CN116064185A - Method for preparing lubricating grease and application thereof - Google Patents

Method for preparing lubricating grease and application thereof Download PDF

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Publication number
CN116064185A
CN116064185A CN202111269492.0A CN202111269492A CN116064185A CN 116064185 A CN116064185 A CN 116064185A CN 202111269492 A CN202111269492 A CN 202111269492A CN 116064185 A CN116064185 A CN 116064185A
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China
Prior art keywords
calcium
sulfonic acid
carboxylate
base oil
grease
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CN202111269492.0A
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Chinese (zh)
Inventor
杨海宁
姚立丹
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Sinopec Research Institute of Petroleum Processing
China Petroleum and Chemical Corp
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Sinopec Research Institute of Petroleum Processing
China Petroleum and Chemical Corp
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Priority to CN202111269492.0A priority Critical patent/CN116064185A/en
Publication of CN116064185A publication Critical patent/CN116064185A/en
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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
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M115/00—Lubricating compositions characterised by the thickener being a non-macromolecular organic compound other than a carboxylic acid or salt thereof
    • C10M115/10—Lubricating compositions characterised by the thickener being a non-macromolecular organic compound other than a carboxylic acid or salt thereof containing sulfur
    • 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
    • C10M123/00—Lubricating compositions characterised by the thickener being a mixture of two or more compounds covered by more than one of the main groups C10M113/00 - C10M121/00, each of these compounds being essential
    • C10M123/02—Lubricating compositions characterised by the thickener being a mixture of two or more compounds covered by more than one of the main groups C10M113/00 - C10M121/00, each of these compounds being essential at least one of them being a non-macromolecular compound
    • 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
    • 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
    • C10M2205/0206—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions containing acyclic monomers used as base material
    • 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
    • C10M2207/121—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of seven or less carbon atoms
    • C10M2207/122—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of seven or less carbon atoms monocarboxylic
    • C10M2207/1225—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of seven or less carbon atoms monocarboxylic used as thickening agent
    • 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
    • C10M2207/121—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of seven or less carbon atoms
    • C10M2207/123—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of seven or less carbon atoms polycarboxylic
    • C10M2207/1236—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of seven or less carbon atoms polycarboxylic used as thickening agent
    • 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
    • C10M2207/121—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of seven or less carbon atoms
    • C10M2207/124—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of seven or less carbon atoms containing hydroxy groups; Ethers thereof
    • C10M2207/1245—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of seven or less carbon atoms containing hydroxy groups; Ethers thereof used as thickening agent
    • 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
    • C10M2207/14—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to carbon atoms of six-membered aromatic rings
    • C10M2207/141—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to carbon atoms of six-membered aromatic rings monocarboxylic
    • C10M2207/1415—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to carbon atoms of six-membered aromatic rings monocarboxylic used as thickening agent
    • 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
    • C10M2207/14—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to carbon atoms of six-membered aromatic rings
    • C10M2207/144—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to carbon atoms of six-membered aromatic rings containing hydroxy groups
    • C10M2207/1446—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to carbon atoms of six-membered aromatic rings containing hydroxy groups used as thickening agent
    • 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
    • C10M2229/00—Organic macromolecular compounds containing atoms of elements not provided for in groups C10M2205/00, C10M2209/00, C10M2213/00, C10M2217/00, C10M2221/00 or C10M2225/00 as ingredients in lubricant compositions
    • C10M2229/04—Siloxanes with specific structure
    • C10M2229/042—Siloxanes with specific structure containing aromatic substituents
    • C10M2229/0425—Siloxanes with specific structure containing aromatic substituents used as base material
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
    • C10N2030/06—Oiliness; Film-strength; Anti-wear; Resistance to extreme pressure
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • 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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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Organic Chemistry (AREA)
  • Lubricants (AREA)

Abstract

The invention relates to the field of lubricating grease, and discloses a method for preparing lubricating grease and application thereof. The method comprises the following steps: mixing alkylbenzene sulfonic acid, a calcium-containing alkaline substance, calcium carboxylate and part of base oil, gradually adding water into the obtained mixture to enable the alkylbenzene sulfonic acid to react with the calcium-containing alkaline substance to generate calcium alkylbenzene sulfonate, heating and dehydrating, and then mixing the product with the rest of base oil and optional additives; wherein the calcium carboxylate is at least one selected from aliphatic calcium carboxylate and aromatic calcium carboxylate. The method for preparing the lubricating grease has simple process, short time and no volatile gas in the reaction process, and is beneficial to environmental protection.

Description

Method for preparing lubricating grease and application thereof
Technical Field
The invention relates to the field of lubricating grease, in particular to a method for preparing lubricating grease and application thereof.
Background
As the requirements of mechanical equipment on lubrication conditions are higher and higher, the used lubricating grease is required to have a higher dropping point, so that the use of the lubricating grease under the high-temperature condition is satisfied.
The composition and preparation of complex calcium sulfonate-based greases are described in some documents. For example, CN1414076a discloses a preparation method of complex calcium sulfonate grease, which needs to convert high-alkalinity petroleum calcium sulfonate to further prepare the grease, and has complex process and difficult quality control. CN102604724a discloses the composition of a composite calcium-based grease thickener, comprising calcium benzoate, calcium salicylate, calcium borate, and calcium acetate, calcium octoate and 12-hydroxystearate, and in order to improve the grease performance, additives such as graphite and tungsten disulfide are also added. The grease composition has poor heat resistance and can be blackened and hardened after long-term use at high temperature. The organic acid and calcium are respectively reacted to prepare the composite calcium-based lubricating grease to finally form a calcium complex (CN 103958653A) with a complex structure, the reaction process is complex, the reaction time is long, and the organic acid possibly generates smell in the reaction process, which is not beneficial to environmental protection.
Disclosure of Invention
The invention aims to solve the problems of long process complexity and environmental protection in the prior art, and provides a method for preparing lubricating grease and application thereof.
In order to achieve the above object, the present invention provides a method of preparing grease, the method comprising: mixing alkylbenzene sulfonic acid, a calcium-containing alkaline substance, calcium carboxylate and part of base oil, gradually adding water into the obtained mixture to enable the alkylbenzene sulfonic acid to react with the calcium-containing alkaline substance to generate calcium alkylbenzene sulfonate, heating and dehydrating, and then mixing the product with the rest of base oil and optional additives; wherein the calcium carboxylate is at least one selected from aliphatic calcium carboxylate and aromatic calcium carboxylate.
The invention also provides application of the method in improving the water resistance of lubricating grease.
The method for preparing the lubricating grease has the advantages of simple process, short time, less volatile gas generation amount in the reaction process, no foam generation and environmental protection. Moreover, the lubricating grease with good water resistance, smaller cone penetration, higher dropping point and stronger extreme pressure abrasion resistance can be obtained under the condition of not additionally introducing other additives.
Detailed Description
The endpoints and any values of the ranges disclosed herein are not limited to the precise range or value, and are understood to encompass values approaching those ranges or values. For numerical ranges, one or more new numerical ranges may be found between the endpoints of each range, between the endpoint of each range and the individual point value, and between the individual point value, in combination with each other, and are to be considered as specifically disclosed herein.
The invention provides a method for preparing lubricating grease, which is characterized by comprising the following steps: mixing alkylbenzene sulfonic acid, a calcium-containing alkaline substance, calcium carboxylate and part of base oil, gradually adding water into the obtained mixture to enable the alkylbenzene sulfonic acid to react with the calcium-containing alkaline substance to generate calcium alkylbenzene sulfonate, heating and dehydrating, and then mixing the product with the rest of base oil and optional additives; wherein the calcium carboxylate is at least one selected from aliphatic calcium carboxylate and aromatic calcium carboxylate.
According to the invention, the alkaline substance containing calcium may be used in an amount of 60 to 160g, preferably 80 to 140g, per kg of alkylbenzenesulfonic acid.
According to the invention, the calcium carboxylate may be used in an amount of 0.5 to 2.5kg, preferably 0.6 to 1.5kg, per kg of alkylbenzenesulfonic acid.
According to the invention, the total amount of base oil used may be 0.5 to 6kg, preferably 1.5 to 3.5kg, per kg of alkylbenzenesulfonic acid.
According to the invention, the rate of addition of water is preferably 0.1 to 20L/min (e.g., 0.3, 0.4, 0.5, 0.9, 1, 1.2, 1.3, 1.4, 2.5, 3, 4, 5, 6, 8, 10, 12, 14, 16, 18L/min or any value in between) per kilogram of alkylbenzenesulfonic acid.
According to the present invention, water is introduced into the system in a gradual manner, and the reaction between the alkylbenzene sulfonic acid and the calcium-containing alkaline substance is usually carried out at a certain temperature, so that it is necessary to heat the system, and water may be added to the system at the beginning of the heating process. According to a preferred embodiment of the invention, the method comprises: mixing alkylbenzene sulfonic acid, calcium-containing alkaline substance, calcium salt of alkylbenzene sulfonate carboxylate and part of base oil, heating the mixture to 100-120 ℃ and maintaining the temperature for 5-10min, gradually adding water into the obtained mixture during heating to react the alkylbenzene sulfonic acid with the calcium-containing alkaline substance to generate calcium alkylbenzene sulfonate, heating to 150-170 ℃ to dehydrate, and mixing the product with the rest of base oil and optional additives. The method may further comprise: mixing with the rest base oil, cooling the materials, and grinding when the temperature is reduced to 80-100deg.C to disperse the materials more uniformly. Those skilled in the art will appreciate that if the water addition is not complete during heating, it is continued during the incubation. The process of the invention is generally effective in reducing the reaction time and avoiding foam generation in the system.
According to the invention, the total amount of water added is preferably 0.2 to 1.5kg (e.g. 0.2, 0.25, 0.3, 0.35, 0.4, 0.45, 0.5, 0.55, 0.6, 0.7, 1, 1.4kg or any value between the above values) per kg of alkylbenzene sulphonic acid. The method of the invention can obviously reduce the relative dosage of water.
According to the invention, the alkylbenzene sulphonic acid has a base number of 100-180mgKOH/g.
According to the present invention, the alkylbenzenesulfonic acid may be alkylbenzenesulfonic acid commonly known in the art, and the structural formula thereof may be: r is R 1 -C 6 H 4 -SO 3 H, where R is 1 Preferably C10-C24 alkyl (straight or branched). The alkylbenzene sulfonic acid may be a single component having a specific structural formula, such as dodecylbenzene sulfonic acid; mixtures of a plurality of alkylbenzene sulfonic acids having different carbon numbers, such as medium alkylbenzene sulfonic acid, heavy alkylbenzene sulfonic acid, etc., are also possible as long as each component in the mixture satisfies the above general formula.
According to a preferred embodiment of the present invention, the alkylbenzene sulfonic acid is at least one selected from dodecylbenzene sulfonic acid, octadecylbenzene sulfonic acid and tetracosyl benzene sulfonic acid.
According to the present invention, the calcium carboxylate may be a calcium carboxylate salt commonly known in the art, for example, a calcium carboxylate having 2 to 10 carbon atoms. The structural formula of the calcium carboxylate can be (R 2 -COO) 2 Ca and/or (OOC-R) 3 -COO) Ca, wherein R 2 Preferably a substituted or unsubstituted phenyl group, or a substituted or unsubstituted C1-C8 hydrocarbon group, R 3 Is a C1-C10 alkylene group. More preferably, the substituted group in the calcium carboxylate is a hydroxyl group.
According to a more preferred embodiment of the present invention, the calcium carboxylate is at least one selected from the group consisting of calcium acetate, calcium propionate, calcium butyrate, calcium lactate, calcium sorbate, calcium salicylate, calcium sebacate and calcium benzoate.
According to the present invention, the calcium-containing alkaline substance is not particularly limited as long as it can react with alkylbenzenesulfonic acid to produce calcium alkylbenzenesulfonate, and preferably, the calcium-containing alkaline substance is at least one selected from calcium hydroxide, calcium carbonate, calcium bicarbonate, calcium phosphate, monocalcium phosphate and monocalcium phosphate.
According to the invention, the weight ratio of part of the base oil to the remainder of the base oil is from 0.5 to 5, preferably from 1 to 4.
According to the present invention, the base oil may be various base oils used in greases, such as mineral oils, synthetic oils (silicone oils, olefin oils and/or ester oils), vegetable oils or mixtures thereof. Preferably, the base oil has a kinematic viscosity at 100℃of from 2 to 300mm 2 S, preferably 6-100mm 2 And/s. In the present invention, "kinematic viscosity" is measured with reference to GB/T265-1988.
According to the present invention, the additives may include various components that can be used to improve the performance of the grease, for example, an extreme pressure antiwear agent, an antioxidant, an anticorrosive agent, an antirust agent, a detergent dispersant, a tackifier, and the like. According to a preferred embodiment of the present invention, the additive may be an extreme pressure antiwear agent to further improve the extreme pressure and antiwear properties of the grease composition. The extreme pressure antiwear agent may be at least one selected from the group consisting of calcium carbonate, calcium bicarbonate, calcium phosphate, monocalcium phosphate and monocalcium phosphate, preferably calcium carbonate, and the crystal type of the calcium carbonate may be conventional, and may include, for example, aragonite type, calcite type, vaterite type, and the like. Other additives besides extreme pressure antiwear agents may be conventional in the art and are not described in detail herein. Although the grease composition of the present invention may contain other additives, the present invention can obtain a grease having a smaller cone penetration, a higher drop point and a higher extreme pressure antiwear property without introducing other additives, and additionally introducing other additives will further improve the performance of the grease.
According to a particularly preferred embodiment of the present invention, the method of preparing a grease composition according to the present invention comprises: adding mineral oil and dodecylbenzene sulfonic acid (with a base number of 170-175mg KOH/g) into a reaction kettle, uniformly stirring, adding calcium hydroxide and calcium benzoate, uniformly stirring, gradually adding water, heating to 100-110 ℃ at constant temperature for 4-6min, continuously heating to 140-160 ℃ at constant temperature for 4-6min, stopping heating, adding mineral oil, cooling to 90-110 ℃ by material, and grinding to obtain the lubricating grease composition, wherein the dosage of calcium hydroxide is 130-140g, the dosage of calcium benzoate is 0.8-1.2kg, the total dosage of mineral oil is 1.5-2kg, the adding speed of water is 0.9-1L/min, and the total adding amount of water is 0.4-0.6kg relative to each kilogram of dodecylbenzene sulfonic acid. According to this preferred embodiment, a grease having better properties can be obtained, see in particular the following examples.
The invention also provides application of the method in improving the water resistance of lubricating grease. That is, the present invention also relates to a method for improving the water resistance of a grease, characterized in that the method comprises: mixing alkylbenzene sulfonic acid, a calcium-containing alkaline substance, calcium carboxylate and part of base oil, gradually adding water into the obtained mixture to enable the alkylbenzene sulfonic acid to react with the calcium-containing alkaline substance to generate calcium alkylbenzene sulfonate, heating and dehydrating, and then mixing the product with the rest of base oil and optional additives; wherein the calcium carboxylate is at least one selected from aliphatic calcium carboxylate and aromatic calcium carboxylate. The specific selection, amounts and conditions of the various materials are as described above and will not be described in detail herein.
The present invention will be described in detail by examples. In the following examples and comparative examples,
cone penetration (25 ℃,0.1mm,60 times) detection reference: GB/T269-1991, the smaller the 60 working cone penetration, the stronger the thickening ability;
detection of drop point reference: GB/T3498-2008, the higher the drop point, the better the high temperature performance is;
extreme pressure Property (maximum no seizure load, P) B Value) of the detection reference: SH/T0202-1992 (four-ball machine method) for measuring extreme pressure property of lubricating grease, wherein the four-ball testing machine is set at the rotating speed of 1770r/min for 10s; extreme pressure Property (sintering load, P) D Value) of the detection reference: SH/T0202-1992 (four-ball machine method) for measuring extreme pressure property of lubricating grease, wherein the four-ball testing machine is set at the rotating speed of 1770r/min for 10s; detection of antiwear properties (d value) reference: SH/T0204-1992 (four-ball machine method) for measuring wear resistance of lubricating grease, wherein the setting condition of a four-ball testing machine is that the rotating speed is 1200r/min, the load is 392N, and the time is 60min; the larger the PB value and the PD value are, the smaller the d value is, which shows that the extreme pressure abrasion resistance is stronger;
detection reference of water resistance of grease: SH/T0643-1997 test method for Water spray resistance of grease, specifically, the method is to uniformly coat the grease on a stainless steel plate, spray the grease with water at a prescribed test temperature (38 ℃ + -0.5 ℃) and pressure (276 kPa+ -7 kPa), and after 5 minutes, determine the spray weight loss percentage of the grease as a measure of the Water spray resistance of the grease. The smaller the number, the better the water resistance of the grease.
The detection standard of the smell of the lubricating grease is referred to GB/T5525-2008 "vegetable oil transparency, smell and taste identification method", and the operation method is as follows: during the greasing process, a small sample of grease was taken and heated to 50 ℃ in a beaker and removed from the heat source. The test person smells the smell while stirring, and the expression level of the smell includes: class 1 (odorless or almost odorless), class 2 (having a small amount of pungent odor) and class 3 (having a pungent odor).
Mineral oil (100 ℃ C. Kinematic viscosity of 30 mm) 2 S) from Peking Yanshan petrochemical; olefin oil (100 ℃ C. Kinematic viscosity of 6 mm) 2 S) from Exxon Mobil; benzyl silicone oil (100 ℃ C. Kinematic viscosity 20 mm) 2 S) from the morning photonics industry of Sichuan;
alkylbenzenesulfonic acid was purchased from the south Beijing alkylbenzene mill; calcium salts of organic acids such as calcium benzoate, calcium acetate, and calcium citrate were purchased from Beijing reagent company.
Example 1
Adding 360g of mineral oil and 270g of dodecylbenzene sulfonic acid (with a base number of 173mg KOH/g) into a reaction kettle, uniformly stirring, adding 36.7g of calcium hydroxide and 270g of calcium benzoate, uniformly stirring, gradually adding 135g of water at an adding rate of 0.25L/min, heating to 100 ℃, keeping the temperature for 5min, continuously heating to 150 ℃, keeping the temperature for 5min, stopping heating, adding 100g of mineral oil, cooling the materials to 100 ℃, and grinding by a three-wheel mill to obtain a lubricating grease sample. The volatile gas is generated in a small amount in the preparation process, and no foam is generated.
Example 2
The feed composition and process conditions were the same as in example 1, with the base oil being replaced by an olefin oil. The volatile gas is generated in a small amount in the preparation process, and no foam is generated.
Example 3
The material composition and process conditions were the same as in example 1, with the base oil being replaced by benzyl silicone oil. The volatile gas is generated in a small amount in the preparation process, and no foam is generated.
Example 4
400g of mineral oil and 150g of dodecylbenzene sulfonic acid (with a base number of 173mg KOH/g) are added into a reaction kettle, the mixture is stirred uniformly, 20.4g of calcium hydroxide and 150g of calcium benzoate are added, the mixture is stirred uniformly, 75g of water is gradually added at an adding rate of 0.2L/min, the mixture is heated and heated to 120 ℃ at the same time, the temperature is kept for 5min, the mixture is continuously heated and heated to 170 ℃ and kept at the constant temperature for 5min, the heating is stopped, 100g of mineral oil is added, the temperature of the mixture is reduced to 100 ℃, and a lubricating grease sample is prepared through three-wheel grinding. The volatile gas is generated in a small amount in the preparation process, and no foam is generated.
Example 5
Adding 300g of mineral oil and 300g of octadecyl benzene sulfonic acid (with a base number of 121mg KOH/g) into a reaction kettle, uniformly stirring, adding 28.4g of calcium hydroxide and 200g of calcium benzoate, uniformly stirring, gradually adding 100g of water at an adding rate of 0.1L/min, heating to 110 ℃, keeping the temperature for 5min, continuously heating to 160 ℃, keeping the temperature for 5min, stopping heating, adding 200g of mineral oil, cooling the materials to 100 ℃, and grinding by a three-wheel mill to obtain a lubricating grease sample. The volatile gas is generated in a small amount in the preparation process, and no foam is generated.
Example 6
Adding 300g of mineral oil and 200g of tetracosyl benzene sulfonic acid (with a base number of 107mg KOH/g) into a reaction kettle, uniformly stirring, adding 17g of calcium hydroxide and 300g of calcium benzoate, uniformly stirring, gradually adding 150g of water at an adding rate of 0.7L/min, heating to 100 ℃, keeping the temperature for 5min, continuously heating to 150 ℃, keeping the temperature for 5min, stopping heating, adding 200g of mineral oil, cooling the materials to 100 ℃, and grinding by a three-wheel mill to obtain a lubricating grease sample. The volatile gas is generated in a small amount in the preparation process, and no foam is generated.
Example 7
Adding 360g of mineral oil and 270g of dodecylbenzene sulfonic acid (with a base number of 173mg KOH/g) into a reaction kettle, uniformly stirring, adding 36.7g of calcium hydroxide and 270g of calcium acetate, uniformly stirring, gradually adding 135g of water at an adding rate of 0.3L/min, heating to 100 ℃, keeping the temperature for 5min, continuously heating to 150 ℃, keeping the temperature for 5min, stopping heating, adding 100g of mineral oil, cooling the materials to 100 ℃, and grinding by a three-wheel mill to obtain the lubricating grease sample. The volatile gas is generated in a small amount in the preparation process, and no foam is generated.
Example 8
Adding 360g of mineral oil and 270g of dodecylbenzene sulfonic acid (with a base number of 173mg KOH/g) into a reaction kettle, uniformly stirring, adding 36.7g of calcium hydroxide and 270g of calcium citrate, uniformly stirring, gradually adding 135g of water at an adding rate of 0.8L/min, heating to 100 ℃, keeping the temperature for 5min, continuously heating to 150 ℃, keeping the temperature for 5min, stopping heating, adding 100g of mineral oil, cooling the materials to 100 ℃, and grinding by a three-wheel mill to obtain a lubricating grease sample. The volatile gas is generated in a small amount in the preparation process, and no foam is generated.
Example 9
Adding 360g of mineral oil and 270g of dodecylbenzene sulfonic acid (with a base number of 173mg KOH/g) into a reaction kettle, uniformly stirring, adding 36.7g of calcium hydroxide and 270g of calcium benzoate, uniformly stirring, gradually adding 135g of water at an adding rate of 1.5L/min, heating to 100 ℃, keeping the temperature for 5min, continuously heating to 150 ℃, keeping the temperature for 5min, stopping heating, adding 100g of mineral oil, cooling the materials to 100 ℃, and grinding by a three-wheel mill to obtain a lubricating grease sample. The volatile gas is generated in a small amount in the preparation process, and no foam is generated.
Test example 1
The grease samples prepared in the examples and comparative examples were subjected to performance tests, and the test results are shown in table 1.
TABLE 1
Figure BDA0003328183900000091
From Table 1, it can be seen that the grease of the present invention can be obtained with good water resistance, less penetration, higher dropping point and higher extreme pressure antiwear property without additional introduction of other additives. Further experiments show that compared with a lubricating grease sample prepared by directly mixing and reacting alkyl benzene sulfonic acid, aliphatic carboxylic acid or aromatic carboxylic acid with a calcium-containing alkaline substance, the lubricating grease obtained by the method has better water resistance and other properties.
The preferred embodiments of the present invention have been described in detail above, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, a number of simple variants of the technical solution of the invention are possible, including combinations of the individual technical features in any other suitable way, which simple variants and combinations should likewise be regarded as being disclosed by the invention, all falling within the scope of protection of the invention.

Claims (11)

1. A method of preparing a grease, the method comprising: mixing alkylbenzene sulfonic acid, a calcium-containing alkaline substance, calcium carboxylate and part of base oil, gradually adding water into the obtained mixture to enable the alkylbenzene sulfonic acid to react with the calcium-containing alkaline substance to generate calcium alkylbenzene sulfonate, heating and dehydrating, and then mixing the product with the rest of base oil and optional additives; wherein the calcium carboxylate is at least one selected from aliphatic calcium carboxylate and aromatic calcium carboxylate.
2. The method according to claim 1, wherein the amount of the calcium-containing basic substance is 60 to 160g, the amount of the calcium carboxylate is 0.5 to 2.5kg, and the total amount of the base oil is 0.5 to 6kg per kg of the alkylbenzenesulfonic acid;
and/or, the rate of addition of water is 0.1 to 20L/min per kg of alkylbenzenesulfonic acid, and the total amount of water added is 0.2 to 1.5kg.
3. The process according to claim 1 or 2, wherein the alkylbenzene sulfonic acid has a base number of 100-180mgKOH/g.
4. The method of claim 1 or 2, wherein the alkylbenzene sulfonic acid has the structural formula: r is R 1 -C 6 H 4 -SO 3 H, where R is 1 Is a C10-C24 alkyl group.
5. The method of claim 4, wherein the alkylbenzene sulfonic acid is selected from at least one of dodecylbenzene sulfonic acid, octadecylbenzene sulfonic acid, and tetracosyl benzene sulfonic acid.
6. The method according to claim 1 or 2, wherein the calcium carboxylate has the structural formula (R 2 -COO) 2 Ca and/or (OOC-R) 3 -COO) Ca, wherein R 2 Is a substituted or unsubstituted phenyl group, or a substituted or unsubstituted C1-C8 hydrocarbon group, R 3 Is a C1-C10 hydrocarbylene group;
preferably, the substituted group in the calcium carboxylate is a hydroxyl group.
7. The method of claim 6, wherein the calcium carboxylate is selected from at least one of calcium acetate, calcium propionate, calcium butyrate, calcium lactate, calcium sorbate, calcium salicylate, calcium sebacate, and calcium benzoate.
8. The method according to claim 1 or 2, wherein the calcium-containing alkaline substance is selected from at least one of calcium hydroxide, calcium carbonate, calcium bicarbonate, calcium phosphate, monocalcium phosphate and monocalcium phosphate.
9. A process according to claim 1 or 2, wherein the weight ratio of part of the base oil to the balance of the base oil is 0.5-5, preferably 1-4.
10. The process according to claim 1 or 2, wherein the base oil has a kinematic viscosity at 100 ℃ of 2-300mm 2 S, preferably 6-100mm 2 /s。
11. Use of the method according to any one of claims 1-10 for improving the water resistance of a grease.
CN202111269492.0A 2021-10-29 2021-10-29 Method for preparing lubricating grease and application thereof Pending CN116064185A (en)

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US5308514A (en) * 1993-03-03 1994-05-03 Witco Corporation Sulfonate greases
CN101679896A (en) * 2007-04-13 2010-03-24 国际壳牌研究有限公司 A lithium hydroxide composition, a process for preparing a lithium hydroxide composition, and a process for using a lithium hydroxide composition
CN104769087A (en) * 2012-11-16 2015-07-08 出光兴产株式会社 Grease composition
CN105482885A (en) * 2015-07-17 2016-04-13 路伯润滑油（苏州）有限公司 Robot-arm grease and preparation method thereof
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