CN108531263A - Lithium base grease and preparation method thereof - Google Patents

Lithium base grease and preparation method thereof Download PDF

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Publication number
CN108531263A
CN108531263A CN201810588136.7A CN201810588136A CN108531263A CN 108531263 A CN108531263 A CN 108531263A CN 201810588136 A CN201810588136 A CN 201810588136A CN 108531263 A CN108531263 A CN 108531263A
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Prior art keywords
lithium
oil
base grease
nano particle
heterocyclic ring
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Inventor
李士成
岳树伟
岳风树
王虹
童蓉
胡秋波
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Shenzhen City New Mstar Technology Ltd
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Shenzhen City New Mstar Technology Ltd
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Priority to CN201810588136.7A priority Critical patent/CN108531263A/en
Publication of CN108531263A publication Critical patent/CN108531263A/en
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    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M169/00Lubricating 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
    • C10M169/02Mixtures of base-materials and thickeners
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M139/00Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing atoms of elements not provided for in groups C10M127/00 - C10M137/00
    • C10M139/04Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing atoms of elements not provided for in groups C10M127/00 - C10M137/00 having a silicon-to-carbon bond, e.g. silanes
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    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M177/00Special 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
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    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2203/00Organic non-macromolecular hydrocarbon compounds and hydrocarbon fractions as ingredients in lubricant compositions
    • C10M2203/10Petroleum or coal fractions, e.g. tars, solvents, bitumen
    • C10M2203/1006Petroleum or coal fractions, e.g. tars, solvents, bitumen used as base material
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    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2203/00Organic non-macromolecular hydrocarbon compounds and hydrocarbon fractions as ingredients in lubricant compositions
    • C10M2203/10Petroleum or coal fractions, e.g. tars, solvents, bitumen
    • C10M2203/102Aliphatic fractions
    • C10M2203/1025Aliphatic fractions used as base material
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    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2203/00Organic non-macromolecular hydrocarbon compounds and hydrocarbon fractions as ingredients in lubricant compositions
    • C10M2203/10Petroleum or coal fractions, e.g. tars, solvents, bitumen
    • C10M2203/106Naphthenic fractions
    • C10M2203/1065Naphthenic fractions used as base material
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    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2207/00Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/10Carboxylix acids; Neutral salts thereof
    • C10M2207/12Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms
    • C10M2207/125Carboxylix 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
    • C10M2207/127Carboxylix 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
    • C10M2207/1276Carboxylix 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
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    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2207/00Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/10Carboxylix acids; Neutral salts thereof
    • C10M2207/12Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms
    • C10M2207/125Carboxylix 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
    • C10M2207/128Carboxylix 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
    • C10M2207/1285Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids containing hydroxy groups; Ethers thereof used as thickening agents
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    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2215/00Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
    • C10M2215/02Amines, e.g. polyalkylene polyamines; Quaternary amines
    • C10M2215/04Amines, e.g. polyalkylene polyamines; Quaternary amines having amino groups bound to acyclic or cycloaliphatic carbon atoms
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    • C10M2215/00Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
    • C10M2215/02Amines, e.g. polyalkylene polyamines; Quaternary amines
    • C10M2215/06Amines, e.g. polyalkylene polyamines; Quaternary amines having amino groups bound to carbon atoms of six-membered aromatic rings
    • C10M2215/064Di- and triaryl amines
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    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2219/00Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions
    • C10M2219/04Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions containing sulfur-to-oxygen bonds, i.e. sulfones, sulfoxides
    • C10M2219/044Sulfonic acids, Derivatives thereof, e.g. neutral salts
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    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2227/00Organic non-macromolecular compounds containing atoms of elements not provided for in groups C10M2203/00, C10M2207/00, C10M2211/00, C10M2215/00, C10M2219/00 or C10M2223/00 as ingredients in lubricant compositions
    • C10M2227/06Organic compounds derived from inorganic acids or metal salts
    • C10M2227/061Esters derived from boron
    • C10M2227/062Cyclic esters
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10NINDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2030/00Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
    • C10N2030/06Oiliness; Film-strength; Anti-wear; Resistance to extreme pressure
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    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
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    • C10N2030/00Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
    • C10N2030/10Inhibition of oxidation, e.g. anti-oxidants
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    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
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    • C10N2030/00Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
    • C10N2030/12Inhibition of corrosion, e.g. anti-rust agents or anti-corrosives
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    • C10N2050/00Form in which the lubricant is applied to the material being lubricated
    • C10N2050/10Semi-solids; greasy

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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 belongs to technical field of lubricating oil, and in particular to a kind of lithium base grease and preparation method thereof.It is in terms of 100% by the gross mass of the lithium base grease, the lithium base grease includes the ingredient of following mass percentage:Base oil 65 93%;Aliphatic acid lithium soap 5 20%;Lipophile nitrogen heterocyclic ring borate nano particle 1 5%;Other additives 0.5% 10%.The lithium base grease has good anti-extreme pressure and antifriction antiwear, and can improve the roughness of surface of friction pair, repairs surface polishing scratch, extends the secondary service life of friction.

Description

Lithium base grease and preparation method thereof
Technical field
The invention belongs to technical field of lubricating oil, and in particular to a kind of lithium base grease and preparation method thereof.
Background technology
With the rapid development of modern industry, lubricating oil proportion in rolling bearing and sliding bearing industry carries year by year It rises, industrial production sector is for various performances such as the high temperature resistant of lubricating oil, anti-extreme-pressure anti-wear, water resistant, protection, bearing lives It is proposed increasingly strict requirement.Modern excellent lubricating grease, can meet subzero 100 DEG C to 300 DEG C above freezing of temperature range, turn It is harsh can also to bear high vacuum, intense radiation and contact strong oxidizer etc. in 4500Mpa or more for 100,000 r/min of speed, contact stress The requirement of condition, accounts for consequence in national economy.
Lubricating grease is made of base oil, thickening agent and additive three parts, it is that thickening agent is distributed in base oil A kind of soft solid product formed, the property of lubricating grease are by its component and its to be formed by structural manufacturing process and determine, this three parts It is the principal element for influencing lubricating oil property.Domestic and foreign scholars have done numerous studies, and base oil directly affects the viscosity of lubricating grease, Thickening agent is the solid particle being dispersed in lubricating grease, and the content of thickening agent influences the thickness of lubrication, and additive improves The stability of lubricating grease, inoxidizability, rotproofness, fatigue resistance and surface adhesion.Experience before is by changing base Plinth oil adjusts viscosity, changes thickness and shape by adding different lubricating grease, but as user proposes more product Harsh requirement, is only uneconomic and faulty to meet the needs of users by both methods, therefore need to pass through Additive of different nature is added to increase its processing performance.The additive that the forties rises, such as wear-resistant anti-pole additive, antioxygen Change additive and dispersant etc., their appearance disclosure satisfy that a variety of environmental demands, be to carry high performance another effective ways.
The nano material state-of-the-art material of 21 century the most, due to its quantum size effect, small-size effect, skin effect With this four big effect of macro quanta tunnel effect, to have the physicochemical property not available for some traditional materials.Nanometer material Material is since large specific surface area, high diffusibility, easily absorption, the characteristics such as fusing point is low are to be considered novel lubriation material.Made It is added in lubricating grease for additive, there is good wear resistence, anti-contact fatigue, antifriction quality, improve high-temperature behavior, Neng Gouxian The bearing capacity for promoting lubricating grease is write, while nano material has good self-repair function in surface of friction pair.
China's grease product from via with the low calcium-base grease of technology and quality level occupy an leading position to Technology and the higher lithium base grease of quality level are occupied an leading position conversion.Lithium base grease have good colloid stability, The advantages that service life is long, applied widely is a kind of ideal long-life, multi-purpose grease, but it is using process In, inoxidizability, wearability, water-resistance and bearing capacity are still unsatisfactory.
Invention content
It is an object of the invention to overcome the above-mentioned deficiency of the prior art, a kind of lithium base grease and its preparation side are provided Method, it is intended to solve the anti-extreme pressure of existing lubricating grease and the technical problem that anti-attrition wear resistence is undesirable.
For achieving the above object, the technical solution adopted by the present invention is as follows:
One aspect of the present invention provides a kind of lithium base grease, is in terms of 100% by the gross mass of the lithium base grease, described Lithium base grease includes the ingredient of following mass percentage:
Another aspect of the present invention provides a kind of preparation method of above-mentioned lithium base grease, includes the following steps:
The base oil, aliphatic acid lithium soap, lipophile nitrogen heterocyclic ring borate nano particle and other additives are provided;
The base oil is divided into two parts, respectively first foundation oil and the second base oil;By the first foundation oil with After the aliphatic acid lithium soap mixing, the first heat treatment is carried out, the first mixed material is obtained;
After the first mixed material expanding treatment, second base oil is added, carries out the second heat treatment, obtains Second mixed material;
By second mixed material and the lipophile nitrogen heterocyclic ring borate nano particle and other described additives Mixing grinds after carrying out third heat treatment, obtains the lithium base grease.
The present invention provides a kind of novel lithium base grease, wherein the base oil and aliphatic acid lithium soap ingredient that contain, retain The advantages that good colloid stability of traditional lithium base grease, splendid mechanical stability, and by lipophile nitrogen heterocyclic ring boron Acid esters nano particle is added in lithium base grease, its lithium base is made to have good dispersibility in lubricating grease, nanostructure There is the anti-extreme pressure and antifriction antiwear for also further improving lithium base grease in lipophile nitrogen heterocyclic ring borate nano particle, And the particle of nanostructure can also act on surface of friction pair, improve the roughness of surface of friction pair, repair surface polishing scratch, Extend the secondary service life of friction;Meanwhile according to the ingredient of other additives difference, lithium base grease can be further improved Other performances such as inoxidizability, metal antirusting agent.In short, each ingredient in the lithium base grease and between content, passes through collaboration Effect, makes the comprehensive performance of lithium base grease reach best.
The preparation method of above-mentioned lithium base grease provided by the invention, simple for process, reproducible, required technique is set Standby cheap and simple, final lithium base grease obtained has good anti-extreme pressure and antifriction antiwear, and it is secondary to improve friction The roughness on surface repairs surface polishing scratch, extends the secondary service life of friction.
Specific implementation mode
In order to make technical problems, technical solutions and advantageous effects to be solved by the present invention be more clearly understood, below in conjunction with Embodiment, the present invention will be described in further detail.It should be appreciated that specific embodiment described herein is only used to explain The present invention is not intended to limit the present invention.
On the one hand, an embodiment of the present invention provides a kind of lithium base grease, the gross mass with the lithium base grease is 100% meter, the lithium base grease includes the ingredient of following mass percentage:
Above-mentioned lithium base grease provided in an embodiment of the present invention, wherein the base oil and aliphatic acid lithium soap ingredient that contain, are protected The advantages that having stayed the good colloid stability of traditional lithium base grease, splendid mechanical stability, and by lipophile nitrogen heterocyclic ring Borate nano particle is added in lithium base grease, its lithium base is made to have good dispersibility, nanostructure in lubricating grease Lipophile nitrogen heterocyclic ring borate nano particle exist and also further improve the anti-extreme pressure and antifriction antiwear of lithium base grease Property, and the particle of nanostructure can also act on surface of friction pair, improve the roughness of surface of friction pair, repair surface mill Trace extends the secondary service life of friction;Meanwhile according to the ingredient of other additives difference, lithium base lubrication can be further improved Other performances such as inoxidizability, metal antirusting agent of fat.In short, each ingredient in the lithium base grease and between content, passes through Synergistic effect, makes the comprehensive performance of lithium base grease reach best.
Further, in the lithium base grease of the embodiment of the present invention, the lipophile nitrogen heterocyclic ring borate nano particle For the nitrogen heterocyclic ring borate nano particle being surface-treated through silane coupling agent.Silane coupling agent is surface-treated nitrogen heterocyclic ring boric acid After ester nano particle, its lipophile is dramatically increased, its dispersibility in lubricating grease is made to be significantly better than common borate nanometer Particle.Preferably, the silane coupling agent includes trim,ethylchlorosilane, perfluoro decyl trimethyl silane, 17 fluorine decyl, three second At least one of oxysilane, N-2- aminoethyl -3- aminopropyl trimethoxysilanes.In one embodiment of the present invention, choosing Nitrogen heterocyclic ring borate nano particle is surface-treated with trim,ethylchlorosilane, detailed process is:By nitrogen heterocyclic ring boric acid Ester is with trim,ethylchlorosilane according to 1:0.1~0.5 mixing, and be dispersed in ethyl alcohol, 1.5h is heated at 90 DEG C, removes second Alcohol obtains lipophile nitrogen heterocyclic ring borate nano particle.
Further, the lipophile nitrogen heterocyclic ring borate nano particle is the chemical combination as shown in following formula I and/or Formula II The nano particle that object is formed;
(i.e. AMTB);
(i.e. AMOB);
Wherein, R1 and R2 is same or different silane coupling agent.
Above-mentioned silane coupling agent includes trim,ethylchlorosilane, perfluoro decyl trimethyl silane, 17 fluorine decyl triethoxies At least one of silane, N-2- aminoethyl -3- aminopropyl trimethoxysilanes.
Further, the grain size of above-mentioned lipophile nitrogen heterocyclic ring borate nano particle is preferably 10-20nm;In the grain The dispersibility of the lipophile nitrogen heterocyclic ring borate nano particle in lithium base grease reaches best within the scope of diameter.And the parent The specific surface area of oiliness nitrogen heterocyclic ring borate nano particle is preferably 150-250m2/ g, within the scope of the specific surface area, oleophylic Property nitrogen heterocyclic ring borate nano particle in lithium base grease with bigger contact area, lithium can be more effectively dispersed in In base grease.Specifically, lipophile nitrogen heterocyclic ring borate nano particle contains in the lithium base grease of the embodiment of the present invention Amount can be selected between 1-5%, such as 1%, 2%, 3%, 4%, 5%.
Further, in the lithium base grease of the embodiment of the present invention, other described additives include that netted thixotroping structure changes At least one of kind agent, antioxidant, metal antirusting agent, matal deactivator, extreme pressure anti-wear additives and corrosion inhibitor.According to other The ingredient of additive is different, can further improve lithium base grease other performances.
Netted thixotroping structural improvement agent is such as added in lithium base grease plays thickening power:When lubricating grease is sheared When, consistency becomes smaller, and when stopping shearing, can increase consistency again because adding netted thixotroping structural improvement agent;The present invention one is embodied In example, netted thixotroping structural improvement agent is preferably cetyl trimethylammonium bromide.It is such as added in lithium base grease anti-oxidant Agent prevents its oxidation, further increases service life;In a specific embodiment of the invention, antioxidant is alkyl diphenylamine.Such as Metal antirusting agent is added in lithium base grease, is prevented when using lithium base grease to corrosions such as equipment, instruments;The present invention one In specific embodiment, metal antirusting agent is preferably barium mahogany sulfonate.In addition, can also add matal deactivator, preferably methylbenzene And triazole derivative.Extreme pressure anti-wear additives are such as added in lithium base grease, to further increase the extreme-pressure anti-wear of lithium base grease Property;In a specific embodiment of the invention, the extreme pressure anti-wear additives are preferably borate.Specifically, the lithium base of the embodiment of the present invention The content of other above-mentioned additives in lubricating grease can be selected between 0.5-10%, such as 0.5%, 2%, 3%, 4%, 5%, 8%, 10% etc..
Further, in the lithium base grease of the embodiment of the present invention, the base oil include mineral oil, Esters oil, silicone oil, At least one of polyethers oil and synthesis hydrocarbon;Such as naphthenic base subtract three line base oil, 500N base oils, 150N base oils and light Gloss varnish etc..The content of above-mentioned base oil in the lithium base grease of the embodiment of the present invention can be selected between 65-93%, such as 65%, 68%, 70%, 72%, 75%, 78%, 80%, 93% etc..
Further, in the lithium base grease of the embodiment of the present invention, the aliphatic acid lithium soap includes 12- hydroxy lithium stearates At least one of soap, 9,10- dihydroxystearic acids lithium soap and 9,10,12- trihydroxy stearic acid lithium soap, stearic acid lithium soap.This The content of above-mentioned aliphatic acid lithium soap in the lithium base grease of inventive embodiments can be selected between 5-20%, such as 5%, 8%, 10%, 12%, 15%, 18%, 20% etc..
On the other hand, the embodiment of the present invention additionally provides a kind of preparation method of above-mentioned lithium base grease, including walks as follows Suddenly:
S01:The base oil, aliphatic acid lithium soap, lipophile nitrogen heterocyclic ring borate nano particle and other additions are provided Agent;
S02:The base oil is divided into two parts, respectively first foundation oil and the second base oil;By the first foundation It is oily mixed with the aliphatic acid lithium soap after, carry out first heat treatment, obtain the first mixed material;
S03:After the first mixed material expanding treatment, second base oil is added, carries out the second heat treatment, Obtain the second mixed material;
S04:Second mixed material and the lipophile nitrogen heterocyclic ring borate nano particle and described other are added Add agent to mix, is ground after carrying out third heat treatment, obtain the lithium base grease.
The preparation method of above-mentioned lithium base grease provided in an embodiment of the present invention, easily prepared, reproducible, required technique Equipment cheap and simple, final lithium base grease obtained has good anti-extreme pressure and antifriction antiwear, and can improve friction The roughness of secondary surface repairs surface polishing scratch, extends the secondary service life of friction.
Further, in above-mentioned preparation method, the weight ratio of the first foundation oil and second base oil is 2:1. 2/3 base oil is mixed into row first with aliphatic acid lithium soap to heat, there is the condition of preferred first heat treatment For:160-180 DEG C of temperature, time 5-20min.
Further, expanding treatment is carried out after the first heat treatment, to improve stability.The optimum condition of expanding treatment For:200-220 DEG C of temperature, the puffing 5-10min of true solution.After puffing, remaining 1/3 base oil is added, carries out the second heating Processing;Base oil is set to be sufficiently mixed uniformly with aliphatic acid lithium soap.Specifically, the condition of the second heat treatment is:Temperature 160-180 DEG C, time 5-10min.
Further, the condition of the third heat treatment is:105-110 DEG C of temperature, time 5-10min;I.e. at this Under the conditions of the second mixed material and the lipophile nitrogen heterocyclic ring borate nano particle and other described additives are mixed into Row heating, then grinding obtain finely dispersed lithium base grease.
In addition, above-mentioned aliphatic acid lithium soap can be obtained by saponification.Detailed process is:Aliphatic acid and lithium hydroxide are mixed It closes, carries out saponification.The condition of saponification is preferably:It is permanent when temperature is 90-110 DEG C, and pressure is 0.3-0.6Mpa Warm constant pressure heats 30-60min.The saponification synchronous with above-mentioned first heat treatment can carry out, in this way can be by aliphatic acid, hydrogen Lithia and base oil, which are mixed, carries out the first heating, carries out saponification, can reduce processing step, saves the energy.Into one Step ground, the aliphatic acid is preferably 12- hydroxy stearic acids, 9,10-dihydroxystearic acid and 9, and 10,12- trihydroxies are hard etc..
The present invention successively carried out test of many times, and it is further detailed to invention progress as reference now to lift A partial experiment result Thin description, is described in detail with reference to specific embodiment.
Embodiment 1
The preparation of lipophile nitrogen heterocyclic ring borate nano particle
Nitrogen heterocyclic ring borate nano particle carries out oleophylic processing using trim,ethylchlorosilane.Preparation method includes:It will Nitrogen heterocyclic ring borate nano particle is with trim,ethylchlorosilane according to 1:0.1~0.5 molar ratio mixing, and it is dispersed in second In alcohol, 1.5h is heated at 90 DEG C, removes ethyl alcohol, obtains the nitrogen heterocyclic ring borate nano particle of oleophylic processing.
Embodiment 2
The preparation of lithium base grease
1) mixed base oil that will be made of the 500N base oils of 25% bright stock, 40% and 35% 150N base oils Volume 1.5M is added in 400kg, 12 hydroxy stearic acid 120kg, lithium hydroxide 30kg and water 150kg3Autoclave pressure in, it is closed, stir It mixes.
2) heating pressurization, by 1-2.8h, when pressurization temperature in the kettle reaches 90-110 DEG C, pressure reaches 0.3-0.6Mpa When, stop heating, keep constant temperature and pressure 30-60min in autoclave, carries out saponification.
3) after the completion of saponification, the pressure in autoclave is discharged, normal pressure state is become, is warming up to 140~160 DEG C, it is dehydrated 10~30min, until being escaped without steam.It is added by 28% bright stock, 50% 500N base oils and 22% 150N The mixed base oil 100kg of base oil composition.
4) continue heating stirring, stop heat temperature raising under normal pressure when temperature rises to 200-220 DEG C, constant temperature 5-10min, then Be added by 28% bright stock, 50% 500N base oils and 22% the mixed base oil 100kg that forms of 150N base oils, turn Enter to reconcile kettle.
5) circulation temperature lowering is sheared by mechanical pump to 110 DEG C to 120-130 DEG C in reconciliation kettle, is added at 105-110 DEG C 6kg lipophile nitrogen heterocyclic ring borate nano particles, 2.5kg alkyl diphenylamines and 0.8kg barium mahogany sulfonates, stir evenly and adjust Whole consistency.
6) lubricating grease is ground using s65 type three-roll grinders, is slightly ground for three times, it is three times thin grind after obtain product.
Embodiment 3
The preparation of lithium base grease
1) by naphthenic base subtract three line base oil 400kg, 9,10- dihydroxystearic acids 120kg, decanedioic acid 10kg, hydroxide Volume 1.5m is added in lithium 30kg, water 150kg and boric acid 5.5kg3Autoclave pressure in, it is closed, stirring.
2) heating pressurization, by 1-2.8h, when pressurization temperature in the kettle reaches 90-110 DEG C, pressure reaches 0.3-0.6Mpa When, stop heating, keep constant temperature and pressure 5-20min in autoclave, carries out saponification.
3) after the completion of saponification, the pressure in autoclave is discharged, normal pressure state is become, is warming up to 140~160 DEG C, it is dehydrated 10~30min, until being escaped without steam.The naphthenic base line base oil 100kg that subtracts three is added.
4) continue heating stirring, stop heat temperature raising under normal pressure when temperature rises to 200-220 DEG C, constant temperature 5-10min, then The naphthenic base line base oil 100kg that subtracts three is added, is transferred to reconciliation kettle.
5) circulation temperature lowering is sheared by mechanical pump to 110 DEG C to 120-130 DEG C in reconciliation kettle, is added at 105-110 DEG C 12kg lipophile nitrogen heterocyclic ring borate nano particles, 3.5kg cetyl trimethylammonium bromides, 2.5kg alkyl diphenylamines and 0.8kg barium mahogany sulfonates stir evenly and adjust consistency.
6) lubricating grease is ground using s65 type three-roll grinders, is slightly ground for three times, it is three times thin grind after obtain product.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention All any modification, equivalent and improvement etc., should all be included in the protection scope of the present invention made by within refreshing and principle.

Claims (10)

1. a kind of lithium base grease, which is characterized in that by the gross mass of the lithium base grease be 100% in terms of, the lithium Ji Run Consistent lubricant includes the ingredient of following mass percentage:
2. lithium base grease as described in claim 1, which is characterized in that the lipophile nitrogen heterocyclic ring borate nano particle For the nitrogen heterocyclic ring borate nano particle being surface-treated through silane coupling agent.
3. lithium base grease as claimed in claim 2, which is characterized in that the lipophile nitrogen heterocyclic ring borate nano particle The nano particle formed for such as following formula I and/or Formula II compound represented;
Wherein, R1 and R2 is same or different silane coupling agent.
4. lithium base grease as claimed in claim 2, which is characterized in that the silane coupling agent include trim,ethylchlorosilane, In perfluoro decyl trimethyl silane, 17 fluorine ruthenium triethoxysilanes, N-2- aminoethyl -3- aminopropyl trimethoxysilanes It is at least one.
5. lithium base grease as described in claim 1, which is characterized in that the lipophile nitrogen heterocyclic ring borate nano particle Grain size be 10-20nm;And/or
The specific surface area of the lipophile nitrogen heterocyclic ring borate nano particle is 150-250m2/g。
6. lithium base grease as described in claim 1, which is characterized in that other described additives include that netted thixotroping structure changes At least one of kind agent, antioxidant, metal antirusting agent, matal deactivator, extreme pressure anti-wear additives and corrosion inhibitor;And/or
The base oil includes at least one of mineral oil, Esters oil, silicone oil, polyethers oil and synthesis hydrocarbon;And/or
The aliphatic acid lithium soap includes 12- hydroxy stearic acids lithium soap, 9,10- dihydroxystearic acids lithium soap and 9,10,12- trihydroxies At least one of stearic acid lithium soap, aliphatic acid lithium soap.
7. lithium base grease as claimed in claim 6, which is characterized in that the netted thixotroping structural improvement agent is cetyl Trimethylammonium bromide;And/or
The antioxidant is alkyl diphenylamine;And/or
The metal antirusting agent is barium mahogany sulfonate;And/or
Shown matal deactivator be methylbenzotrazole derivative and/or
The extreme pressure anti-wear additives are borate.
8. such as the preparation method of claim 1-7 any one of them lithium base greases, which is characterized in that include the following steps:
The base oil, aliphatic acid lithium soap, lipophile nitrogen heterocyclic ring borate nano particle and other additives are provided;
The base oil is divided into two parts, respectively first foundation oil and the second base oil;By the first foundation oil with it is described After the mixing of aliphatic acid lithium soap, the first heat treatment is carried out, the first mixed material is obtained;
After the first mixed material expanding treatment, second base oil is added, carries out the second heat treatment, obtains second Mixed material;
Second mixed material is mixed with the lipophile nitrogen heterocyclic ring borate nano particle and other described additives, It is ground after carrying out third heat treatment, obtains the lithium base grease.
9. claim require 8 as described in preparation method, which is characterized in that it is described first heat treatment condition be:Temperature 160-180 DEG C, time 5-20min;And/or
It is described second heat treatment condition be:160-180 DEG C of temperature, time 5-10min;And/or
The condition of third heat treatment is:105-110 DEG C of temperature, time 5-10min;And/or
The condition of the expanding treatment is:200-220 DEG C of temperature, the puffing 5-10min of true solution;And/or
The weight ratio of the first foundation oil and second base oil is 2:1.
10. the preparation method as described in claim requires 8, which is characterized in that the preparation method of the aliphatic acid lithium soap includes: Aliphatic acid is mixed with lithium hydroxide, carries out saponification.
CN201810588136.7A 2018-06-08 2018-06-08 Lithium base grease and preparation method thereof Pending CN108531263A (en)

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CN113201390A (en) * 2021-04-27 2021-08-03 北京化工大学 Antifriction heat-resistant lithium-based grease and preparation method thereof

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Application publication date: 20180914