CN110616103B - Commercial vehicle wheel hub bearing lubricating grease and preparation method thereof - Google Patents

Commercial vehicle wheel hub bearing lubricating grease and preparation method thereof Download PDF

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Publication number
CN110616103B
CN110616103B CN201910639261.0A CN201910639261A CN110616103B CN 110616103 B CN110616103 B CN 110616103B CN 201910639261 A CN201910639261 A CN 201910639261A CN 110616103 B CN110616103 B CN 110616103B
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stirring
constant temperature
cooling
minutes
heating
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CN110616103A (en
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许扬
王彦冬
闫瑾
徐小鹏
王清国
桃春生
汪玉瑄
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FAW Jiefang Automotive Co Ltd
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FAW Jiefang Automotive Co Ltd
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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
    • C10M113/00—Lubricating compositions characterised by the thickening agent being an inorganic 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
    • 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
    • C10M117/00—Lubricating compositions characterised by the thickener being a non-macromolecular carboxylic acid or salt thereof
    • C10M117/02—Lubricating compositions characterised by the thickener being a non-macromolecular carboxylic acid or salt thereof having only one carboxyl group bound to an acyclic carbon atom, cycloaliphatic carbon atom or hydrogen
    • C10M117/04—Lubricating compositions characterised by the thickener being a non-macromolecular carboxylic acid or salt thereof having only one carboxyl group bound to an acyclic carbon atom, cycloaliphatic carbon atom or hydrogen containing hydroxy groups
    • 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
    • C10M117/00—Lubricating compositions characterised by the thickener being a non-macromolecular carboxylic acid or salt thereof
    • C10M117/06—Lubricating compositions characterised by the thickener being a non-macromolecular carboxylic acid or salt thereof having more than one carboxyl group bound to an acyclic carbon atom or cycloaliphatic carbon atom
    • 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
    • C10M119/00—Lubricating compositions characterised by the thickener being a macromolecular compound
    • C10M119/24—Lubricating compositions characterised by the thickener being a macromolecular compound containing nitrogen
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M169/00—Lubricating compositions characterised by containing as components a mixture of at least two types of ingredient selected from base-materials, thickeners or additives, covered by the preceding groups, each of these compounds being essential
    • C10M169/06—Mixtures of thickeners and additives
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/087—Boron oxides, acids or salts
    • C10M2201/0876—Boron oxides, acids or salts 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
    • C10M2203/00—Organic non-macromolecular hydrocarbon compounds and hydrocarbon fractions as ingredients in lubricant compositions
    • C10M2203/10—Petroleum or coal fractions, e.g. tars, solvents, bitumen
    • C10M2203/102—Aliphatic fractions
    • C10M2203/1025—Aliphatic fractions used as base material
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/02—Hydroxy compounds
    • C10M2207/023—Hydroxy compounds having hydroxy groups bound to carbon atoms of six-membered aromatic rings
    • C10M2207/026—Hydroxy compounds having hydroxy groups bound to carbon atoms of six-membered aromatic rings with tertiary alkyl groups
    • C—CHEMISTRY; METALLURGY
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    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/10—Carboxylix acids; Neutral salts thereof
    • C10M2207/12—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms
    • C10M2207/125—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids
    • C10M2207/127—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
    • C10M2207/1276—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 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
    • C10M2207/125—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids
    • C10M2207/128—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids containing hydroxy groups; Ethers thereof
    • C10M2207/1285—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids containing hydroxy groups; Ethers thereof used as thickening agents
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2209/00—Organic macromolecular compounds containing oxygen as ingredients in lubricant compositions
    • C10M2209/02—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • C10M2209/08—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds containing monomers having an unsaturated radical bound to a carboxyl radical, e.g. acrylate type
    • 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
    • C10M2215/22—Heterocyclic nitrogen compounds
    • C10M2215/223—Five-membered rings containing nitrogen and carbon only
    • 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
    • C10M2217/00—Organic macromolecular compounds containing nitrogen as ingredients in lubricant compositions
    • C10M2217/04—Macromolecular compounds from nitrogen-containing monomers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • C10M2217/045—Polyureas; Polyurethanes
    • C10M2217/0456—Polyureas; Polyurethanes 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
    • 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
    • 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
    • C10N2030/08—Resistance to extreme temperature
    • 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
    • C10N2030/68—Shear stability
    • 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
    • C10N2040/00—Specified use or application for which the lubricating composition is intended
    • C10N2040/02—Bearings
    • 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
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02T—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO TRANSPORTATION
    • Y02T10/00—Road transport of goods or passengers
    • Y02T10/80—Technologies aiming to reduce greenhouse gasses emissions common to all road transportation technologies
    • Y02T10/86—Optimisation of rolling resistance, e.g. weight reduction 

Abstract

The invention discloses a commercial vehicle hub bearing lubricating grease and a preparation method thereof, belonging to the technical field of commercial vehicle hub bearing lubricating grease, aiming at improving the high-temperature stability and the colloid stability of the lubricating grease, reducing the oil distribution amount of the lubricating grease, improving the extreme pressure property and the shearing resistance of the lubricating grease, reducing the consistency change of the lubricating grease and reducing the grease throwing risk of the lubricating grease; the extreme pressure property and the shearing resistance of the lubricating grease are improved, the consistency change of the lubricating grease is reduced, and the risk of throwing the lubricating grease is reduced. The composition of the synthetic adhesive and the natural adhesive has a synergistic effect, the shear stability of the lubricating grease is obviously improved, the consistency change of the lubricating grease is reduced, the lubricating grease is well adhered to the surface of a friction pair, and the risk of grease throwing of the lubricating grease is reduced.

Description

Commercial vehicle wheel hub bearing lubricating grease and preparation method thereof
Technical Field
The invention belongs to the technical field of commercial vehicle wheel hub bearing lubricating grease.
Background
The bearing is divided into an open bearing and a closed bearing according to the sealing condition, and along with the development of the bearing to unitization, the use of the bearing unit based on the closed bearing is increased. Sealed bearings can be lubricated with lubricating oil, but lubricating oil has a high requirement for oil resistance of seals, and grease is still the main lubricating medium for bearings.
Commercial wheel hub bearings are divided into open pairs of bearings and closed bearing units. The closed bearing unit is usually lubricated by using lubricating oil, so that the long service life of the bearing can be realized without maintenance. The open paired bearings cannot be lubricated by lubricating oil, and usually are lubricated by lithium-based lubricating grease and lithium complex lubricating grease, but the lubricating grease is limited by use conditions, so that the problems of oil leakage, grease throwing and the like easily occur to the lubricating grease, and the long service life and maintenance-free performance of the bearings cannot be realized.
The lubricating grease is subjected to the actions of high temperature, frequent shearing and the like, a space network structure formed by a thickening agent is damaged, a large amount of free oil and adsorbed oil are irreversibly separated out, the consistency is rapidly reduced and softened, the lubricating grease is influenced by a large centrifugal force, the problems of oil leakage and grease throwing of the lubricating grease occur, the corrosion protection and the lubrication protection degree of a bearing are reduced, and the service life of the bearing is influenced.
In order to solve the problems of oil leakage and grease throwing of the hub bearing lubricating grease, a proper method is needed to improve the stability of a lubricating grease densifier under the action of high temperature and high shear, so that the oil distribution amount is controlled within a reasonable range, the adhesion capacity of the lubricating grease on the surface of a bearing friction pair is improved by a proper method, and the risk of throwing the lubricating grease under the action of centrifugal force is reduced. Specifically, a thickener with good thermal stability and strong mechanical stability is required to be adopted during the formula design of the lubricating grease, so that the structural stability of the lubricating grease thickener fiber under the action of high temperature and high shear is maintained; the capability of the lubricating grease for resisting centrifugal force is improved by adding special additives.
Currently, greases of the common thickener type exhibit different high temperature properties. On the dropping point project, the composite calcium sulfonate lubricating grease > the composite lithium lubricating grease > the polyurea lubricating grease > the composite aluminum-based lubricating grease > the lithium-based lubricating grease; on the high-temperature rheological property project, the structure retention capacity of the lubricating grease is reduced along with the temperature rise, the structure retention capacity is stronger and easier to be hardened, the structure retention capacity is that composite lithium lubricating grease is greater than carbamido lubricating grease (arylarylamine) > composite aluminum-based lubricating grease is greater than carbamido lubricating grease (long-chain amine) > carbamido lubricating grease (short-chain arylamine) > composite calcium sulfonate lubricating grease at normal temperature, and the structure retention capacity is that carbamido lubricating grease (arylarylamine) > lubricating grease (short-chain arylamine) > carbamido lubricating grease (long-chain amine) > composite aluminum-based lubricating grease is greater than composite lithium lubricating grease is greater than composite calcium sulfonate lubricating grease at high temperature.
Grease adhesion agents, like viscosity index improvers for lubricating oils, on the one hand increase the viscosity of the base oil in the grease and reduce the fluidity of the base oil, and on the other hand increase the "contact angle" of the grease base oil with the solid interface and increase the adhesion of the grease to the solid. Common grease adhesives include Polyisobutylene (PIB), polymethacrylate (PMA), ethylene-propylene copolymer (OCP).
The preparation method of the lubricating grease is generally divided into a coacervation method and a dispersion method, namely, chemical substances forming the thickening agent are added into base oil step by step, and the lubricating grease is produced through the technical processes of heating dissolution, high-temperature esterification (saponification), high-temperature dehydration, cooling homogenization, grinding and the like, wherein the high-temperature esterification (saponification) process is an important step for forming a network structure of the thickening agent, is beneficial to the sufficient association among molecules of the thickening agent, is simple to operate and easy to industrialize, and has higher control requirements on the technical parameters such as preparation temperature, stirring time and the like.
CN 102618368B discloses a lubricating grease for heavy duty automobile hubs and a preparation method thereof, wherein a composite lithium soap thickener is used as a thickening agent, and borate oil, a compound viscosity index improver, a detergent dispersant, an amine antioxidant, a sulfur-phosphorus antioxidant and a sulfonate antirust agent are added to obtain the hub lubricating grease with heat resistance, adhesion, mechanical stability, water resistance and extreme pressure abrasion resistance. However, the invention only comprises one thickening agent, and the additive is various.
CN 102839041B discloses a composite lithium lubricating grease composition and a preparation method thereof, which takes composite lithium as a thickening agent and is added with polybutene or polymethacrylate, an antioxidant, an extreme pressure antiwear agent and an antirust agent. The obtained lubricating grease has good adhesion, excellent water resistance and heat resistance, and is suitable for lubricating automobile hub bearings under harsh working conditions. However, the invention only comprises one thickening agent, and the additive is various.
CN 108841430A discloses a composite urea aluminum-based lubricating grease composition and a preparation method thereof, wherein polyurea and composite aluminum are used as thickening agents, and antirust agents are added, and the polyurea and the composite aluminum are mixed to obtain the lubricating grease with high-temperature colloid stability, metal adhesion, film-forming property and extreme pressure abrasion resistance, and the lubricating grease composition is suitable for being used in high-temperature, heavy-load, humid and other environments. However, the thickening agent disclosed by the invention is high in production cost and is not beneficial to industrial popularization.
CN 1257963C discloses a preparation method of polyurea-lithium-based lubricating grease, which comprises the steps of preparing a polyurea thickening agent, continuously preparing a lithium-based thickening agent in the same reaction kettle, heating, cooling, homogenizing and the like to obtain the lubricating grease with the same technical performance as a mixing method. However, the thickening agent disclosed by the invention is only a lithium-based thickening agent, and the compounding of a composite lithium thickening agent and a polyurea thickening agent is not involved.
CN1414076A discloses a high base number composite calcium sulfonate lubricating grease and a preparation method thereof, wherein a calcium sulfonate thickening agent is prepared firstly, and then a carbamido thickening agent is prepared, so that the compounding of calcium sulfonate and the carbamido thickening agent is realized. However, the thickening agent disclosed by the method has high production cost and is not beneficial to industrial production.
CN104711080B discloses a modified composite calcium sulfonate lubricating grease and a preparation method thereof, wherein high-base-number calcium sulfonate, lithium hydroxide, dodecahydroxystearic acid and binary acid are used as basic raw materials, and the prepared lubricating grease contains a composite calcium sulfonate thickening agent and a composite lithium thickening agent. However, the thickening agent disclosed by the invention does not contain a composite polyurea thickening agent.
Disclosure of Invention
In order to improve the high-temperature stability and the colloid stability of the lubricating grease, reduce the oil content of the lubricating grease, improve the extreme pressure property and the shearing resistance of the lubricating grease, reduce the consistency change of the lubricating grease and reduce the risk of throwing the lubricating grease, the invention provides the commercial vehicle hub bearing lubricating grease, which adopts the following technical scheme:
the commercial vehicle wheel hub bearing lubricating grease comprises the following raw material components in parts by weight: 81-88wt% of base oil, 10-15wt% of composite thickening agent, 1.2-1.8wt% of composite adhesive, 0.5-0.9wt% of antioxidant, 0.5-0.9wt% of extreme pressure antiwear agent and 0.001-0.005wt% of antirust agent.
The base oil is a group II base oil, a group III base oil or a combination of the two.
The composite thickening agent comprises a composite polyurea thickening agent, a composite calcium sulfonate thickening agent and a composite lithium thickening agent in a weight ratio of (1.
The composite polyurea thickening agent is prepared by compounding 1.02-2.30wt% of diisocyanate, 0.42-0.95wt% of organic amine, 0.24-0.54wt% of carboxyl source and 0.08-0.18wt% of alkali metal.
Wherein the diisocyanate is diphenylmethane-4,4-diisocyanate (MDI) or Toluene Diisocyanate (TDI), preferably diphenylmethane-4,4-diisocyanate (MDI); the organic amine is one or more of cyclohexylamine, p-toluidine, decaamine, hexamethylenediamine and p-phenylenediamine, preferably a composition of cyclohexylamine and p-toluidine; the carboxyl source is caprolactam or ethyl p-aminobenzoate, and caprolactam is preferred; the alkali metal is sodium hydroxide or lithium hydroxide, preferably lithium hydroxide.
The compound calcium sulfonate thickening agent is prepared by compounding 0.77-2.31wt% of high-alkalinity calcium sulfonate, 0.13-0.39wt% of transforming agent, 0.06-0.18wt% of saponification acid and 0.03-0.09wt% of saponification alkali. Wherein the overbased calcium sulfonate is overbased calcium petroleum sulfonate or overbased synthetic calcium sulfonate, preferably overbased calcium petroleum sulfonate; the transforming agent is water, acetic acid or methanol, preferably water; the saponification acid is dodecahydroxystearic acid, dodecanoic acid, hexadecanoic acid or boric acid, preferably dodecahydroxystearic acid; the saponification base is calcium hydroxide or calcium carbonate, preferably calcium hydroxide.
The composite lithium thickening agent is prepared by compounding 4.41-6.62wt% of normal soap, 0.90-1.89wt% of complexing agent and 0.90-1.90wt% of lithium hydroxide. Wherein, the normal soap is dodecahydroxystearic acid or stearic acid, preferably dodecahydroxystearic acid; the complexing agent is one or more of sebacic acid, azelaic acid and boric acid, preferably the composition of sebacic acid and boric acid.
The composite adhesive is compounded by a synthetic adhesive and a natural adhesive in a compounding ratio of 1:1, wherein the synthetic adhesive is one or a composition of more of polymethacrylate, polyisobutylene and an ethylene-propylene copolymer, and the natural adhesive is one or two of natural rubber and rosin.
The antioxidant is diphenylamine or 2,6-di-tert-butyl-p-cresol.
The extreme pressure antiwear agent is zinc dialkyl dithiophosphate.
The antirust agent consists of benzotriazole and dodecenylsuccinic acid.
The invention relates to a preparation method of commercial vehicle wheel hub bearing lubricating grease, which comprises the following steps:
1) Adding 0.77-2.31wt% of overbased calcium sulfonate and 0.13-0.39wt% of transforming agent into a reaction kettle, stirring, heating to 90-100 ℃, and stirring for 35 minutes at constant temperature;
2) Adding 0.06-0.18wt% of saponification acid and 0.03-0.09wt% of saponification alkali (diluted with 3 times of water to obtain suspension when in use), heating to 140-150 deg.C, and stirring at constant temperature for 35 min;
3) Cooling to 90-100 deg.C, adding base oil and 4.41-6.62wt% of normal soap, stirring at constant temperature for 35 min;
4) Cooling to 83-87 deg.C, adding 0.45-0.95wt% lithium hydroxide (diluted with 9 times of water to obtain water solution when in use), heating to 140-150 deg.C, and stirring at constant temperature for 35 min;
5) Cooling to 90-100 ℃, adding the base oil, 0.42-0.95wt% of organic amine and 0.24-0.54wt% of carboxyl source, and stirring for 35 minutes at constant temperature;
6) Cooling to 65-75 ℃, adding 0.24-0.54wt% of hexamethylene diamine, base oil and 1.02-2.30wt% of diisocyanate within 40 +/-5 minutes, and stirring at constant temperature for 60-120 minutes;
7) Heating to 90-100 deg.C, adding 0.90-1.89wt% complexing agent, stirring, heating to 140-150 deg.C, and stirring at constant temperature for 35 min;
8) Cooling to 83-87 deg.C, adding 0.57-1.07wt% lithium hydroxide (diluted with 9 times of water to obtain water solution) within 60 + -5 min, stirring, heating to 140-150 deg.C, stirring at constant temperature for 60 min, heating to 220-240 deg.C, and stirring at constant temperature for 35 min;
9) Cooling to 140-150 ℃, adding the base oil, and stirring for 30 minutes at constant temperature;
10 Raising the temperature to 220-240 ℃ again, and stirring for 5 minutes at constant temperature;
11 Cooling to 170-190 deg.C, adding composite adhesive (composed of synthetic adhesive, natural adhesive, and base oil in balance), cooling to 90-100 deg.C, and adding antioxidant, extreme pressure antiwear agent, and antirust agent;
12 ) continuously cooling, cooling to 65-75 ℃, grinding and homogenizing.
The invention has the beneficial effects that:
1. the composite polyurea thickening agent, the composite calcium sulfonate thickening agent and the composite lithium thickening agent are compounded by an integrated synthesis method, so that the high-temperature stability and the colloid stability of the lubricating grease can be obviously improved, the oil content of the lubricating grease is reduced, the service life of a high-temperature bearing is prolonged, and the oil leakage risk of the lubricating grease is reduced; the extreme pressure property and the shearing resistance of the lubricating grease are improved, the consistency change of the lubricating grease is reduced, and the risk of throwing the lubricating grease is reduced.
2. The composition of the synthetic adhesive and the natural adhesive has a synergistic effect, the shear stability of the lubricating grease is obviously improved, the consistency change of the lubricating grease is reduced, the lubricating grease is well adhered to the surface of a friction pair, and the risk of grease throwing of the lubricating grease is reduced.
Detailed Description
Example 1
The commercial vehicle wheel hub bearing lubricating grease comprises the following raw material components in parts by weight: 81.4% of base oil, 15% of a composite thickening agent, 1.8% of a composite adhesive, 0.9% of an antioxidant, 0.9% of an extreme pressure antiwear agent and 0.005% of an antirust agent, wherein the composite polyurea thickening agent, the composite calcium sulfonate thickening agent, the composite lithium thickening agent = 2.
The preparation method comprises the following steps:
1) Adding 1.16wt% of overbased calcium petroleum sulfonate and 0.20wt% of water into a reaction kettle, stirring, heating to 90-100 ℃, and stirring at constant temperature for 35 minutes;
2) Adding 0.10wt% of dodecahydroxystearic acid and 0.05wt% of calcium hydroxide (diluted into suspension by 3 times of water when in use), heating to 140-150 ℃, and stirring at constant temperature for 35 minutes;
3) Cooling to 90-100 ℃, adding 30wt% of base oil and 6.62wt% of dodecahydroxystearic acid, and stirring for 35 minutes at constant temperature;
4) Cooling to 83-87 deg.C, adding 0.95wt% lithium hydroxide monohydrate (diluted with 9 times of water to obtain water solution when in use), heating to 140-150 deg.C, and stirring at constant temperature for 35 min;
5) Cooling to 90-100 ℃, adding 15wt% of base oil, 0.30wt% of cyclohexylamine, 0.33wt% of p-toluidine and 0.36wt% of caprolactam, and stirring for 35 minutes at constant temperature;
6) Cooling to 65-75 ℃, adding 0.36wt% of hexamethylene diamine, 15wt% of base oil and 1.53wt% of diphenylmethane-4,4-diisocyanate (MDI) within 40 +/-5 minutes, and stirring at constant temperature for 60-120 minutes;
7) Heating to 90-100 ℃, adding 1.26wt% of sebacic acid and 0.63wt% of boric acid, stirring, continuously heating to 140-150 ℃, and stirring at constant temperature for 35 minutes;
8) Cooling to 83-87 deg.C, adding 1.07wt% lithium hydroxide monohydrate (diluted with 9 times of water to obtain water solution in use) within 60 + -5 min, stirring, heating to 140-150 deg.C, stirring at constant temperature for 60 min, heating to 220-240 deg.C, and stirring at constant temperature for 35 min;
9) Cooling to 140-150 ℃, adding 20wt% of base oil, and stirring for 30 minutes at constant temperature;
10 Raising the temperature to 220-240 ℃ again, and stirring for 5 minutes at constant temperature;
11 Cooling to 170-190 deg.C, adding 1.80wt% of composite adhesive (composed of 0.90wt% of polymethacrylate, 0.90wt% of natural rubber and the balance base oil), continuously cooling to 90-100 deg.C, adding 0.90wt% of 2,6-di-tert-butyl p-cresol, 0.90wt% of zinc dialkyl dithiophosphate, 0.003wt% of benzotriazole and 0.002wt% of dodecenyl succinic acid;
12 ) continuously cooling, cooling to 65-75 ℃, grinding and homogenizing.
Example 2
The commercial vehicle wheel hub bearing lubricating grease comprises the following raw material components in parts by weight: 81.4% of base oil, 15% of a composite thickening agent, 1.8% of a composite adhesive, 0.9% of an antioxidant, 0.9% of an extreme pressure antiwear agent and 0.005% of an antirust agent, wherein the composite polyurea thickening agent, the composite calcium sulfonate thickening agent and the composite lithium thickening agent are as follows, and the weight ratio is as follows, namely, the weight ratio is 5.
The preparation method comprises the following steps:
1) Adding 2.31wt% of overbased calcium petroleum sulfonate and 0.39wt% of water into a reaction kettle, stirring, heating to 90-100 ℃, and stirring at constant temperature for 35 minutes;
2) Adding 0.18wt% of dodecahydroxystearic acid and 0.09wt% of calcium hydroxide (diluted into suspension by 3 times of water when in use), heating to 140-150 ℃, and stirring at constant temperature for 35 minutes;
3) Cooling to 90-100 ℃, adding 30wt% of base oil and 4.72wt% of dodecahydroxystearic acid, and stirring for 35 minutes at constant temperature;
4) Cooling to 83-87 deg.C, adding 0.68wt% lithium hydroxide monohydrate (diluted with 9 times of water to obtain water solution when in use), heating to 140-150 deg.C, and stirring at constant temperature for 35 min;
5) Cooling to 90-100 ℃, adding 15wt% of base oil, 0.45wt% of cyclohexylamine, 0.50wt% of p-toluidine and 0.54wt% of caprolactam, and stirring for 35 minutes at constant temperature;
6) Cooling to 65-75 ℃, adding 0.54wt% of hexamethylene diamine, 15wt% of base oil and 2.30wt% of diphenylmethane-4,4-diisocyanate (MDI) within 40 +/-5 minutes, and stirring at constant temperature for 60-120 minutes;
7) Heating to 90-100 ℃, adding 0.90wt% of sebacic acid and 0.45wt% of boric acid, stirring, continuously heating to 140-150 ℃, and stirring at constant temperature for 35 minutes;
8) Cooling to 83-87 deg.C, adding 0.86wt% lithium hydroxide monohydrate (diluted with 9 times of water to obtain water solution in use) within 60 + -5 min, stirring, heating to 140-150 deg.C, stirring at constant temperature for 60 min, heating to 220-240 deg.C, and stirring at constant temperature for 35 min;
9) Cooling to 140-150 ℃, adding 20wt% of base oil, and stirring for 30 minutes at constant temperature;
10 Raising the temperature to 220-240 ℃ again, and stirring for 5 minutes at constant temperature;
11 Cooling to 170-190 deg.C, adding 1.80wt% of composite adhesive (composed of 0.90wt% of polymethacrylate, 0.90wt% of natural rubber and the balance base oil), continuously cooling to 90-100 deg.C, adding 0.90wt% of 2,6-di-tert-butyl p-cresol, 0.90wt% of zinc dialkyl dithiophosphate, 0.003wt% of benzotriazole and 0.002wt% of dodecenyl succinic acid;
12 ) continuously cooling, cooling to 65-75 ℃, grinding and homogenizing.
Example 3
The commercial vehicle wheel hub bearing lubricating grease comprises the following raw material components in parts by weight: 87.8% of base oil, 10% of a composite thickening agent, 1.2% of a composite adhesive, 0.5% of an antioxidant, 0.5% of an extreme pressure antiwear agent and 0.001% of an antirust agent, wherein the composite polyurea thickening agent is a composite calcium sulfonate thickening agent and a composite lithium thickening agent = 2.
The preparation method comprises the following steps:
1) Adding 0.77wt% of overbased calcium petroleum sulfonate and 0.13wt% of water into a reaction kettle, stirring, heating to 90-100 ℃, and stirring for 35 minutes at constant temperature;
2) Adding 0.06wt% of dodecahydroxystearic acid and 0.03wt% of calcium hydroxide (diluted by 3 times of water to form suspension when in use), heating to 140-150 ℃, and stirring at constant temperature for 35 minutes;
3) Cooling to 90-100 ℃, adding 30wt% of base oil and 4.41wt% of dodecahydroxystearic acid, and stirring for 35 minutes at constant temperature;
4) Cooling to 83-87 deg.C, adding 0.63wt% lithium hydroxide monohydrate (diluted with 9 times of water to obtain water solution when in use), heating to 140-150 deg.C, and stirring at constant temperature for 35 min;
5) Cooling to 90-100 ℃, adding 15wt% of base oil, 0.20wt% of cyclohexylamine, 0.22wt% of p-toluidine and 0.24wt% of caprolactam, and stirring for 35 minutes at constant temperature;
6) Cooling to 65-75 ℃, adding 0.24wt% of hexamethylene diamine, 15wt% of base oil and 1.02wt% of diphenylmethane-4,4-diisocyanate (MDI) within 40 +/-5 minutes, and stirring at constant temperature for 60-120 minutes;
7) Heating to 90-100 ℃, adding 0.84wt% of sebacic acid and 0.42wt% of boric acid, stirring, continuously heating to 140-150 ℃, and stirring at constant temperature for 35 minutes;
8) Cooling to 83-87 deg.C, adding 0.71wt% lithium hydroxide monohydrate (diluted with 9 times of water to obtain water solution in use) within 60 + -5 min, stirring, heating to 140-150 deg.C, stirring at constant temperature for 60 min, heating to 220-240 deg.C, and stirring at constant temperature for 35 min;
9) Cooling to 140-150 ℃, adding 20wt% of base oil, and stirring for 30 minutes at constant temperature;
10 Raising the temperature to 220-240 ℃ again, and stirring for 5 minutes at constant temperature;
11 Cooling to 170-190 deg.C, adding 1.20wt% of composite adhesive (composed of 0.60wt% of polymethacrylate, 0.60wt% of natural rubber and the balance base oil), cooling to 90-100 deg.C, adding 0.50wt% of 2,6-di-tert-butyl p-cresol, 0.50wt% of zinc dialkyl dithiophosphate, 0.0005wt% of benzotriazole and 0.0005wt% of dodecenyl succinic acid;
12 ) continuously cooling, cooling to 65-75 ℃, grinding and homogenizing.
Example 4
The commercial vehicle wheel hub bearing lubricating grease comprises the following raw material components in parts by weight: 87.8% of base oil, 10% of a composite thickening agent, 1.2% of a composite adhesive, 0.5% of an antioxidant, 0.5% of an extreme pressure antiwear agent and 0.001% of an antirust agent, wherein the composite polyurea thickening agent, the composite calcium sulfonate thickening agent, the composite lithium thickening agent = 3.
The preparation method comprises the following steps:
1) Adding 1.54wt% of overbased calcium petroleum sulfonate and 0.26wt% of water into a reaction kettle, stirring, heating to 90-100 ℃, and stirring at constant temperature for 35 minutes;
2) Adding 0.12wt% of dodecahydroxystearic acid and 0.06wt% of calcium hydroxide (diluted by 3 times of water to form suspension when in use), heating to 140-150 ℃, and stirring at constant temperature for 35 minutes;
3) Cooling to 90-100 ℃, adding 30wt% of base oil and 3.15wt% of dodecahydroxystearic acid, and stirring for 35 minutes at constant temperature;
4) Cooling to 83-87 deg.C, adding 0.45wt% lithium hydroxide monohydrate (diluted with 9 times of water to obtain water solution when in use), heating to 140-150 deg.C, and stirring at constant temperature for 35 min;
5) Cooling to 90-100 ℃, adding 15wt% of base oil, 0.30wt% of cyclohexylamine, 0.33wt% of p-toluidine and 0.36wt% of caprolactam, and stirring for 35 minutes at constant temperature;
6) Cooling to 65-75 ℃, adding 0.36wt% of hexamethylene diamine, 15wt% of base oil and 1.53wt% of diphenylmethane-4,4-diisocyanate (MDI) within 40 +/-5 minutes, and stirring at constant temperature for 60-120 minutes;
7) Heating to 90-100 ℃, adding 0.60wt% of sebacic acid and 0.30wt% of boric acid, stirring, continuously heating to 140-150 ℃, and stirring at constant temperature for 35 minutes;
8) Cooling to 83-87 deg.C, adding 0.57wt% lithium hydroxide monohydrate (diluted with 9 times of water to obtain water solution in use) within 60 + -5 min, stirring, heating to 140-150 deg.C, stirring at constant temperature for 60 min, heating to 220-240 deg.C, and stirring at constant temperature for 35 min;
9) Cooling to 140-150 ℃, adding 20wt% of base oil, and stirring for 30 minutes at constant temperature;
10 Raising the temperature to 220-240 ℃ again, and stirring for 5 minutes at constant temperature;
11 Cooling to 170-190 deg.C, adding 1.20wt% composite adhesive (composed of 0.60wt% polymethacrylate, 0.60wt% natural rubber, and base oil, the rest), cooling to 90-100 deg.C, adding 0.50wt% 2,6-di-tert-butyl p-cresol, 0.50wt% zinc dialkyl dithiophosphate, 0.0005wt% benzotriazole, and 0.0005wt% dodecenyl succinic acid;
12 ) continuously cooling, cooling to 65-75 ℃, grinding and homogenizing.
Comparative example 1
The commercial vehicle wheel hub bearing lubricating grease comprises the following raw material components in parts by weight: 87.8% of base oil, 10% of composite thickening agent, 1.2% of composite adhesive, 0.5% of antioxidant, 0.5% of extreme pressure antiwear agent and 0.001% of antirust agent, wherein the composite calcium sulfonate thickening agent is composite lithium thickening agent =3:7.
The preparation method comprises the following steps:
1) Adding 2.31wt% of overbased calcium petroleum sulfonate and 0.39wt% of water into a reaction kettle, stirring, heating to 90-100 ℃, and stirring at constant temperature for 35 minutes;
2) Adding 0.18wt% of dodecahydroxystearic acid and 0.09wt% of calcium hydroxide (diluted into suspension by 3 times of water when in use), heating to 140-150 ℃, and stirring at constant temperature for 35 minutes;
3) Cooling to 90-100 ℃, adding 30wt% of base oil, 4.41wt% of dodecahydroxystearic acid, 0.84wt% of sebacic acid and 0.42wt% of boric acid, stirring, continuously heating to 140-150 ℃, and stirring at constant temperature for 35 minutes;
4) Cooling to 83-87 deg.C, adding 1.26wt% lithium hydroxide monohydrate (diluted with 9 times of water to obtain water solution), stirring, heating to 140-150 deg.C, stirring at constant temperature for 60 min, heating to 220-240 deg.C, and stirring at constant temperature for 35 min;
5) Cooling to 140-150 ℃, adding 20wt% of base oil, and stirring for 30 minutes at constant temperature;
6) Heating to 220-240 deg.c again, and stirring at constant temperature for 5 min;
7) Cooling to 170-190 deg.C, adding 1.20wt% composite adhesive (composed of 0.60wt% polymethacrylate, 0.60wt% natural rubber, and base oil, the rest), cooling to 90-100 deg.C, adding 0.50wt% 2,6-di-tert-butyl p-cresol, 0.50wt% zinc dialkyl dithiophosphate, 0.0005wt% benzotriazole, and 0.0005wt% dodecenyl succinic acid;
8) Continuously cooling to 65-75 ℃, grinding and homogenizing.
Comparative example 2
The commercial vehicle wheel hub bearing lubricating grease comprises the following raw material components in parts by weight: 87.8% of base oil, 10% of a composite thickening agent, 1.2% of a composite adhesive, 0.5% of an antioxidant, 0.5% of an extreme pressure antiwear agent and 0.001% of an antirust agent, wherein the composite polyurea thickening agent is a composite lithium thickening agent =3:7.
The preparation method comprises the following steps:
1) Cooling to 90-100 ℃, adding 30wt% of base oil and 4.41wt% of dodecahydroxystearic acid into the reaction kettle, stirring, heating to 90-100 ℃, and stirring at constant temperature for 35 minutes;
2) Cooling to 83-87 deg.C, adding 0.63wt% lithium hydroxide monohydrate (diluted with 9 times of water to obtain water solution when in use), heating to 140-150 deg.C, and stirring at constant temperature for 35 min;
3) Cooling to 90-100 ℃, adding 15wt% of base oil, 0.30wt% of cyclohexylamine, 0.33wt% of p-toluidine and 0.36wt% of caprolactam, and stirring for 35 minutes at constant temperature;
4) Cooling to 65-75 ℃, finishing adding 0.36wt% of hexamethylene diamine, 15wt% of base oil and 1.53wt% of diphenylmethane-4,4-diisocyanate (MDI) within 40 +/-5 minutes, and stirring for 60-120 minutes at constant temperature;
5) Heating to 90-100 ℃, adding 0.84wt% of sebacic acid and 0.42wt% of boric acid, stirring, continuously heating to 140-150 ℃, and stirring at constant temperature for 35 minutes;
6) Cooling to 83-87 deg.C, adding 0.75wt% lithium hydroxide monohydrate (diluted with 9 times of water to obtain water solution in use) within 60 + -5 min, stirring, heating to 140-150 deg.C, stirring at constant temperature for 60 min, heating to 220-240 deg.C, and stirring at constant temperature for 35 min;
7) Cooling to 140-150 ℃, adding 20wt% of base oil, and stirring for 30 minutes at constant temperature;
8) Heating to 220-240 deg.c again, and stirring at constant temperature for 5 min;
9) Cooling to 170-190 deg.C, adding 1.20wt% composite adhesive (composed of 0.60wt% polymethacrylate, 0.60wt% natural rubber, and base oil, the rest), cooling to 90-100 deg.C, adding 0.50wt% 2,6-di-tert-butyl p-cresol, 0.50wt% zinc dialkyl dithiophosphate, 0.0005wt% benzotriazole, and 0.0005wt% dodecenyl succinic acid;
10 ) continuously cooling, cooling to 65-75 ℃, grinding and homogenizing.
Comparative example 3
The commercial vehicle wheel hub bearing lubricating grease comprises the following raw material components in parts by weight: 87.8% of base oil, 10% of a composite thickening agent, 1.2% of a synthetic adhesive, 0.5% of an antioxidant, 0.5% of an extreme pressure antiwear agent and 0.001% of an antirust agent, wherein the composite polyurea thickening agent, the composite calcium sulfonate thickening agent, the composite lithium thickening agent = 2.
1) Adding 0.77wt% of high-alkalinity petroleum calcium sulfonate and 0.13wt% of water into a reaction kettle, stirring, heating to 90-100 ℃, and stirring for 35 minutes at constant temperature;
2) Adding 0.06wt% of dodecahydroxystearic acid and 0.03wt% of calcium hydroxide (diluted by 3 times of water to form suspension when in use), heating to 140-150 ℃, and stirring at constant temperature for 35 minutes;
3) Cooling to 90-100 ℃, adding 30wt% of base oil and 4.41wt% of dodecahydroxystearic acid, and stirring for 35 minutes at constant temperature;
4) Cooling to 83-87 deg.C, adding 0.63wt% lithium hydroxide monohydrate (diluted with 9 times of water to obtain water solution when in use), heating to 140-150 deg.C, and stirring at constant temperature for 35 min;
5) Cooling to 90-100 ℃, adding 15wt% of base oil, 0.20wt% of cyclohexylamine, 0.22wt% of p-toluidine and 0.24wt% of caprolactam, and stirring for 35 minutes at constant temperature;
6) Cooling to 65-75 ℃, adding 0.24wt% of hexamethylene diamine, 15wt% of base oil and 1.02wt% of diphenylmethane-4,4-diisocyanate (MDI) within 40 +/-5 minutes, and stirring at constant temperature for 60-120 minutes;
7) Heating to 90-100 ℃, adding 0.84wt% of sebacic acid and 0.42wt% of boric acid, stirring, continuously heating to 140-150 ℃, and stirring at constant temperature for 35 minutes;
8) Cooling to 83-87 deg.C, adding 0.71wt% of lithium hydroxide monohydrate (diluted with 9 times of water to obtain water solution when in use) within 60 + -5 min, stirring, heating to 140-150 deg.C, stirring at constant temperature for 60 min, heating to 220-240 deg.C, and stirring at constant temperature for 35 min;
9) Cooling to 140-150 ℃, adding 20wt% of base oil, and stirring for 30 minutes at constant temperature;
10 ) heating to 220-240 ℃ again, and stirring for 5 minutes at constant temperature;
11 Cooling to 170-190 deg.C, adding 1.20wt% synthetic adhesive (composed of 1.20wt% polymethacrylate and the balance base oil), cooling to 90-100 deg.C, adding 0.50wt% 2,6-di-tert-butyl p-cresol, 0.50wt% zinc dialkyl dithiophosphate, 0.0005wt% benzotriazole, and 0.0005wt% dodecenyl succinic acid;
12 ) continuously cooling, cooling to 65-75 ℃, grinding and homogenizing.
Comparative example 4
The commercial vehicle wheel hub bearing lubricating grease comprises the following raw material components in parts by weight: 87.8% of base oil, 10% of a composite thickening agent, 1.2% of a natural adhesive, 0.5% of an antioxidant, 0.5% of an extreme pressure antiwear agent and 0.001% of an antirust agent, wherein the composite polyurea thickening agent, the composite calcium sulfonate thickening agent, the composite lithium thickening agent = 2.
1) Adding 0.77wt% of high-alkalinity petroleum calcium sulfonate and 0.13wt% of water into a reaction kettle, stirring, heating to 90-100 ℃, and stirring for 35 minutes at constant temperature;
2) Adding 0.06wt% of dodecahydroxystearic acid and 0.03wt% of calcium hydroxide (diluted by 3 times of water to form suspension when in use), heating to 140-150 ℃, and stirring at constant temperature for 35 minutes;
3) Cooling to 90-100 ℃, adding 30wt% of base oil and 4.41wt% of dodecahydroxystearic acid, and stirring for 35 minutes at constant temperature;
4) Cooling to 83-87 deg.C, adding 0.63wt% lithium hydroxide monohydrate (diluted with 9 times of water to obtain water solution when in use), heating to 140-150 deg.C, and stirring at constant temperature for 35 min;
5) Cooling to 90-100 ℃, adding 15wt% of base oil, 0.20wt% of cyclohexylamine, 0.22wt% of p-toluidine and 0.24wt% of caprolactam, and stirring for 35 minutes at constant temperature;
6) Cooling to 65-75 ℃, adding 0.24wt% of hexamethylene diamine, 15wt% of base oil and 1.02wt% of diphenylmethane-4,4-diisocyanate (MDI) within 40 +/-5 minutes, and stirring at constant temperature for 60-120 minutes;
7) Heating to 90-100 ℃, adding 0.84wt% of sebacic acid and 0.42wt% of boric acid, stirring, continuously heating to 140-150 ℃, and stirring at constant temperature for 35 minutes;
8) Cooling to 83-87 deg.C, adding 0.71wt% of lithium hydroxide monohydrate (diluted with 9 times of water to obtain water solution when in use) within 60 + -5 min, stirring, heating to 140-150 deg.C, stirring at constant temperature for 60 min, heating to 220-240 deg.C, and stirring at constant temperature for 35 min;
9) Cooling to 140-150 ℃, adding 20wt% of base oil, and stirring for 30 minutes at constant temperature;
10 Raising the temperature to 220-240 ℃ again, and stirring for 5 minutes at constant temperature;
11 Cooling to 170-190 deg.C, adding 1.20wt% natural adhesive (composed of 1.20wt% natural rubber, and base oil), cooling to 90-100 deg.C, adding 0.50wt% 2,6-di-tert-butyl p-cresol, 0.50wt% zinc dialkyl dithiophosphate, 0.0005wt% benzotriazole, and 0.0005wt% dodecenyl succinic acid;
12 ) continuously cooling, cooling to 65-75 ℃, grinding and homogenizing.
The contents of the components of examples 1 to 4 and comparative examples 1 to 4 are shown in Table 1.
TABLE 1
Figure BDA0002131313480000111
Figure BDA0002131313480000121
Some of the performance data for examples 1-4 and comparative examples 1-4 are shown in Table 2.
TABLE 2
Figure BDA0002131313480000122
The composite polyurea thickening agent, the composite calcium sulfonate thickening agent and the composite lithium thickening agent are compounded by an integrated synthesis method, so that the high-temperature stability and the colloid stability of the lubricating grease can be obviously improved, the oil distribution amount of the lubricating grease is reduced, the service life of a high-temperature bearing is prolonged, and the oil leakage risk of the lubricating grease is reduced; the extreme pressure property and the shearing resistance of the lubricating grease are improved, the consistency change of the lubricating grease is reduced, and the risk of throwing the lubricating grease is reduced.
As can be seen from the comparison between example 3 and comparative examples 3-4 in Table 2, the composition of the synthetic adhesive and the natural adhesive has a synergistic effect, the shear stability of the grease is obviously improved, the consistency change of the grease is reduced, the grease is well adhered to the surface of a friction pair, and the risk of grease throwing of the grease is reduced.

Claims (11)

1. Commercial vehicle hub bearing grease, characterized in that the grease comprises the following raw material components by weight: 81-88wt% of base oil, 10-15wt% of composite thickening agent, 1.2-1.8wt% of composite adhesive, 0.5-0.9wt% of antioxidant, 0.5-0.9wt% of extreme pressure antiwear agent and 0.001-0.005wt% of antirust agent;
the base oil is a group II base oil, a group III base oil or a combination of the group II base oil and the group III base oil;
the composite thickening agent consists of a composite polyurea thickening agent, a composite calcium sulfonate thickening agent and a composite lithium thickening agent, wherein the weight ratio of the composite polyurea thickening agent to the composite calcium sulfonate thickening agent to the composite lithium thickening agent is (2;
the composite polyurea thickening agent is prepared by compounding 1.02-2.30wt% of diisocyanate, 0.66-1.49wt% of organic amine, 0.24-0.54wt% of carboxyl source and 0.08-0.18wt% of alkali metal;
wherein the diisocyanate is diphenylmethane-4,4-diisocyanate or toluene diisocyanate; the organic amine is one or the combination of more of cyclohexylamine, p-toluidine, decaamine, hexamethylene diamine and p-phenylenediamine; the carboxyl source is caprolactam or ethyl p-aminobenzoate; the alkali metal is lithium hydroxide;
the compound calcium sulfonate thickening agent is prepared by compounding 0.77-2.31wt% of high-alkalinity calcium sulfonate, 0.13-0.39wt% of transforming agent, 0.06-0.18wt% of saponification acid and 0.03-0.09wt% of saponification alkali; wherein the overbased calcium sulfonate is overbased calcium petroleum sulfonate or overbased synthetic calcium sulfonate; the transforming agent is water, acetic acid or methanol; the saponification acid is dodecahydroxystearic acid, dodecanoic acid, hexadecanoic acid or boric acid; the saponification alkali is calcium hydroxide or calcium carbonate;
the composite lithium thickening agent is prepared by compounding 4.41-6.62wt% of positive soap, 0.90-1.89wt% of complexing agent and 0.90-1.90wt% of lithium hydroxide; wherein the normal soap is dodecahydroxystearic acid or stearic acid; the complexing agent is one or the combination of more of sebacic acid, azelaic acid and boric acid;
the composite adhesive is compounded by a synthetic adhesive and a natural adhesive, wherein the compounding ratio is 1:1, the synthetic adhesive is one or a composition of more of polymethacrylate, polyisobutylene and an ethylene-propylene copolymer, and the natural adhesive is one or two of natural rubber and rosin;
the antioxidant is diphenylamine or 2,6-di-tert-butyl-p-cresol;
the extreme pressure antiwear agent is zinc dialkyl dithiophosphate;
the antirust agent consists of benzotriazole and dodecenylsuccinic acid;
the preparation method comprises the following steps:
1) Adding 0.77-2.31wt% of high-alkalinity calcium sulfonate and 0.13-0.39wt% of transforming agent into a reaction kettle, stirring, heating to 90-100 ℃, and stirring for 35 minutes at constant temperature;
2) Adding 0.06-0.18wt% of saponification acid and 0.03-0.09wt% of saponification alkali, diluting the saponification alkali with 3 times of water to obtain suspension when the saponification alkali is used, heating to 140-150 ℃, and stirring at constant temperature for 35 minutes;
3) Cooling to 90-100 deg.C, adding base oil and 4.41-6.62wt% of normal soap, stirring at constant temperature for 35 min;
4) Cooling to 83-87 deg.C, adding 0.45-0.95wt% lithium hydroxide, diluting with 9 times of water to obtain water solution, heating to 140-150 deg.C, and stirring at constant temperature for 35 min;
5) Cooling to 90-100 ℃, adding the base oil, 0.42-0.95wt% of organic amine and 0.24-0.54wt% of carboxyl source, and stirring for 35 minutes at constant temperature;
6) Cooling to 65-75 ℃, adding 0.24-0.54wt% of hexamethylene diamine, base oil and 1.02-2.30wt% of diisocyanate within 40 +/-5 minutes, and stirring at constant temperature for 60-120 minutes;
7) Heating to 90-100 deg.C, adding 0.90-1.89wt% complexing agent, stirring, heating to 140-150 deg.C, and stirring at constant temperature for 35 min;
8) Cooling to 83-87 deg.C, adding 0.53-1.13wt% lithium hydroxide within 60 + -5 min, diluting with 9 times of water to obtain water solution, stirring, heating to 140-150 deg.C, stirring at constant temperature for 60 min, heating to 220-240 deg.C, and stirring at constant temperature for 35 min;
9) Cooling to 140-150 ℃, adding the base oil, and stirring for 30 minutes at constant temperature;
10 ) heating to 220-240 ℃ again, and stirring for 5 minutes at constant temperature;
11 Cooling to 170-190 deg.C, adding composite adhesive, cooling to 90-100 deg.C, and adding antioxidant, extreme pressure antiwear agent, and antirust agent;
12 ) continuously cooling, cooling to 65-75 ℃, grinding and homogenizing.
2. The commercial wheel hub bearing grease of claim 1 wherein the diisocyanate is diphenylmethane-4,4-diisocyanate.
3. The commercial wheel hub bearing grease of claim 1 wherein the organic amine is a combination of cyclohexylamine and p-toluidine.
4. The commercial wheel hub bearing grease of claim 1 wherein the carboxyl source is caprolactam.
5. The commercial vehicle hub bearing grease of claim 1 wherein the overbased calcium sulfonate is overbased calcium petroleum sulfonate.
6. The commercial wheel hub bearing grease of claim 1 wherein the converting agent is water.
7. The commercial vehicle hub bearing grease of claim 1 wherein the saponified acid is dodecahydroxystearic acid.
8. The commercial wheel hub bearing grease of claim 1 wherein the saponified base is calcium hydroxide.
9. The commercial vehicle hub bearing grease of claim 1 wherein the normal soap is dodecahydroxystearic acid.
10. The commercial wheel hub bearing grease of claim 1 wherein the complexing agent is a combination of sebacic acid and boric acid.
11. A method of preparing the commercial wheel hub bearing grease of claim 1, comprising the steps of:
1) Adding 0.77-2.31wt% of overbased calcium sulfonate and 0.13-0.39wt% of transforming agent into a reaction kettle, stirring, heating to 90-100 ℃, and stirring for 35 minutes at constant temperature;
2) Adding 0.06-0.18wt% of saponification acid and 0.03-0.09wt% of saponification alkali, diluting the saponification alkali with 3 times of water to obtain suspension when the saponification alkali is used, heating to 140-150 ℃, and stirring at constant temperature for 35 minutes;
3) Cooling to 90-100 deg.C, adding base oil and 4.41-6.62wt% of normal soap, stirring at constant temperature for 35 min;
4) Cooling to 83-87 deg.C, adding 0.45-0.95wt% lithium hydroxide, diluting with 9 times of water to obtain water solution, heating to 140-150 deg.C, and stirring at constant temperature for 35 min;
5) Cooling to 90-100 ℃, adding the base oil, 0.42-0.95wt% of organic amine and 0.24-0.54wt% of carboxyl source, and stirring for 35 minutes at constant temperature;
6) Cooling to 65-75 ℃, adding 0.24-0.54wt% of hexamethylene diamine, base oil and 1.02-2.30wt% of diisocyanate within 40 +/-5 minutes, and stirring at constant temperature for 60-120 minutes;
7) Heating to 90-100 deg.C, adding 0.90-1.89wt% complexing agent, stirring, heating to 140-150 deg.C, and stirring at constant temperature for 35 min;
8) Cooling to 83-87 deg.C, adding 0.53-1.13wt% lithium hydroxide within 60 + -5 min, diluting with 9 times of water to obtain water solution, stirring, heating to 140-150 deg.C, stirring at constant temperature for 60 min, heating to 220-240 deg.C, and stirring at constant temperature for 35 min;
9) Cooling to 140-150 ℃, adding the base oil, and stirring for 30 minutes at constant temperature;
10 Raising the temperature to 220-240 ℃ again, and stirring for 5 minutes at constant temperature;
11 Cooling to 170-190 deg.C, adding composite adhesive, cooling to 90-100 deg.C, and adding antioxidant, extreme pressure antiwear agent, and antirust agent;
12 ) continuously cooling, cooling to 65-75 ℃, grinding and homogenizing.
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CN108865373B (en) * 2018-08-05 2021-08-17 杭州新港润滑科技有限公司 Composite calcium sulfonate polyurea mixed lubricating grease and preparation method thereof
CN112029558A (en) * 2020-08-20 2020-12-04 中国石油化工股份有限公司 Lubricating grease and preparation method and application thereof
CN117264682A (en) * 2023-11-21 2023-12-22 新乡市恒星科技有限责任公司 Lubricating grease composition for pulleys and preparation method thereof

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