CN106867630A - Environment-friendly type high performance antiwear additive - Google Patents
Environment-friendly type high performance antiwear additive Download PDFInfo
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- CN106867630A CN106867630A CN201710001740.0A CN201710001740A CN106867630A CN 106867630 A CN106867630 A CN 106867630A CN 201710001740 A CN201710001740 A CN 201710001740A CN 106867630 A CN106867630 A CN 106867630A
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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
- C10M163/00—Lubricating compositions characterised by the additive being a mixture of a compound of unknown or incompletely defined constitution and a non-macromolecular compound, each of these compounds being essential
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
- C10M2201/04—Elements
- C10M2201/041—Carbon; Graphite; Carbon black
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
- C10M2201/06—Metal compounds
- C10M2201/065—Sulfides; Selenides; Tellurides
- C10M2201/066—Molybdenum sulfide
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
- C10M2207/28—Esters
- C10M2207/281—Esters of (cyclo)aliphatic monocarboxylic acids
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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
- C10M2209/00—Organic macromolecular compounds containing oxygen as ingredients in lubricant compositions
- C10M2209/10—Macromolecular compoundss obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- C10M2209/103—Polyethers, i.e. containing di- or higher polyoxyalkylene groups
- C10M2209/104—Polyethers, i.e. containing di- or higher polyoxyalkylene groups of alkylene oxides containing two carbon atoms only
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2209/00—Organic macromolecular compounds containing oxygen as ingredients in lubricant compositions
- C10M2209/10—Macromolecular compoundss obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- C10M2209/103—Polyethers, i.e. containing di- or higher polyoxyalkylene groups
- C10M2209/108—Polyethers, i.e. containing di- or higher polyoxyalkylene groups etherified
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2219/00—Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions
- C10M2219/04—Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions containing sulfur-to-oxygen bonds, i.e. sulfones, sulfoxides
- C10M2219/044—Sulfonic acids, Derivatives thereof, e.g. neutral salts
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- 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
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
- C10N2030/10—Inhibition of oxidation, e.g. anti-oxidants
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
- C10N2030/12—Inhibition of corrosion, e.g. anti-rust agents or anti-corrosives
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- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Organic Chemistry (AREA)
- Lubricants (AREA)
Abstract
Environment-friendly type high performance antiwear additive, in parts by weight, its preparing raw material includes：100 parts of sulfonated graphene, 8 12 parts of terpinyl acetate, 46 parts of nano molybdenum disulfide, 14 16 parts of anion surfactant, 55 75 parts of solvent naphtha.
Description
Technical field
The invention belongs to oil product Technical Development Area, more particularly to a kind of environment-friendly type high performance antiwear additive.
Background technology
The most important functions of lubricant are to reduce friction and wear, and in some cases, only when lubricant is present
When two supporting surfaces be possible to carry out relative motion.Lubricant main landing low friction and the work for slowing down abrasion in machinery
With, with ensure it is mechanical effectively and long-term work, that is, play lubrication.Next plays cooling effect, and lubricant can be by mechanical friction
When the torrid zone that produces walk, keep certain thermal equilibrium state, control machinery works within the scope of certain temperature, prevents temperature not
Break and raise and part of damage.
In classical lubrication theory, lubrication is divided into fluid lubrication and boundary lubrication.In boundary lubrication, metal surface
When being solely subjected to moderate duty, if any a kind of additive can adsorb on the metal surface or with metal surface reaction, formed adsorbed film
Or reaction film, to prevent the sharp wear of metal surface, this additive to be referred to as antiwear additive.
Conventional lubrication oil antiwear additive, by active element point, can be divided into sulphur class antiwear additive (including olefine sulfide (SIB and
HPSIB), sulfurised ester and sulfurized oil etc.), Phosphorus antiwear additive (including (acidity) phosphate, phosphite ester, phosphonate ester etc.),
Halogen class antiwear additive (including chlorinated paraffin, chlorohydrocarbon, chlorinated fatty acid etc.), organic metal class (including lead naphthenate and dialkyl group
Dithiophosphates (ZnDDP) etc.), boron class antiwear additive (including inorganic borate and organic boric acid ester) etc..
But the continuous improvement of the requirement and health perception with the fast development of modern industry and the mankind to autogenous environment, this
A little list active element type antiwear additives have been increasingly difficult to meet the requirement of harsh operating mode and era development to them.As chlorine class is wear-resistant
Agent is disabled to the country such as U.S. and the West Europe that have been had by its toxicity problem；Lead naphthenate also because ecological and toxicity problem gradually by
Eliminate；The P and S that sulphur class, Phosphorus antiwear additive and ZnDDP contain by it can make catalyst poisoning, influence oxygen in tail gas converter
Gas sensor measurement accuracy and the toxicity to ecological environment, are used by international regulations limitation, and boron class antiwear additive there is also
Dispersion stabilization and water sensitivity problem etc..
Zinc dialkyl dithiophosphate (ZnDDP) is current most popular antiwear additive, but the phosphorous conversion of ZnDDP
Product can be used in the catalyst reduced in vehicle exhaust in the catalyst of noxious gas emission such as nitrogen oxides (NOx)
Poison simultaneously influences oxygen sensor；ZnDDP can produce ash content to block filtration system, the particle trapper of diesel engine can be produced bad
Influence；Element Zn can make some alloy bearings (referring mainly to argentiferous, lead part) produce electrochemical corrosion；In the work higher than 160 DEG C
Anti-oxidant and extreme pressure and antiwear behavior can be lost because drastically decomposing under condition.
Generally research is boron class antiwear additive and rare earth metal class antiwear additive with cooperate with wear-resistant effect.Rare earth metal class
Antiwear additive can occur friction chemical reaction in friction process in itself, in simple substance, oxygen of the surface of friction pair generation by rare earth metal
Compound, sulfide (sulfate), the chemical reaction film of phosphate composition.Boron class antiwear additive also can be in friction process in friction pair
One layer of protecting film containing the composition such as pure boron and its oxide, FexOy of Surface Creation.The presence of rare earth metal can be to boron to rubbing
" friction is urged and oozed " effect is played in the diffusion for wiping secondary sub-surface, and along with the osmosis of itself, they can be in friction pair Asia table
Face forms the friction co-penetration layer of rare earth metal-boron so that material hardness increases, wearability enhancing.But boron compound is easy
Produce hydrolysis.
The content of the invention
In order to solve prior art problem, the first aspect of the present invention provides a kind of environment-friendly type high performance antiwear additive, with weight
Amount part meter, its preparing raw material includes：100 parts of sulfonated graphene, terpinyl acetate 8-12 parts, nano molybdenum disulfide 4-6 parts, it is cloudy from
Sub- surfactant 14-16 parts, solvent naphtha 55-75 parts.
In some embodiments, the preparing raw material of the environment-friendly type high performance antiwear additive also includes lithium niobate 8-12 parts.
In some embodiments, the sulfonation degree of institute's sulfonated graphene is 1%-5%.
In some embodiments, the solvent naphtha is selected from least in D40, D70, D80, D85, D90, D95, D100
Kind.
In some embodiments, the particle diameter of the nano molybdenum disulfide is 70-100nm.
In some embodiments, the anion surfactant contains sulfonic acid group.
In some embodiments, the anion surfactant is selected from alkylbenzenesulfonate, alkylsulfonate, oil
One kind in sulfonate.
The second aspect of the present invention provides application of the environment-friendly type high performance antiwear additive as described above in oil product industry.
The third aspect of the present invention provides a kind of lubricating oil, contains environment-friendly type high performance antiwear additive as described above.
In some embodiments, the content of the environment-friendly type high performance antiwear additive in the lubricating oil is 0.5-5wt%.
The environment-friendly type high performance antiwear additive that the present invention is provided has good oil-soluble, not only with very excellent extreme pressure
Performance, wear-resistant and Wear vesistance, also with preferable corrosion resistance, inoxidizability, can extensively should as lube oil additive
For in lubricating oil.
Specific embodiment
Unless otherwise defined, all technologies used herein and scientific terminology have and the common skill of art of the present invention
The identical implication that art personnel are generally understood that.When there is contradiction, the definition in this specification is defined.
Quality, concentration, temperature, time, or other values or parameter it is preferred with scope, preferred scope or a series of upper limits
During the Range Representation that value and lower preferable values are limited, this is appreciated that and specifically discloses by any range limit or preferred value
The all scopes formed with any pairing of any range lower limit or preferred value, regardless of whether whether the scope separately discloses.
For example, the scope of 1-50 be understood to include selected from 1,2,3,4,5,6,7,8,9,10,11,12,13,14,15,16,17,18,
19、20、21、22、23、24、25、26、27、28、29、30、31、32、33、34、35、36、37、38、39、40、41、42、43、
44th, 45,46,47,48,49 or 50 any numeral, number combinatorics on words or subrange and all between above-mentioned integer
Fractional value, for example, 1.1,1.2,1.3,1.4,1.5,1.6,1.7,1.8 and 1.9.It is specific to consider from scope on subrange
Interior any end points starts " the nested subrange " for extending.For example, the nested subrange of exemplary range 1-50 can include
1-10,1-20,1-30 and 1-40 on one direction, or 50-40,50-30,50-20 and 50-10 on other direction.
The first aspect of the present invention provides a kind of environment-friendly type high performance antiwear additive, and in parts by weight, its preparing raw material includes：
100 parts of sulfonated graphene, terpinyl acetate 8-12 parts, nano molybdenum disulfide 4-6 parts, anion surfactant 14-16 parts, it is molten
55-75 parts of agent oil.
It is perfect condition that lubricating oil maintains fluid lubrication, usually occurs other states in real work, when in border
During friction, lubricating oil reduces fretting wear and prevents the ability of metal sintering from claiming lubricity.The lubricity of lubricating oil depends on it
Oiliness and extreme pressure property.Oiliness is sorptive on frictional metal surface lubricating oil.Polar molecule is aligned in lubricating oil
Absorption forms adsorbed film on the metal surface, and this film is typically only capable in normal temperature, low speed, underload or middle temperature, middling speed, middle load
In the case of, keep boundary lubrication.When high pressure, high temperature, high speed, adsorbed film desorption, oiliness failure.Extreme pressure property is that lubricating oil exists
The chemical reactivity of friction surface.When sulfur-bearing, phosphorus, chlorine compound additive is added in oil, these compounds are decomposed under high temperature
The active element of generation forms chemical reaction film with metal, compared with metallic matrix the fusing point and shear strength of film all than relatively low,
Friction and wear can be reduced.Effective boundary lubrication requirement reaction film thickness is more than 1nm.The greasy property of lubricating oil is general with rubbing
Wipe abrasion tester to evaluate, have four-ball tester, ring block abrasion tester, the method Simon Rex (Flxa) commonly used in these experiments are tested
Machine, SAE machine etc..
Four-ball tester is a kind of now widely used simple frictional testing machine, and its friction element is a diameter of by four
The steel ball of 12.7mm is constituted.Three steel balls (bottom ball) are stuck in oil sample cup jam-packed mutually and do not roll to each other below
Dynamic, pasta flooded bottom ball in cup.Upper ball (heading) is fixed in rotating shaft by spring chuck or nut, by machine shaft band during experiment
Dynamic rotation.Relying on institute's application of load on cross bar makes the following upward jack-up of three balls be pressed in ball bottom, between upper ball and following three ball
The load that is squeezed makees point contact, line slip friction of going forward side by side.Load (pressure), rotating speed, time and temperature can be choosing during experiment
Select.Within the perdurabgility of regulation experiment, depending on the size of load, abrasion spot, upper ball can be produced to be likely to lower ball on the ball of bottom
It is melted together by weldering.Four-ball tester simple structure, the sample quantities needed for experiment are few every time, pressed in testpieces contact point unit area
Power is larger, and result of the test repeatability is preferably, and separating capacity is strong.
Experimental condition：The speed of mainshaft is 1420-1500rpm, and temperature is room temperature, and load 60-8000N is divided into 22 loads
Level, specifies to operate 10s per under first order load from low to high, is added to untill steel ball sinters until load.And in every operating 10s
Afterwards, the wear scar diameter of steel ball is measured, grinding defect diameter and corresponding load according to steel ball are drawn on log-log paper
Abrasion-load curve.
Graphene (Graphene) is a kind of cellular flat film formed with sp2 hybrid forms by carbon atom, is one
The quasi- two-dimensional material of only one of which atomic layer level thickness is planted, so be called doing monoatomic layer graphite.Its thickness is about
, there are different fluctuatings according to the difference of preparation method in 0.335nm, generally in height about 1nm or so of vertical direction, water
It is the basic structural unit of all carbon crystals in addition to diamond square to width about 10nm to 25nm.
Graphene can be by physics and chemistry such as micromechanics stripping, chemical vapor deposition, epitaxial growth and redox
Method is obtained.Micromechanics stripping method is the method for making it successively separate to the effective external force of graphite linings applying.Use the method
The Graphene that purity is higher and defect is little can be synthesized.Have the disadvantage to be difficult to control to the size of single-layer graphene film, not only yield, weight
Renaturation is also poor, it is difficult to carry out large-scale production.Chemical vapour deposition technique is that under high temperature, gaseous atmosphere, carbonaceous gas is in reaction
Graphene presoma is first generated in chamber, hot matrix surface is then deposited into and the technology of prepared solid material.The method
The Graphene stock size of synthesis is larger and high-quality.Epitaxial growth method is with carborundum as raw material, in ultrahigh vacuum, high temperature 1300
It is pyrolyzed under the conditions of DEG C, surface silicon atoms are evaporated and leave surface, very thin graphite linings are just formed on silicon carbide substrates
.Heating-up temperature determines the number of plies of Graphene.The shortcoming of silicon carbide epitaxial growth method is harsh preparation condition, it is difficult to control carbonization
The decomposition of silicon, can form defect, with many crystalline domain structures, be difficult to isolate the Graphene of preparation, and carborundum material from substrate
Material is sufficiently expensive, so as to limit the extensive use of the method.Advantage is the single or multiple lift Graphene that can obtain large area.Oxidation
Reducing process is to obtain Graphene by using operations such as ultrasound, centrifugation and reduction.The method is mainly graphite oxidation into oxidation first
Graphite (GO), GO is reduced to obtain reduzate, as Graphene (RGO) again.
The sulfonated graphene is obtained by the sulfonated reaction of Graphene.
Sulfonating reaction is directed to organic molecule and introduces sulfonic group (- SO3H), sulphonate-base (such as-SO3Na) or sulphonyl halogen (-
SO2X chemical reaction), wherein the reaction for introducing sulphonyl halogen can be defined as halogen sulfonating reaction again.Drawn according to sulfonating reaction
The substitution base for entering, the product of sulfonating reaction can be sulfonic acid (RSO3H), sulfonate (RSO3M, M are ammonium or metal ion) or sulphonyl
Halogen (RSO2X).Different according to the atom being connected in sulphur atom in sulfonic group and organic molecule, the product for obtaining can be and carbon
Connected sulfoacid compound (the RSO of atom3H)；Sulfuric ester (the ROSO being connected with oxygen atom3H)；The sulfanilamide (SN) being connected with nitrogen-atoms
Compound (RNHSO3H)。
The species of sulfonating agent is more, and reaction mechanism is also different.Have plenty of electrophilic reaction, such as sulfuric acid, sulfur trioxide, smoke
Sulfuric acid etc.；Have plenty of necleophilic reaction, such as sodium sulfite, sodium hydrogensulfite；Have plenty of radical reaction, such as sulfur dioxide and chlorine
Gas, sulfur dioxide and oxygen etc..Sulfonation on phenyl ring is electrophilic reaction.First be electrophilic reagent attack phenyl ring, generation carbon just from
Son, then loses a proton, generates benzene sulfonic acid or substituted benzenesulfonic acid.
Conventional sulfonating agent has sulfur trioxide, the concentrated sulfuric acid, oleum, chlorosulfonic acid.
Sulfur trioxide is a kind of colourless easy-sublimation solid, with three kinds of thing phases.Reacted using sulfur trioxide as sulfonating agent
Speed is fast, and volume of equipment is small, and need not additionally heat.Because the activity of sulfur trioxide is big, respond is strong, and will not give birth to
Cheng Shui, the consumption of sulfur trioxide can not need concentrating waste acid close to theoretical amount after sulfonation, be produced without neutralizing spent acid
Unnecessary neutral salt, has the advantages that other sulfonating agents are incomparable.But it has the disadvantage that sulfonating reaction heat release acutely, is easily led
The accessory substance such as Substrate hydrolysis or generation sulfone class is caused, and the viscosity of reactant is high, comes difficult to heat transmission belt.
The concentrated sulfuric acid is a kind of strong mineral acid with high corrosiveness, and the concentrated sulfuric acid has strong oxidizing property, dehydration property, deep-etching
Property, difficult volatility, acidity, water imbibition.When the concentrated sulfuric acid is as sulfonating agent, the side reaction of generation is less, but sulfonating reaction is anti-
Answer speed slower.Often generation 1mol sulfonated products can generate 1mol water simultaneously, can decline the concentration of the concentrated sulfuric acid, while in order that
Sulfonating reaction is smoothed out, it is necessary to add excessive sulfuric acid to be dehydrated, the amount of the general concentrated sulfuric acid for adding is 3-4 times of reactant.
Oleum is the product that sulfur trioxide is dissolved in the concentrated sulfuric acid, generally there is two kinds of specifications, i.e., be containing free sulfur trioxide
20%-25% and 60%-65%.The freezing point of both oleums is low, is liquid under normal temperature, is easy to use and transports.Hair
When cigarette sulfuric acid is as sulfonating agent, reaction speed is fast, and reaction temperature is relatively low, while having process is simple, equipment investment low, easy to operate
The advantages of.Have the disadvantage excessively violent to the effect of organic matter, be often accompanied by oxidation, the generation byproduct such as sulfone.Additionally, can be produced after sulfonation
Unboiled water.
Chlorosulfonic acid is a kind of colourless or flaxen liquid, and with acrid odors, smoke in atmosphere is of sulfuric acid
The compound that hydroxyl is formed after being replaced by chlorine.When chlorosulfonic acid is used as sulfonating agent, respond is strong, and reaction condition is gentle, obtains
The product for arriving is purer.Accessory substance is hydrogen chloride, can be discharged under negative pressure, is conducive to reaction to carry out completely.Have the disadvantage price compared with
Height, and molecular weight is big, introduces a sulfonic sulfonating agent consumption more.Additionally, the hydrogen chloride produced in reaction has strong corruption
Corrosion.
The sulfonating agent of sulfonating reaction can also be inorganic salts sulfonating agent, can include for example：Sodium sulfite, bisulfite
Sodium, sodium pyrosulfite.This class sulfonating agent can be used for the sulfonation of alkene or with the organic compound containing active halogen atom
Thing reacts.
Sulfonating agent can also be mixed gas, the sulfonyl of mixed gas, sulfur dioxide and the oxygen of sulfur dioxide and chlorine
Chlorine, sulfamic acid.
During using the mixed gas of sulfur dioxide and chlorine as sulfonating agent, it is radical reaction to react, can be with ultraviolet
It is light-initiated.During using the mixed gas of sulfur dioxide and oxygen as sulfonating agent, it is radical reaction to react, can with illumination,
Radiation or ozone trigger.When chlorosulfuric acid is as sulfonating agent, generally carry out under light illumination, reaction mechanism and sulfur dioxide and chlorine
Mixed gas it is similar as sulfonating agent.Sulfamic acid is the nonhygroscopic solid of stabilization, similar to three oxygen in sulfonating reaction
Change sulphur tertiary amine complex compound, be a difference in that sulfamic acid is applied in high-temperature anhydrous medium.
In some embodiments, the sulfonation degree of institute's sulfonated graphene is 1%-5%.
The method for determining sulfonation degree is included but is not limited to：Elemental microanalysis method, conductometry, gas chromatography, colorimetric method,
Thin layer chromatography.Elemental microanalysis method is the percentage composition that element sulphur in polymer is directly determined using elemental analyser, element sulphur
Mass fraction directly reflect the content of sulfonic acid group in polymer.Elemental microanalysis method is simple and convenient, but elementary analysis needs
It is relatively costly by means of elemental analyser, especially when the sulphur of the copolymer for needing the multiple difference sulfonating agent dosages of system measurement
When change is spent, somewhat expensive.Conductometry is titrated with standard solution of sodium hydroxide, by adding the hydrogen in hydroxyl and solution
Ionic reaction, generates nonconducting hydrone.With the addition of standard solution of sodium hydroxide, the electrical conductivity of solution is gradually reduced,
When reaching titration end-point, electrical conductivity is preferably minimized value.NaOH is continuously added, the ion populations in solution can again increased,
Electrical conductivity increases.Calculated by the volume that titration end-point is the standard solution of sodium hydroxide consumed when electrical conductivity reaches minimum
Go out sulfonic content, computing formula is：
M is the concentration of standard solution of sodium hydroxide, and unit is mol/L；V when reaching titration end-point to be consumed NaOH
The volume of standard liquid, unit is mL；M is the quality of sample, and unit is g.
Influenceing the factor of sulfonation degree has molar ratio of material, sulfonating reaction temperature, sulfonating reaction time.Increase the bar of sulfonation degree
Part can be：Add more sulfonating agent, sulfonating reaction temperature higher, the sulfonating reaction time more long.It is pre- in order to obtain
The sulfonation degree of phase, can be by the relation between amount, three factors of reaction temperature and reaction time for balancing sulfonating agent.For example：
It is relatively low reaction temperature, reaction time more long and shorter reaction time, higher when the sulfonation dosage for adding is certain
Reaction temperature can obtain identical sulfonation degree.Therefore present invention addition, sulfonating reaction temperature, sulfonation not to sulfonating agent
Reaction time carries out excessive restriction, as long as the sulfonated graphene that sulfonation degree is 1%-5% can be obtained.But when temperature mistake
Gao Shi, sulfonating reaction is more violent, is not easy to control sulfonation degree in practical operation, therefore, sulfonation temperature is preferably -5-55
℃。
In order to preferably adjust the sulphonation rate of Graphene and improve wear resistence, the preparation of the sulfonated graphene that the present invention is used
Method is, by the Graphene of 10 weight portions with ultrasonic disperse in ethanol, add vinyl chlorosilane, heating stirring 24h, mistake
Solid is collected in filter, and ultrasonic disperse adds SSS, initiator in acetonitrile after drying, and continues under conditions of 100 DEG C
Stirring 3h, after product is filtered, is washed and is dried to solid, obtains final product sulfonated graphene.
In environment-friendly type high performance antiwear additive of the present invention, sulfonated graphene a certain degree of can increase lubricating oil
Extreme pressure property, especially showing can significantly improve maximum nonseizure load.
Molybdenum bisuphide is the main component of molybdenite.Black solid powder, there is metallic luster.1185 DEG C of fusing point, density
4.80g/cm3, Mohs' hardness 1.0-1.5.Molybdenum bisuphide is important kollag, is particularly well-suited under HTHP.It
Also diamagnetism, can be used as linear photoconductor conductor and display p-type or N-type conductivity can semiconductor, with rectification and transducing
Effect.Molybdenum bisuphide also acts as the catalyst of complicated dehydrogenation of hydrocarbons.The lubricity and extreme pressure property of grease can be increased.It is also applied for
High temperature, high pressure, the machine work state of rotating speed high load capacity high, extension device life-span.Molybdenum bisuphide is used for the main work(of friction material
Antifriction when can be low temperature, increases during high temperature and rubs, and loss on ignition is small, volatile in friction material.But molybdenum bisuphide also has limitation,
It is not strong etc. that such as poor thermal conductivity, coefficient of friction are also insufficient to low, penetrating power, limits its application.
In some embodiments, the particle diameter of the nano molybdenum disulfide is 70-100nm.
When the particle diameter of nano molybdenum disulfide is too high, anti-wear effect is bad.When its particle diameter is too small, surface can be high, between particle
It is susceptible to reunite, performance can be also had undesirable effect.
It has been generally acknowledged that nano-particle plays deposition film, i.e., because the effect of tribochemistry in friction process can be in friction pair
One layer of deposition film of Surface Creation, i.e., under high load, can cause the slip of nano-particle, make its contact surface can
Play a part of similar " ball (or bearing) ", sliding friction is partially changed into rolling friction.
In some embodiments, the preparing raw material of the environment-friendly type high performance antiwear additive also includes lithium niobate 8-12 parts.
Lithium niobate (LiNbO3) be a kind of niobium, lithium and oxygen compound.The environment-friendly type high performance antiwear additive that the present invention is provided
After adding lithium niobate, it can intert and is distributed between sulfonated graphene and the planes of molecules of molybdenum bisuphide, function similarly to
The effect of rolling friction, effectively facilitates be combineding with each other between sulfonated graphene and nano molybdenum disulfide, common to improve maximum nothing
Seizing load.
In some embodiments, the lithium niobate and the weight ratio of nano molybdenum disulfide are 2：1.
In some embodiments, the solvent naphtha is selected from least in D40, D70, D80, D85, D90, D95, D100
Kind.D range of solvents oil is a kind of solvent of environmental protection, is typically only capable to dissolve the material of low polarity or as regulation solution pole
The conditioning agent of property is used.The sulfonation degree of present invention control sulfonated graphene, in the presence of a small amount of terpinyl acetate, can be by sulphur
Graphite alkene and molybdenum bisuphide are distributed in solvent naphtha.
In some embodiments, the anion surfactant contains sulfonic acid group.
In some embodiments, the anion surfactant is selected from alkylbenzenesulfonate, alkylsulfonate, oil
One kind in sulfonate.
The alkylbenzenesulfonate includes linear alkylbenzene sulfonate (LAS), and it is the benzene sulphur for 8-16 alkyl with carbon number
Hydrochlorate or for carbon number for 12-16 p alkylphenylaceticacid.Preferably, it is 12-16 alkyl with carbon number
Benzene sulfonate, its instantiation includes but is not limited to, neopelex, Potassium dodecylbenzenesulfonate, tridecyl
Benzene sulfonic acid sodium salt, myristyl benzene sulfonic acid sodium salt, Pentadecylbenzene sulfonic acid sodium, cetyl benzenesulfonic acid sodium, hexadecyl diphenyloxide are double
Sodium sulfonate.
The second aspect of the present invention provides application of the environment-friendly type high performance antiwear additive as described above in oil product industry.
The third aspect of the present invention provides a kind of lubricating oil, contains environment-friendly type high performance antiwear additive as described above.
In some embodiments, the content of the environment-friendly type high performance antiwear additive in the lubricating oil is 0.5-5wt%.
Current most widely used sulfur-containing extreme-pressure additive is olefine sulfide, and two section based bisulfides also have preferable extreme-pressure anti-wear
Performance, as lubricating grease, extreme pressure industrial gear oil, the fortifying of petroleum products such as hydraulic oil, but its oil-soluble is poor, as oil
Certain limitation is received when the EP agent of product is used.Sulfonate by modified with preferable extreme pressure anti-wear, and
And its toxicity is low.The advantage of sulfur-containing extreme-pressure additive is that have sintering load higher, and anti-caking power is better than phosphorous extreme pressure agent, and it lacks
Point is that wear resistence is nothing like phosphorous extreme pressure agent.Therefore sulfur-containing extreme-pressure additive is mainly used as extreme pressure agent and oiliness improver.Improve sulfur-bearing pole
The method for pressing agent is that by itself and phosphorous extreme pressure agent, nitrogenous extreme pressure agent etc. is compound.
The environment-friendly type high performance antiwear additive that the present invention is provided has good oil-soluble, with very excellent extreme pressure property
Energy, wear-resistant and Wear vesistance, can be widely used in lubricating oil as lube oil additive.
The present invention is expanded on further with reference to specific embodiment.
The preparation method of sulfonated graphene is in embodiment 1-12：Counted with the weight portion of Graphene as 100 parts, by 100 weights
The Graphene of amount part in ethanol, adds 8 parts by weight of ethylene base trichlorosilanes with ultrasonic disperse, and heating stirring 24h, filtering is received
Collection solid, ultrasonic disperse the need for sulfonation degree, adds the SSS of 1-8 weight portions in acetonitrile after drying, then
The 2 of 0.01 weight portion are added, 2 '-azodiisobutyronitrile persistently stirs 3h under conditions of 100 DEG C, after product is filtered, to solid
Body is washed and dried, and obtains final product sulfonated graphene.
Embodiment 1
Environment-friendly type high performance antiwear additive, in parts by weight, its preparing raw material includes：100 parts of sulfonated graphene, acetic acid pine tar
10 parts of ester, 5 parts of nano molybdenum disulfide, 15 parts of myristyl benzene sulfonic acid sodium salt, 60 parts of D70 solvent naphthas.The sulphur of the sulfonated graphene
Change degree is 1%, and the particle diameter of the nano molybdenum disulfide is 80nm.
The environment-friendly type high performance antiwear additive preparation method is, by 100 weight portion sulfonated graphenes, 10 weight portion acetic acid pine
Grease, 5 weight portion nano molybdenum disulfides, 15 weight portion myristyl benzene sulfonic acid sodium salts, 60 weight portion D70 solvent naphthas are in a kettle.
Mixing, stirs 30min, obtains final product.
Embodiment 2
Environment-friendly type high performance antiwear additive, in parts by weight, its preparing raw material includes：100 parts of sulfonated graphene, acetic acid pine tar
10 parts of ester, 5 parts of nano molybdenum disulfide, 15 parts of myristyl benzene sulfonic acid sodium salt, 60 parts of D70 solvent naphthas.The sulphur of the sulfonated graphene
Change degree is 3%, and the particle diameter of the nano molybdenum disulfide is 80nm.
The environment-friendly type high performance antiwear additive preparation method is, by 100 weight portion sulfonated graphenes, 10 weight portion acetic acid pine
Grease, 5 weight portion nano molybdenum disulfides, 15 weight portion myristyl benzene sulfonic acid sodium salts, 60 weight portion D70 solvent naphthas are in a kettle.
Mixing, stirs 30min, obtains final product.
Embodiment 3
Environment-friendly type high performance antiwear additive, in parts by weight, its preparing raw material includes：100 parts of sulfonated graphene, acetic acid pine tar
10 parts of ester, 5 parts of nano molybdenum disulfide, 15 parts of myristyl benzene sulfonic acid sodium salt, 60 parts of D70 solvent naphthas.The sulphur of the sulfonated graphene
Change degree is 5%, and the particle diameter of the nano molybdenum disulfide is 80nm.
The environment-friendly type high performance antiwear additive preparation method is, by 100 weight portion sulfonated graphenes, 10 weight portion acetic acid pine
Grease, 5 weight portion nano molybdenum disulfides, 15 weight portion myristyl benzene sulfonic acid sodium salts, 60 weight portion D70 solvent naphthas are in a kettle.
Mixing, stirs 30min, obtains final product.
Embodiment 4
Environment-friendly type high performance antiwear additive, in parts by weight, its preparing raw material includes：100 parts of sulfonated graphene, acetic acid pine tar
10 parts of ester, 5 parts of nano molybdenum disulfide, 15 parts of myristyl benzene sulfonic acid sodium salt, 60 parts of D70 solvent naphthas, 10 parts of lithium niobate.The sulfonation
The sulfonation degree of Graphene is 3%, and the particle diameter of the nano molybdenum disulfide is 80nm.
The environment-friendly type high performance antiwear additive preparation method is, by 100 weight portion sulfonated graphenes, 10 weight portion acetic acid pine
Grease, 5 weight portion nano molybdenum disulfides, 15 weight portion myristyl benzene sulfonic acid sodium salts, 60 weight portion D70 solvent naphthas, 10 weight portions
Lithium niobate mixes in a kettle., stirs 30min, obtains final product.
Embodiment 5
Environment-friendly type high performance antiwear additive, in parts by weight, its preparing raw material includes：100 parts of sulfonated graphene, acetic acid pine tar
10 parts of ester, 5 parts of nano molybdenum disulfide, 15 parts of myristyl benzene sulfonic acid sodium salt, 60 parts of D70 solvent naphthas.The sulphur of the sulfonated graphene
Change degree is 3%, and the particle diameter of the nano molybdenum disulfide is 200nm.
The environment-friendly type high performance antiwear additive preparation method is, by 100 weight portion sulfonated graphenes, 10 weight portion acetic acid pine
Grease, 5 weight portion nano molybdenum disulfides, 15 weight portion myristyl benzene sulfonic acid sodium salts, 60 weight portion D70 solvent naphthas are in a kettle.
Mixing, stirs 30min, obtains final product.
Embodiment 6
Environment-friendly type high performance antiwear additive, in parts by weight, its preparing raw material includes：100 parts of sulfonated graphene, acetic acid pine tar
10 parts of ester, 5 parts of nano molybdenum disulfide, 15 parts of myristyl benzene sulfonic acid sodium salt, 60 parts of D70 solvent naphthas.The sulphur of the sulfonated graphene
Change degree is 3%, and the particle diameter of the nano molybdenum disulfide is 50nm.
The environment-friendly type high performance antiwear additive preparation method is, by 100 weight portion sulfonated graphenes, 10 weight portion acetic acid pine
Grease, 5 weight portion nano molybdenum disulfides, 15 weight portion myristyl benzene sulfonic acid sodium salts, 60 weight portion D70 solvent naphthas are in a kettle.
Mixing, stirs 30min, obtains final product.
Embodiment 7
Environment-friendly type high performance antiwear additive, in parts by weight, its preparing raw material includes：100 parts of sulfonated graphene, acetic acid pine tar
12 parts of ester, 4 parts of nano molybdenum disulfide, 15 parts of myristyl benzene sulfonic acid sodium salt, 60 parts of D70 solvent naphthas.The sulphur of the sulfonated graphene
Change degree is 3%, and the particle diameter of the nano molybdenum disulfide is 80nm.
The environment-friendly type high performance antiwear additive preparation method is, by 100 weight portion sulfonated graphenes, 10 weight portion acetic acid pine
Grease, 5 weight portion nano molybdenum disulfides, 15 weight portion myristyl benzene sulfonic acid sodium salts, 60 weight portion D70 solvent naphthas are in a kettle.
Mixing, stirs 30min, obtains final product.
Embodiment 8
Environment-friendly type high performance antiwear additive, in parts by weight, its preparing raw material includes：100 parts of sulfonated graphene, acetic acid pine tar
10 parts of ester, 5 parts of nano molybdenum disulfide, 15 parts of myristyl benzene sulfonic acid sodium salt, 60 parts of D70 solvent naphthas.The sulphur of the sulfonated graphene
Change degree is 0.5%, and the particle diameter of the nano molybdenum disulfide is 80nm.
The environment-friendly type high performance antiwear additive preparation method is, by 100 weight portion sulfonated graphenes, 10 weight portion acetic acid pine
Grease, 5 weight portion nano molybdenum disulfides, 15 weight portion myristyl benzene sulfonic acid sodium salts, 60 weight portion D70 solvent naphthas are in a kettle.
Mixing, stirs 30min, obtains final product.
Embodiment 9
Environment-friendly type high performance antiwear additive, in parts by weight, its preparing raw material includes：100 parts of sulfonated graphene, acetic acid pine tar
10 parts of ester, 5 parts of nano molybdenum disulfide, 15 parts of myristyl benzene sulfonic acid sodium salt, 60 parts of D70 solvent naphthas.The sulphur of the sulfonated graphene
Change degree is 10%, and the particle diameter of the nano molybdenum disulfide is 80nm.
The environment-friendly type high performance antiwear additive preparation method is, by 100 weight portion sulfonated graphenes, 10 weight portion acetic acid pine
Grease, 5 weight portion nano molybdenum disulfides, 15 weight portion myristyl benzene sulfonic acid sodium salts, 60 weight portion D70 solvent naphthas are in a kettle.
Mixing, stirs 30min, obtains final product.
Embodiment 10
Environment-friendly type high performance antiwear additive, in parts by weight, its preparing raw material includes：100 parts of sulfonated graphene, acetic acid pine tar
10 parts of ester, 5 parts of nano molybdenum disulfide, 15 parts of AEO-9,60 parts of D70 solvent naphthas.The sulfonation degree of the sulfonated graphene is 3%,
The particle diameter of the nano molybdenum disulfide is 80nm.
The environment-friendly type high performance antiwear additive preparation method is, by 100 weight portion sulfonated graphenes, 10 weight portion acetic acid pine
Grease, 5 weight portion nano molybdenum disulfides, 15 weight portion AEO-9,60 weight portion D70 solvent naphthas mix in a kettle., stirring
30min, obtains final product.
Method of testing：
The preparation of sample：Blank sample is the weight portion of commercially available multigrade lubricating oil 100, and detection sample is commercially available multigrade lubricating oil
The weight portion of 95.5 weight portions+embodiment 4.5.
1. extreme pressure property test
The maximum nonseizure load P of blank sample and detection sample is determined according to GB/T 3142-1982 (2004)B, sintering
Load PD, integrated abrasion value ZMZ.
2. abrasion resistance test
The wear scar diameter D of blank sample and detection sample is determined according to SH/T 0189-1992.
3. antifriction performance test
The coefficient of friction f of blank sample and detection sample is determined with four-ball tribotester according to ASTM5183.
| ZMZ/N | D392N60min,75℃,1200rpm | f | |||
| Embodiment 1 | 1153 | 3923 | 549.89 | 0.36 | 0.072 |
| Embodiment 2 | 1182 | 3984 | 558.43 | 0.33 | 0.068 |
| Embodiment 3 | 1164 | 3934 | 551.38 | 0.35 | 0.071 |
| Embodiment 4 | 1203 | 4127 | 564.62 | 0.29 | 0.054 |
| Embodiment 5 | 1113 | 3644 | 532.41 | 0.37 | 0.072 |
| Embodiment 6 | 1124 | 3586 | 528.63 | 0.36 | 0.071 |
| Embodiment 7 | 1133 | 3886 | 538.84 | 0.36 | 0.076 |
| Embodiment 8 | 1134 | 3782 | 533.14 | 0.38 | 0.075 |
| Embodiment 9 | 1138 | 3655 | 519.21 | 0.4 | 0.084 |
| Embodiment 10 | 1079 | 3187 | 492.58 | 0.41 | 0.088 |
| Blank sample | 1079 | 3089 | 468.22 | 0.44 | 0.091 |
4 additions are tested
Blank sample is commercially available multigrade lubricating oil, and detection sample is to add Different Weight percentage to commercially available multigrade lubricating oil
Embodiment 2 and embodiment 4.The maximum of blank sample and detection sample is determined without seizing according to GB/T 3142-1982 (2004)
Load PB。
The above, the only present invention preferably specific embodiment, but protection scope of the present invention is not limited thereto, and appoints
What those familiar with the art the invention discloses in the range of, technology according to the present invention scheme and inventive concept
It is subject to equivalent or change, belongs to protection scope of the present invention.
Claims (10)
1. environment-friendly type high performance antiwear additive, it is characterised in that in parts by weight, its preparing raw material includes：Sulfonated graphene 100
Part, terpinyl acetate 8-12 parts, nano molybdenum disulfide 4-6 parts, anion surfactant 14-16 parts, solvent naphtha 55-75 parts.
2. environment-friendly type high performance antiwear additive as claimed in claim 1, it is characterised in that its preparing raw material also includes lithium niobate 8-
12 parts.
3. environment-friendly type high performance antiwear additive as claimed in claim 1, it is characterised in that the sulfonation degree of institute's sulfonated graphene is
1%-5%.
4. environment-friendly type high performance antiwear additive as claimed in claim 1, it is characterised in that the solvent naphtha be selected from D40, D70,
At least one in D80, D85, D90, D95, D100.
5. environment-friendly type high performance antiwear additive as claimed in claim 1, it is characterised in that the particle diameter of the nano molybdenum disulfide is
70-100nm。
6. environment-friendly type high performance antiwear additive as claimed in claim 1, it is characterised in that the anion surfactant contains
Sulfonic acid group.
7. environment-friendly type high performance antiwear additive as claimed in claim 6, it is characterised in that the anion surfactant is selected from
One kind in alkylbenzenesulfonate, alkylsulfonate, petroleum sulfonate.
8. the environment-friendly type high performance antiwear additive as described in any one of claim 1-7 claim oil product industry in should
With.
9. a kind of lubricating oil, it is characterised in that contain the property high of the environment-friendly type as described in any one of claim 1-7 claim
Can antiwear additive.
10. lubricating oil as claimed in claim 9, it is characterised in that environment-friendly type high performance antiwear additive in the lubricating oil
Content is 0.5-5wt%.
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