooling, shearing reflux and second cooling in sequence, and mixing with diphenylamine, sulfurized olefin, calcium petroleum sulfonate and graphite to obtain the composite calcium sulfonate-based lubricating grease for the open gear.
The invention mixes the compound calcium sulfonate thickener with part of base oil to carry out phase inversion reaction, thus obtaining a phase inversion reaction product. In the invention, the composite calcium sulfonate thickener is prepared in situ, and in the specific embodiment of the invention, the composite calcium sulfonate thickener is prepared by carrying out phase inversion reaction on the following raw materials: high base number calcium petroleum sulfonate, isopropanol, calcium carbonate, glacial acetic acid and dodecylbenzene sulfonic acid; the specific process is consistent with the above scheme, and is not described in detail here.
In the present invention, the mass of the part of the base oil is preferably 1/2 of the total mass of the base oil. After the phase inversion reaction product is obtained, the phase inversion reaction product, the ethylene propylene rubber and the residual base oil are mixed to obtain a mixed material.
In the specific embodiment of the invention, the phase inversion reaction product is preferably subjected to heat preservation for 60-70 min at the temperature of 95-105 ℃, then subjected to heat preservation for 30-40 min at the temperature of 130-140 ℃, and then mixed with the rest of the base oil and the ethylene propylene rubber at the temperature of 170-180 ℃ to obtain the mixed material. According to the invention, the temperature is preferably raised and the mechanical stirring is carried out at the same time, and the speed of the mechanical stirring is preferably 40-70 rpm. In the present invention, the mixing is preferably performed by mechanical stirring; the rotation speed of the mechanical stirring is preferably 40-70 rpm.
In the present invention, the mass of the remaining base oil is preferably 1/2 of the total mass of the base oil.
After the mixed material is obtained, the mixed material is sequentially filtered, subjected to first cooling, shearing reflux and second cooling, and then mixed with diphenylamine, sulfurized olefin, calcium petroleum sulfonate and graphite to obtain the composite calcium sulfonate-based lubricating grease for the open gear.
In the specific embodiment of the invention, the mixed material is preferably subjected to filtration, first cooling, shearing reflux and second cooling in sequence at 198-203 ℃.
In the invention, the filtration mode is preferably metal mesh filtration, and the pore diameter of the metal mesh is preferably 120-150 meshes.
In the present invention, the temperature of the first cooling is preferably 130 to 140 ℃, and the cooling rate of the first cooling to the temperature of the first cooling is not particularly limited, and may be a cooling rate known to those skilled in the art. The first cooling method of the present invention is not particularly limited, and a cooling method known to those skilled in the art may be used.
In the invention, the pressure of the reflux shearing is preferably 0.5-0.7 MPa; the time of the reflux shearing is preferably 30-90 min. The mode of the reflux shear is not particularly limited in the present invention, and a reflux shear known to those skilled in the art may be used.
In the invention, the temperature of the second cooling is preferably less than or equal to 90 ℃, and more preferably 80-90 ℃. The temperature reduction rate of the temperature reduction to the second cooling temperature is not particularly limited in the present invention, and a temperature reduction rate well known to those skilled in the art may be adopted. The second cooling method is not particularly limited in the present invention, and a cooling method known to those skilled in the art may be used.
The mixing sequence of the second cooled product, diphenylamine, sulfurized olefin, high-calcium petroleum sulfonate and graphite is not particularly limited, and any mixing sequence can be adopted.
After the lubricating grease for the composite calcium sulfonate-based open gear is obtained, the lubricating grease for the composite calcium sulfonate-based open gear is preferably sampled and inspected, and after the lubricating grease is qualified, the lubricating grease is sequentially filtered and packaged.
The invention also provides application of the lubricating grease for the compound calcium sulfonate-based open gear in the technical scheme or the lubricating grease for the compound calcium sulfonate-based open gear prepared by the preparation method in lubrication of an open gear machine, a crusher, a vibrating screen, a tooth type coupler and a chain, and leakage prevention and sealing of a heavy-load gear box.
The mode of application of the present invention is not particularly limited, and may be any mode of application known to those skilled in the art.
The grease for a complex calcium sulfonate-based open gear of the present invention, the preparation method and the application thereof will be described in detail with reference to the following examples, but they should not be construed as limiting the scope of the present invention.
Examples 1 to 3
According to the dosage of the raw materials in the table 1, the lubricating grease for the compound calcium sulfonate-based open gear is prepared, and the preparation method comprises the following steps:
(1) mixing 150BS bright stock and polyethylene propylene synthetic oil to obtain base oil;
(2) mixing isopropanol with part of water to obtain an isopropanol aqueous solution, wherein the mass ratio of the isopropanol to the part of water is 3: 7;
mixing glacial acetic acid and residual water to obtain a glacial acetic acid aqueous solution, wherein the mass ratio of the glacial acetic acid to the residual water is 1: 3;
adding part of base oil and high-base number calcium petroleum sulfonate T106D into a saponification kettle, stirring and heating to 70 ℃, then rotating at 30rpm, adding an isopropanol aqueous solution and calcium carbonate, heating to 75 ℃ while stirring, adding a glacial acetic acid aqueous solution, carrying out a first phase inversion reaction, after 5min and heating to 80 ℃, linearly adding dodecylbenzene sulfonic acid, wherein the rate of adding the dodecylbenzene sulfonic acid is 2kg/min, heating to 100 ℃, carrying out a second phase inversion reaction, and after 30min, thickening and smoothing the material to obtain a phase inversion reaction product;
(3) heating the phase-inversion reaction product to 105 ℃, accelerating stirring, keeping the rotation speed at 70rpm for 60min, continuing to heat to 140 ℃, keeping the temperature for 30min, continuing to heat to 175 ℃, and mixing with the rest base oil and the ethylene propylene rubber to obtain a mixed material, wherein the mass ratio of part of the base oil to the rest base oil is 1: 1;
(4) and (2) heating the mixed material to 203 ℃, moving the mixed material to a kettle, filtering and cooling the mixed material by using a 120-mesh metal net, cooling the mixed material to 140 ℃, performing reflux shearing, keeping the pressure of the reflux shearing at 0.5MPa, continuously cooling the mixed material to below 90 ℃ after 30min, uniformly stirring the mixed material, diphenylamine, olefin sulfide, high-calcium petroleum calcium sulfonate and graphite, sampling, inspecting and packaging the mixture by using a 120-mesh filter after the mixture is qualified, thus obtaining the composite calcium sulfonate-based lubricating grease for the open gear.
The performance of the lubricating grease for a complex calcium sulfonate-based type open gear prepared in examples 1 to 3 was examined according to the criteria in table 2, and the results are shown in table 2.
Comparative example 1
This comparative example differs from example 1 in the amount of olefin sulfide and calcium petroleum sulfonate used in the feed, and the specific amounts of feed used are shown in Table 1.
The grease prepared in comparative example 1 was tested for properties according to the criteria in table 2, and the results are shown in table 2.
Comparative example 2
This comparative example differs from example 1 in that no sulfurized olefin is used in the feed and the specific amounts of calcium petroleum sulfonate and other feed materials used are shown in table 1.
The grease prepared in comparative example 1 was tested for properties according to the criteria in table 2, and the results are shown in table 2.
TABLE 1 amount of raw materials used in examples 1 to 3 and comparative examples 1 to 2
| Raw materials (kg) | Example 1 | Example 2 | Example 3 | Comparative example 1 | Comparative example 2 |
| High base number calcium sulfonate T106D | 115 | 120 | 125 | 120 | 120 |
| Isopropanol (I-propanol) | 3.4 | 3.6 | 3.8 | 3.6 | 3.6 |
| Water (W) | 5.7 | 5.7 | 5.7 | 5.7 | 5.7 |
| Nano calcium carbonate | 2.1 | 2.4 | 2.6 | 2.4 | 2.4 |
| Glacial acetic acid | 1.7 | 1.8 | 1.9 | 1.8 | 1.8 |
| Dodecyl benzene sulfonic acid | 3.4 | 3.6 | 3.8 | 3.6 | 3.6 |
| 150BS bright stock | 355 | 283 | 310 | 306 | 328 |
| Polyethylene propylene synthetic oil HC2000 | 355 | 416 | 388 | 416 | 416 |
| Sulfurized olefin 5340 | 30 | 30 | 30 | 15 | -- |
| High calcium sulfonate 75GR | 15 | 15 | 15 | 7 | -- |
| Ethylene propylene rubber | 15 | 20 | 15 | 20 | 20 |
| Graphite | 100 | 100 | 100 | 100 | 100 |
TABLE 2 Properties of greases prepared in examples 1 to 3 and comparative examples 1 to 2
The data analysis shows that the compound calcium sulfonate-based open gear lubricating grease provided by the invention has excellent dropping point and bearing capacity, and excellent wear resistance, water resistance, rust resistance, mechanical stability and impact load resistance.
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 (7)
1. The composite calcium sulfonate-based lubricating grease for the open gear comprises the following components in percentage by mass:
67-72% of base oil, 11-15% of composite calcium sulfonate thickening agent, 4.5-6.0% of extreme pressure antiwear additive, 1.5-3% of ethylene propylene rubber, 0.4-0.5% of diphenylamine and 10-12% of graphite, wherein the sum of the mass percentages of the components is 100%;
the extreme pressure antiwear additive comprises sulfurized olefin and calcium petroleum sulfonate, wherein the mass ratio of the sulfurized olefin to the calcium petroleum sulfonate is (3-4): 1.0 to 1.5; the sulfur content of the sulfurized olefin is 35-36 wt%; the calcium content of the petroleum calcium sulfonate is 14.5-16.5 wt%;
the composite calcium sulfonate thickener is prepared from the following raw materials through phase inversion reaction: high base number calcium petroleum sulfonate, isopropanol, calcium carbonate, glacial acetic acid and dodecylbenzene sulfonic acid;
the mass ratio of the high-base number petroleum calcium sulfonate to the isopropanol to the calcium carbonate to the glacial acetic acid to the dodecylbenzene sulfonic acid is 10-13.5: 0.3-0.4: 0.2-0.3: 0.15-0.25: 0.3 to 0.4; the base number of the high-base-number calcium petroleum sulfonate is 395-430;
the base oil is a mixture of 150BS bright stock and polyethylene propylene synthetic oil, and the mass ratio of the 150BS bright stock to the polyethylene propylene synthetic oil is 4-6: 5-6;
the 100 ℃ viscosity of the polyethylene propylene synthetic oil is 2000cst, the pour point is lower than-15 ℃, and the flash point is higher than 280 ℃;
the particle size of the graphite is 10-13 mu m.
2. The lubricating grease for the compound calcium sulfonate-based open gear according to claim 1, wherein the base oil has a viscosity at 40 ℃ of 3000-4000 cst, a pour point of less than-15 ℃ and a flash point of more than 280 ℃.
3. The lubricating grease for the compound calcium sulfonate-based open gear according to claim 1, wherein the 150BS bright stock has a viscosity of 28-32 cst at 100 ℃, a pour point lower than-15 ℃ and a flash point higher than 280 ℃.
4. The lubricating grease for a complex calcium sulfonate-based open gear according to claim 1, wherein the particle size of the lubricating grease for a complex calcium sulfonate-based open gear is 120 to 150 mesh.
5. The method for producing a lubricating grease for a complex calcium sulfonate-based open gear according to any one of claims 1 to 4, comprising the steps of:
mixing the composite calcium sulfonate thickener with part of base oil, and carrying out phase inversion reaction to obtain a phase inversion reaction product;
mixing the phase inversion reaction product, the ethylene propylene rubber and the residual base oil to obtain a mixed material;
and filtering the mixed material, carrying out first cooling, shearing reflux and second cooling in sequence, and mixing with diphenylamine, sulfurized olefin, calcium petroleum sulfonate and graphite to obtain the composite calcium sulfonate-based lubricating grease for the open gear.
6. The preparation method according to claim 5, wherein the temperature of the reflux shearing is 130-140 ℃, the pressure is 0.5-0.7 MPa, and the time is 30-90 min.
7. Use of the grease for a complex calcium sulfonate-based open gear according to any one of claims 1 to 4 or the grease for a complex calcium sulfonate-based open gear prepared by the preparation method according to claim 5 or 6 in lubrication of an open gear machine, a crusher, a vibrating screen, a tooth type coupler and a chain, and leakage prevention and sealing of a heavy-duty gear box.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010902519.4A CN111961518B (en) | 2020-09-01 | 2020-09-01 | Composite calcium sulfonate-based lubricating grease for open gears and preparation method and application thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010902519.4A CN111961518B (en) | 2020-09-01 | 2020-09-01 | Composite calcium sulfonate-based lubricating grease for open gears and preparation method and application thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN111961518A CN111961518A (en) | 2020-11-20 |
| CN111961518B true CN111961518B (en) | 2022-02-15 |
Family
ID=73400191
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202010902519.4A Active CN111961518B (en) | 2020-09-01 | 2020-09-01 | Composite calcium sulfonate-based lubricating grease for open gears and preparation method and application thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN111961518B (en) |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101787324B (en) * | 2010-02-03 | 2013-09-11 | 上海禾泰特种润滑技术有限公司 | Heavy duty gear lubricant and preparation method thereof |
| MX349575B (en) * | 2011-10-31 | 2017-07-28 | Nch Corp | Calcium hydroxyapatite based calcium sulfonate grease compositions and method of manufacture. |
| CN102634400B (en) * | 2012-03-31 | 2014-11-26 | 江苏龙蟠科技股份有限公司 | High-performance calcium sulfonate complex grease and preparation method thereof |
| CN105255561A (en) * | 2015-10-15 | 2016-01-20 | 安徽中天石化股份有限公司 | Lubricating grease dedicated to blender mixer and preparation method of lubricating grease |
-
2020
- 2020-09-01 CN CN202010902519.4A patent/CN111961518B/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| CN111961518A (en) | 2020-11-20 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107312598B (en) | Low-temperature overweight load synthetic gear oil | |
| CN107828473B (en) | High-low temperature resistant long-life extreme pressure lubricating grease and preparation method thereof | |
| CN107312597B (en) | Triple composite film wear-resistant energy-saving engine oil | |
| CN101200670A (en) | Composite lithium-base grease and method for making same | |
| CN102690716A (en) | Multifunctional superstrong extreme pressure antiwear lubricating grease and preparation method thereof | |
| CN102627997A (en) | High-temperature extreme-pressure bentonite grease lubricant | |
| CN102604715A (en) | Composite lithium based lubricating grease composition and its preparation method | |
| CN112521997A (en) | Lubricating grease composition for metallurgical sintering machine and preparation method thereof | |
| CN103409208A (en) | Blower main shaft bearing lubricating grease and preparation method thereof | |
| CN112961724A (en) | Extreme pressure antiwear agent and preparation method thereof | |
| CN109233959A (en) | A kind of automobile hub bearing lubricant composition and preparation method thereof | |
| RU2717349C2 (en) | Lubricating composition | |
| CN102746925A (en) | Grease used specially for concrete pump truck and preparation method thereof | |
| CN111961518B (en) | Composite calcium sulfonate-based lubricating grease for open gears and preparation method and application thereof | |
| CN102703177B (en) | Lubricating grease special for outer ball cage of automotive universal joint and preparation method for lubricating grease | |
| CN108865350A (en) | A kind of exposed gear quasi-hydrodynamic lubrication oil/fat composition | |
| CN112646639A (en) | Low-odor lubricating grease and preparation method thereof | |
| CN114426898B (en) | Lubricating grease compound additive and lubricating grease composition prepared from same | |
| CN111944590B (en) | Synthetic high-sintering load lubricating grease and preparation method and application thereof | |
| CN104726173A (en) | Lubricating grease composition produced by utilizing reclaimed oil | |
| CN111876221B (en) | Lubricating grease for roller press and preparation method and application thereof | |
| CN110776980B (en) | Chain high-low temperature lubricating grease and preparation method and application thereof | |
| CN114231338A (en) | Ultrahigh-temperature anti-stress paste and preparation method thereof | |
| CN111334363A (en) | Energy-saving antifriction lithium-based lubricating grease and preparation method thereof | |
| CN105861123A (en) | Gear oil composition and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |