CN107236581A - High-performance graphene complex grease - Google Patents
High-performance graphene complex grease Download PDFInfo
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- CN107236581A CN107236581A CN201710545162.7A CN201710545162A CN107236581A CN 107236581 A CN107236581 A CN 107236581A CN 201710545162 A CN201710545162 A CN 201710545162A CN 107236581 A CN107236581 A CN 107236581A
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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
- C10M125/00—Lubricating compositions characterised by the additive 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
- C10M125/00—Lubricating compositions characterised by the additive being an inorganic material
- C10M125/02—Carbon; Graphite
-
- 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
- C10M125/00—Lubricating compositions characterised by the additive being an inorganic material
- C10M125/20—Compounds 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
- C10M125/00—Lubricating compositions characterised by the additive being an inorganic material
- C10M125/22—Compounds containing sulfur, selenium or tellurium
-
- 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
- C10N2050/00—Form in which the lubricant is applied to the material being lubricated
- C10N2050/10—Semi-solids; greasy
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- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Organic Chemistry (AREA)
- Lubricants (AREA)
Abstract
The present invention relates to lubrication technical field, and in particular to a kind of High-performance graphene complex grease.A kind of High-performance graphene complex grease is specifically disclosed, in parts by weight, at least including following components, 100 parts of lubricating base oil；1~5 part of dispersant；5~15 parts of thickening agent；10~30 parts of antiwear additive；0.1~3 part of graphene mixture；10~40 parts of calcium lignosulfonate；1~5 part of nano-particle；The graphene mixture is graphene oxide, ammonification graphene, the mixing of sulfonated graphene.
Description
Technical field
The present invention relates to lubrication technical field, and in particular to a kind of High-performance graphene complex grease.
Background technology
Lubricating grease is the lubricant that base oil is crowded into solid-like with thickening agent from semifluid.Lubricating grease is very early by people
Used as lubricant, but lubricating grease is prepared as an independent industrial department, no matter in China or in world wide
It is interior less than an one-hundred-year history, it may be said that grease industry is one just in expanding industry.The application field of lubricating grease is non-
Normal is extensive, almost covers industrial machinery, agricultural machinery, traffic transport industry, aerospace industry, electronic and information industry and all kinds of
Military equipment, and need the part type of lubricating grease then to have bearing, gear, chain, steel wire rope etc..With petrochemical industry, metallurgy, make
The development of the industries such as paper, printing and dyeing, increasing plant equipment is operated under the conditions of high temperature heavy load, and people are to grease product
Performance requirement more and more higher.For example, the equipment longtime running such as conticaster, sintering machine in metallurgical industry is in high temperature, heavy duty and water
Under the operating modes such as flushing, to maintain the operating of the equipment steadily in the long term, there is higher requirement to the lubrication of equipment, profit is not required nothing more than
Consistent lubricant has higher bearing capacity, and requires that lubricating grease has good high temperature, water resistant, anti-rotten candle performance.
The main of the grease product of China is moistened with complex lithium grease, polyureas base grease and Composite calcium-sulfonate-batetrapolyurea
Based on the products such as consistent lubricant.The wherein high-temperature behavior deficiency of complex lithium grease, polyureas base grease, and its water resistant drenches loss
Performance is not good；There is complex calcium sulfonate grease outstanding water resistant to drench leachability, but its decay resistance is poor.Therefore, it is anxious
The good grease product of a greasy property need to be researched and developed.
Graphene has unique two-dimensional structure and excellent performance, such as Young's modulus (about 1100GPa), thermal conductivity, load
Transport factor and specific surface area etc. are flowed higher, also with fractional quantum hall effect, quantum Hall ferromagnetism and exciton band
The phenomenons such as gap.Exactly because graphene has these excellent performances and unique structure, extensive concern in recent years is become
Focus, cause greatly study hotspot in the energy, material, electronics, biology, medicine and other fields.
Thus, graphene is added in lubricating grease field, with larger application value.
The content of the invention
In order to solve prior art problem, it is composite lubricated that the first aspect of the present invention provides a kind of High-performance graphene
Fat, in parts by weight, at least including following components,
100 parts of lubricating base oil；
1~5 part of dispersant；
5~15 parts of thickening agent；
10~30 parts of antiwear additive；
0.1~3 part of graphene mixture；
10~40 parts of calcium lignosulfonate；
1~5 part of nano-particle；
The graphene mixture is graphene oxide, ammonification graphene, the mixing of sulfonated graphene.
As a kind of preferred technical scheme of the present invention, the lubricating base oil is selected from：Mineral oil, hydrocarbon system artificial oil, ester
It is any one in oil, ether system oil.
As a kind of preferred technical scheme of the present invention, kinematic viscosity of the lubricating base oil at 40 DEG C is 50~
200mm2/s。
As a kind of preferred technical scheme of the present invention, the dispersant is selected from：Polyisobutene succinimide, acetone,
Any one in propene carbonate.
As a kind of preferred technical scheme of the present invention, the thickening agent is selected from：In sulfurized alkylphenol calcium, carbamido thickening agent
The mixing of any one or more.
As a kind of preferred technical scheme of the present invention, the antiwear additive is selected from：It is two thio Acidic phosphates zinc, two thio
Dialkyl amido formic acid molybdenum, two thio dialkyl amido lead formates, molybdenum disulfide, polytetrafluoroethylene (PTFE), dibutyl dithio amino
The mixing of any one or more in formic acid antimony, tungsten disulfide, selenium disulfide.
As a kind of preferred technical scheme of the present invention, in the graphene mixture, graphene oxide, ammonification graphite
Weight ratio between alkene, sulfonated graphene is 100：1：12.
As a kind of preferred technical scheme of the present invention, the nano-particle is selected from：It is nano silicon, nano oxidized
In aluminium, nanometer sulfoacid calcium, nano-calcium carbonate, nano molybdenum disulfide, nano aluminum nitride, nano titanium oxide any one or it is several
The mixing planted.
As a kind of preferred technical scheme of the present invention, the High-performance graphene complex grease also includes anti-oxidant
In agent, antirust agent, oiliness improver, viscosity index improving agent, pour-point depressant, defoamer, emulsifying agent, matal deactivator, detergent-dispersant additive
The mixing of any one or more.
The second aspect of the invention provides the preparation method of above-mentioned High-performance graphene complex grease, at least includes
Following steps：
(1) lubricating base oil of corresponding parts by weight, calcium lignosulfonate, graphene mixture are added in reactor,
Stirred at 50~100 DEG C 1~2 hour, be then incubated 1~5 hour at 70~80 DEG C；
(2) dispersant, thickening agent, the antiwear additive of corresponding parts by weight are added into step (1), at 70~120 DEG C, is continued
Stirring 1~3 hour, then adds nano-particle, is warming up to 150~200 DEG C, refining continues to be incubated 30~100 minutes；
(3) cool, it is composite lubricated to obtain High-performance graphene after temperature drops to 20~40 DEG C, after grinding homogenizing
Fat.
Embodiment
The participation in the election detailed description of the invention below for being preferable to carry out method and including embodiment this hair can be more easily understood
Bright content.Unless otherwise defined, all technologies used herein and scientific terminology have common with art of the present invention
The identical implication that technical staff is generally understood that.When there is contradiction, the definition in this specification is defined.
As used herein term " by ... prepare " it is synonymous with "comprising".Term "comprising" used herein, " comprising ",
" having ", " containing " or its any other deformation, it is intended that cover including for non-exclusionism.For example, the combination comprising listed elements
Thing, step, method, product or device are not necessarily limited to those key elements, but can include not expressly listed other key elements or
Such a composition, step, method, product or the intrinsic key element of device.
Conjunction " Consists of " excludes any key element do not pointed out, step or component.If be used in claim, this
Phrase will make claim be closed, it is not included the material in addition to materials of those descriptions, but relative normal
Except rule impurity.When being rather than immediately following in the clause that phrase " Consists of " appears in claim main body after theme,
It is only limited to the key element described in the clause；Other key elements are not excluded outside as the overall claim.
Equivalent, concentration or other values or parameter are excellent with scope, preferred scope or a series of upper limit preferred values and lower limit
During the Range Representation that choosing value is limited, this, which is appreciated that, specifically discloses by any range limit or preferred value and any scope
All scopes that any pairing of lower limit or preferred value is formed, regardless of whether whether the scope separately discloses.For example, when open
During scope " 1 to 5 ", described scope should be interpreted as including scope " 1 to 4 ", " 1 to 3 ", " 1 to 2 ", " 1 to 2 and 4 to
5 ", " 1 to 3 and 5 " etc..When number range is described herein, unless otherwise indicated, otherwise the scope is intended to include its end
Value and all integers and fraction within the range.
Singulative includes plural number and object is discussed, unless the context clearly dictates otherwise." optional " or it is " any
It is a kind of " refer to that the item or event that describe thereafter may or may not occur, and the description include situation that event occurs and
The situation that event does not occur.
Approximate term in specification and claims is used for modifying quantity, represents that the present invention is not limited to this specific
Quantity, includes the part of the amendment of the acceptable change without cause related basic function close to the quantity.Phase
Answer, modify a numerical value with " about ", " about " etc., mean that the invention is not restricted to the exact numerical.In some examples, approximately
Term likely corresponds to the precision of the instrument of measured value.In present specification and claims, scope is limited can be with
Combine and/or exchange, these scopes include all subranges contained therebetween if not stated otherwise.
In addition, the indefinite article " one kind " and " one " before key element of the present invention or component are to key element or the quantitative requirement of component
(i.e. occurrence number) unrestriction.Therefore " one " or " one kind " should be read as including one or at least one, and odd number
The key element or component of form also include plural form, unless the obvious purport of the quantity refers to singulative.
In order to solve prior art problem, it is composite lubricated that the first aspect of the present invention provides a kind of High-performance graphene
Fat, in parts by weight, at least including following components,
100 parts of lubricating base oil；
1~5 part of dispersant；
5~15 parts of thickening agent；
10~30 parts of antiwear additive；
0.1~3 part of graphene mixture；
10~40 parts of calcium lignosulfonate；
1~5 part of nano-particle；
The graphene mixture is graphene oxide, ammonification graphene, the mixing of sulfonated graphene.
As a kind of preferred technical scheme of the present invention, the lubricating base oil is selected from：Mineral oil, hydrocarbon system artificial oil, ester
It is any one in oil, ether system oil.
Described mineral oil, alias white oil, paraffin oil.From reducing in the angle of cost, the application, the mineral of selection
Oil is industrial grade white oil.The trade mark that can be enumerated be 2# white oils, 3# white oils, 5# white oils, 10# white oils, 15# white oils, 26# white oils,
32# white oils, 46# white oils, 60# white oils, 90# white oils, 120# white oils, 150# white oils, 300# white oils, 500# white oils etc., wherein, #
Representative number.
Described hydrocarbon system artificial oil, what can be enumerated has：Polyalphaolefin, specifically there are：Polybutene, polyisobutene, 1- are pungent
Any one or a few mixing in alkene oligomer, 1- decylene oligomers, ethylene-propylene copolymer.
Described ester system oil, what can be enumerated has：Dibutyl sebacate, decanedioic acid two (2- ethylhexyls) ester, adipic acid
The sour first of dioctyl ester, diisodecyl adipate (DIDA), adipic acid two (tridecyl) ester, glutaric acid two (tridecyl) ester, acetylricinoleate
The diester oils such as ester；The aromatic ester oils such as trioctyl trimellitate (TOTM), tri trimellitate last of the ten Heavenly stems ester, tetraoctyl 1,2,4,5-benzenetetra-carboxylate；Trihydroxy methyl
Propane caprylate, trimethylolpropane pelargonate, pentaerythrite -2 ethyl hexanoic acid ester, pentaerythrite pelargonate etc..
Described ether system oil, what can be enumerated has：Polyethylene glycol, polypropylene glycol, polyethylene glycol monoether, polypropyleneglycol monoether
Deng polyethylene glycol；Alkyl diphenyl ether, dialkyl diphenyl ether, five phenyl ethers, tetraphenyl ether, monoalkyl tetraphenyl ether, dialkyl group
The phenyl ether oil such as tetraphenyl ether.
As a kind of preferred technical scheme of the present invention, kinematic viscosity of the lubricating base oil at 40 DEG C is 50~
200mm2/s。
As a kind of preferred technical scheme of the present invention, the dispersant is selected from：Polyisobutene succinimide, acetone,
Any one in propene carbonate.
As a kind of preferred technical scheme of the present invention, the thickening agent is selected from：In sulfurized alkylphenol calcium, carbamido thickening agent
The mixing of any one or more.
As a kind of preferred technical scheme of the present invention, the antiwear additive is selected from：It is two thio Acidic phosphates zinc, two thio
Dialkyl amido formic acid molybdenum, two thio dialkyl amido lead formates, molybdenum disulfide, polytetrafluoroethylene (PTFE), dibutyl dithio amino
The mixing of any one or more in formic acid antimony, tungsten disulfide, selenium disulfide.
As a kind of preferred technical scheme of the present invention, in the graphene mixture, graphene oxide, ammonification graphite
Weight ratio between alkene, sulfonated graphene is 100：1：12.
Term " graphene " refers to carbon atom with sp2The cellular flat film of hybrid form formation, is a kind of only one
The quasi- two-dimensional material of individual atomic layer level thickness, monoatomic layer graphite is done so being called, carbon atom it is regular be arranged in honeycomb lattice
Among construction unit.Each carbon atom with three carbon atoms of σ keys and other in addition to being connected, remaining pi-electron and other carbon
The pi-electron formation big pi bond of delocalization of atom, thus, graphene is acted on due to stronger π-π, and its dispersiveness is poor.
The preparation method of graphene：Mechanical stripping method, epitaxial growth method, chemical vapour deposition technique, chemical synthesis, oxidation
Graphene reducing process and longitudinally cutting carbon tube method etc. are several.In the application, described graphene oxide obtains to be commercially available, is purchased from
Suzhou Heng Qiu graphenes Co., Ltd.
As a kind of preferred technical scheme of the present invention, the graphene oxide is layered graphite oxide alkene.
Term " graphene oxide " refers to include tri- kinds of elements of C, H, O with graphene of the strong oxidizer after treated.Oxidation
The active force such as hydrogen bond that graphene passes through interlayer stacked in multi-layers is together.
The method that three kinds commonly used at present prepare graphene oxide, i.e. Brodie methods, Staudenmaier methods and Hummers
Method, is that graphite is handled using the combination of oxidation reinforced dose of strong acid.Strong protonic acid enters graphite layers formation graphite
Intercalation compound, subsequent strong oxidizer carries out oxidation to graphite and introduces a large amount of hydrophilic oxygen-containing functional groups to graphenic surface and side
Edge formation graphene oxide.Due to the stronger hydrophily of oxy radical, graphene oxide can completely be peeled off and is dispersed in water-soluble
Among liquid.
In the application, the graphene oxide obtains to be commercially available, is purchased from Suzhou Heng Qiu graphenes Co., Ltd.
The ammonification graphene is also known as amination graphene, is purchased from Suzhou Heng Qiu graphenes Co., Ltd.
The sulfonated graphene is purchased from Suzhou Heng Qiu graphenes Co., Ltd.
In a preferred embodiment, in the graphene mixture, in addition to nitrogen-doped graphene.
The nitrogen-doped graphene is purchased from Suzhou Heng Qiu graphenes Co., Ltd.
As a kind of preferred technical scheme of the present invention, the nano-particle is selected from：It is nano silicon, nano oxidized
In aluminium, nanometer sulfoacid calcium, nano-calcium carbonate, nano molybdenum disulfide, nano aluminum nitride, nano titanium oxide any one or it is several
The mixing planted.
As a kind of preferred technical scheme of the present invention, the nano silicon is silane coupler modified nano-silica
SiClx.
Term " silane coupler modified nano silicon " refers to N- (2- aminoethyls) -3- aminopropyl trimethoxy silicon
Alkane, 3- Mercaptopropyltriethoxysilanes are modified to nano silicon simultaneously.
In a preferred embodiment, N- (2- the aminoethyls) -3- aminopropyl trimethoxysilanes, 3- sulfydryls third
Weight ratio between ethyl triethoxy silicane alkane, nano silicon is 5：1：10.
In a preferred embodiment, the preparation method of the silane coupler modified nano silicon is at least wrapped
Include following steps：
In the reactor, solvent 80ml toluene and 10g nano silicons, ultrasonic disperse 30min are added, 5g is sequentially added
N- (2- aminoethyls) -3- aminopropyl trimethoxysilanes, 1g 3- Mercaptopropyltriethoxysilanes, the back flow reaction at 100 DEG C
5h, filtering, ethanol is washed 3 times, and silane coupler modified nano silicon is obtained after drying.
As a kind of preferred technical scheme of the present invention, the High-performance graphene complex grease also includes anti-oxidant
In agent, antirust agent, oiliness improver, viscosity index improving agent, pour-point depressant, defoamer, emulsifying agent, matal deactivator, detergent-dispersant additive
The mixing of any one or more.
As a kind of preferred technical scheme of the present invention, the antioxidant is selected from：Phenol antioxidant, sulphur system are anti-oxidant
The mixing of any one or more in agent, phosphorous antioxidant, amine system antioxidant.
What the antioxidant can be enumerated has：Containing in sulphur ester antioxidant, phenolic antioxidant, phosphite ester kind antioxidant
It is at least one.
It can be enumerated containing sulphur ester antioxidant：Dilauryl thiodipropionate, thio-2 acid 2 stearyl ester or thio
Dipropionic acid two (octadecyl ester), β, β '-thio two butyric acid two (18) ester, thio-2 acid bay octadecyl ester, thio-2 acid two
(13) ester, thio-2 acid two (14) ester etc..
Phenolic antioxidant can be enumerated：1- hydroxy-3-methyl -4- cumenes, 2,6- DI-tert-butylphenol compounds, the uncles of 2,6- bis-
Butyl -4- ethyl -phenols, BHT, 2,6- di-t-butyl -4- normal-butyls phenol, 4- methylols -2,6- bis-
Tert-butyl phenol, butylhydroxy anisole, 2- (1- methylcyclohexyls) -4,6- xylenols, the tertiary fourths of 2,4- dimethyl -6-
Base phenol, 2- methyl -4,6- dinonyl phenol, 2,6- di-t-butyls-alpha, alpha-dimethyl amino-p-cresol, 2,4,6- tri-butyl benzenes
Double (the octylsulfo) -1,3,5-triazines of phenol, 6- (4- hydroxyl -3,5- di-tert-butyls amido) -2,4-, 4,6- it is double (4- hydroxyl -3,
5- di-t-butyls phenoxy group) -2- n-octylthios -1,3,5-triazines, β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid first
Ester, β-positive octadecanol ester of (4-hydroxyl-3,5-di-tert-butyl-phenyl) propionic acid, styrenated phenol, 4,4 '-dihydroxy connection
Benzene, butylated octylated phenol, butylated stytrene cresols, 2,2 '-methylene bis (4- methyl-6-tert-butylphenols) or 2,
2 '-methylene bis (the 6- tert-butyl group -4- cresols), 2,2 '-methylene bis (4- ethyl -6- tert-butyl phenols), 2,2 '-methylene bis (4- first
Base -6- cyclohexylphenols), 4,4 '-methylene bis (2,6- DI-tert-butylphenol compounds), 2, (6- α-methylbenzyls are to first for 2 '-methylene bis
Phenol), 1,1- double (4- hydroxy benzenes) hexamethylene, 2,2 '-methylene bis (4- methyl -6- (Alpha-Methyl cyclohexyl) phenol) or 2,2 '-two
Hydroxyl -3,3 '-two (Alpha-Methyl cyclohexyl) -5,5 '-dimethyl diphenylmethane, 1,3,5- trimethyls -2,4,6- tri- (3,5- bis-
Tertiary butyl-4-hydroxy benzyl) benzene, 1,1,3- tri- (2- methyl -4- hydroxyl -5- tert-butyl-phenyls) butane, four (3- (3 ' 5 '-two uncles
Butyl -4 '-hydroxy phenyl) propionic acid) pentaerythritol ester, 4,4 '-thiobis (the 6- tert-butyl group -3- methylphenols) or 4,4 '-thio
Double (6- tert-butyl-m-cresols), 4,4 '-thiobis (2- methyl-6-tert-butylphenols) or 4,4 '-thiobis (6- tert-butyl o first
Phenol), 2, the double (β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid of 2 '-thiobis (4- methyl-6-tert-butylphenols), hexylene glycol
Ester), 2,2 '-thiobis (3 ,-(3,5- di-tert-butyl-hydroxy phenyl) ethyl propionate), N, double (3,5- bis- uncles of N '-hexamethylene
Butyl-4- hydroxyls hydrocinnamamide), 1,3,5- tri- (the 4- tert-butyl group-3- hydroxyls-2,6- dimethyl benzyls) 1,3,5-triazine-2,4,
6- (1H, 3H, 5H)-triketone, 1,3,5- tri- (3,5- di-tert-butyl-4-hydroxyl benzyl) guanamines, 4,6- (1H, 3H, 5H) three
Ketone or isocyanuric acid three (3,5- di-tert-butyl-4-hydroxyl benzyl ester), [β-(3,5- di-t-butyl -4- hydroxy benzenes of isocyanuric acid three
Base) propionyloxy ethyl ester], double [3,3- double (3 '-tert-butyl group -4 '-hydroxy phenyl) butyric acid] glycol esters, 1,1 '-thiobis (2-
Naphthols), double (3,5- di-tert-butyl-4-hydroxyl benzyl) thioethers, 2,5- di-tert-butyl hydroquinones, the tertiary pentyls of 2,5- bis- are to benzene two
Phenol, 3,5- di-tert-butyl-4-hydroxyl benzyls di(2-ethylhexyl)phosphate (18) ester, 3,5- di-tert-butyl-4-hydroxyl benzyls diethyl phosphate, three
One kind in glycol double -3- (3- tertiary butyl-4-hydroxy -5- aminomethyl phenyls) propionic ester, hydroquinone dibenzyl ethers.
Phosphite ester kind antioxidant can be enumerated：Triphenyl phosphite, phosphorous acid three (nonyl phenyl ester), phosphorous acid three are different pungent
Ester, triisodecyl phosphite ester, the isodecyl ester of phosphorous acid benzene two, trilauryl trithiophosphite, trilauryl phosphite, phosphorous acid
Three (octadecyl esters), the isodecyl ester of diphosphorous acid pentaerythrite two, diphosphorous acid pentaerythrite distearyl alcohol ester, 4,4 '-fourth fork are double (sub-
Phosphoric acid (3- methyl-6-tert butyl phenyl) two (tridecyl) esters), isooctyl diphenyl phosphite, phosphorous acid benzene di-isooctyl, Asia
Diphenyl octyl phosphate, phosphorous acid hexichol isodecyl ester, dioctyl phosphite, phosphorous acid dilauryl, dimethylphosphite, phosphorous acid
Double 13 esters of two oleyl alcohol esters, didecyl phosphite, dibutyl phosphite, phosphorous acid, phosphorous acid double 14 esters, phosphorous triethylenetetraminehexaacetic acids
Ester, tributyl phosphite, triisopropyl phosphite, the monooctyl ester of phosphorous acid three or phosphorous acid three (2- ethylhexyls), phosphorous acid-benzene are double
One kind in (nonyl benzene) ester, phosphorous acid hexichol nonyl phenyl ester, phosphorous acid three (2,4- di-tert-butyl-phenyl) ester.
The second aspect of the invention provides the preparation method of above-mentioned High-performance graphene complex grease, at least includes
Following steps：
(1) lubricating base oil of corresponding parts by weight, calcium lignosulfonate, graphene mixture are added in reactor,
Stirred at 50~100 DEG C 1~2 hour, be then incubated 1~5 hour at 70~80 DEG C；
(2) dispersant, thickening agent, the antiwear additive of corresponding parts by weight are added into step (1), at 70~120 DEG C, is continued
Stirring 1~3 hour, then adds nano-particle, is warming up to 150~200 DEG C, refining continues to be incubated 30~100 minutes；
(3) cool, it is composite lubricated to obtain High-performance graphene after temperature drops to 20~40 DEG C, after grinding homogenizing
Fat.
The present invention is specifically described below by embodiment.It is necessarily pointed out that, following examples are only used
In the invention will be further described, it is impossible to be interpreted as limiting the scope of the invention, professional and technical personnel in the field
Some the nonessential modifications and adaptations made according to the content of the invention described above, still fall within protection scope of the present invention.
Embodiment 1
Embodiments of the invention 1 provide a kind of High-performance graphene complex grease, in parts by weight, at least including with
Lower component,
100 parts of lubricating base oil；
1 part of dispersant；
5 parts of thickening agent；
10 parts of antiwear additive；
0.1 part of graphene mixture；
10 parts of calcium lignosulfonate；
1 part of nano silicon；
The graphene mixture is graphene oxide, ammonification graphene, the mixing of sulfonated graphene.
Described lubricating base oil is mineral oil, and the mineral oil is 150# white oils；
In the graphene mixture, the weight ratio between graphene oxide, ammonification graphene, sulfonated graphene is 100：
1：12；
Described dispersant is polyisobutene succinimide；
Described thickening agent is sulfurized alkylphenol calcium；
Described antiwear additive is molybdenum disulfide；
Described calcium lignosulfonate, is purchased from Shandong Lv Cheng Chemical Co., Ltd.s；
Described nano silicon is purchased from Guangzhou SunNa trade Co., Ltds, and product type is SQ-1；
The preparation method of the High-performance graphene complex grease, at least comprises the following steps：
(1) lubricating base oil of corresponding parts by weight, calcium lignosulfonate, graphene mixture are added in reactor,
Stirred at 100 DEG C 1 hour, be then incubated 3 hours at 70 DEG C；
(2) dispersant, thickening agent, the antiwear additive of corresponding parts by weight are added into step (1), at 120 DEG C, continues to stir
1 hour, nano silicon is then added, 150 DEG C are warming up to, refining continues to be incubated 100 minutes；
(3) cool, after temperature drops to 20 DEG C, High-performance graphene complex grease is obtained after grinding homogenizing.
Embodiment 2
Embodiments of the invention 2 provide a kind of High-performance graphene complex grease, in parts by weight, at least including with
Lower component,
100 parts of lubricating base oil；
5 parts of dispersant；
15 parts of thickening agent；
30 parts of antiwear additive；
3 parts of graphene mixture；
40 parts of calcium lignosulfonate；
5 parts of nano silicon；
The graphene mixture is graphene oxide, ammonification graphene, the mixing of sulfonated graphene.
Described lubricating base oil is mineral oil, and the mineral oil is 150# white oils；
In the graphene mixture, the weight ratio between graphene oxide, ammonification graphene, sulfonated graphene is 100：
1：12；
Described dispersant is polyisobutene succinimide；
Described thickening agent is sulfurized alkylphenol calcium；
Described antiwear additive is molybdenum disulfide；
Described calcium lignosulfonate, is purchased from Shandong Lv Cheng Chemical Co., Ltd.s；
Described nano silicon is purchased from Guangzhou SunNa trade Co., Ltds, and product type is SQ-1；
The preparation method of the High-performance graphene complex grease, at least comprises the following steps：
(1) lubricating base oil of corresponding parts by weight, calcium lignosulfonate, graphene mixture are added in reactor,
Stirred at 100 DEG C 1 hour, be then incubated 3 hours at 70 DEG C；
(2) dispersant, thickening agent, the antiwear additive of corresponding parts by weight are added into step (1), at 120 DEG C, continues to stir
1 hour, nano silicon is then added, 150 DEG C are warming up to, refining continues to be incubated 100 minutes；
(3) cool, after temperature drops to 20 DEG C, High-performance graphene complex grease is obtained after grinding homogenizing.
Embodiment 3
Embodiments of the invention 3 provide a kind of High-performance graphene complex grease, in parts by weight, at least including with
Lower component,
100 parts of lubricating base oil；
3 parts of dispersant；
10 parts of thickening agent；
20 parts of antiwear additive；
2 parts of graphene mixture；
30 parts of calcium lignosulfonate；
3 parts of nano silicon；
The graphene mixture is graphene oxide, ammonification graphene, the mixing of sulfonated graphene.
Described lubricating base oil is mineral oil, and the mineral oil is 150# white oils；
In the graphene mixture, the weight ratio between graphene oxide, ammonification graphene, sulfonated graphene is 100：
1：12；
Described dispersant is polyisobutene succinimide；
Described thickening agent is sulfurized alkylphenol calcium；
Described antiwear additive is molybdenum disulfide；
Described calcium lignosulfonate, is purchased from Shandong Lv Cheng Chemical Co., Ltd.s；
Described nano silicon is purchased from Guangzhou SunNa trade Co., Ltds, and product type is SQ-1；
The preparation method of the High-performance graphene complex grease, at least comprises the following steps：
(1) lubricating base oil of corresponding parts by weight, calcium lignosulfonate, graphene mixture are added in reactor,
Stirred at 100 DEG C 1 hour, be then incubated 3 hours at 70 DEG C；
(2) dispersant, thickening agent, the antiwear additive of corresponding parts by weight are added into step (1), at 120 DEG C, continues to stir
1 hour, nano silicon is then added, 150 DEG C are warming up to, refining continues to be incubated 100 minutes；
(3) cool, after temperature drops to 20 DEG C, High-performance graphene complex grease is obtained after grinding homogenizing.
Embodiment 4
Embodiments of the invention 4 provide a kind of High-performance graphene complex grease, in parts by weight, at least including with
Lower component,
100 parts of lubricating base oil；
3 parts of dispersant；
10 parts of thickening agent；
20 parts of antiwear additive；
2 parts of graphene mixture；
30 parts of calcium lignosulfonate；
3 parts of nano silicon；
The graphene mixture be graphene oxide, ammonification graphene, sulfonated graphene, nitrogen-doped graphene it is mixed
Close.
Described lubricating base oil is mineral oil, and the mineral oil is 150# white oils；
In the graphene mixture, between graphene oxide, ammonification graphene, sulfonated graphene, nitrogen-doped graphene
Weight ratio be 100：1：12：10；
Described dispersant is polyisobutene succinimide；
Described thickening agent is sulfurized alkylphenol calcium；
Described antiwear additive is molybdenum disulfide；
Described calcium lignosulfonate, is purchased from Shandong Lv Cheng Chemical Co., Ltd.s；
Described nano silicon is purchased from Guangzhou SunNa trade Co., Ltds, and product type is SQ-1；
The preparation method of the High-performance graphene complex grease, at least comprises the following steps：
(1) lubricating base oil of corresponding parts by weight, calcium lignosulfonate, graphene mixture are added in reactor,
Stirred at 100 DEG C 1 hour, be then incubated 3 hours at 70 DEG C；
(2) dispersant, thickening agent, the antiwear additive of corresponding parts by weight are added into step (1), at 120 DEG C, continues to stir
1 hour, nano silicon is then added, 150 DEG C are warming up to, refining continues to be incubated 100 minutes；
(3) cool, after temperature drops to 20 DEG C, High-performance graphene complex grease is obtained after grinding homogenizing.
Embodiment 5
Embodiments of the invention 5 provide a kind of High-performance graphene complex grease, in parts by weight, at least including with
Lower component,
100 parts of lubricating base oil；
3 parts of dispersant；
10 parts of thickening agent；
20 parts of antiwear additive；
2 parts of graphene mixture；
30 parts of calcium lignosulfonate；
3 parts of nano silicon；
The graphene mixture be graphene oxide, ammonification graphene, sulfonated graphene, nitrogen-doped graphene it is mixed
Close.
Described lubricating base oil is mineral oil, and the mineral oil is 150# white oils；
In the graphene mixture, between graphene oxide, ammonification graphene, sulfonated graphene, nitrogen-doped graphene
Weight ratio be 100：1：12：10；
Described dispersant is polyisobutene succinimide；
Described thickening agent is sulfurized alkylphenol calcium；
Described antiwear additive is molybdenum disulfide；
Described calcium lignosulfonate, is purchased from Shandong Lv Cheng Chemical Co., Ltd.s；
Described nano silicon is silane coupler modified nano silicon.
The preparation method of the silane coupler modified nano silicon at least comprises the following steps：
In the reactor, solvent 80ml toluene and 10g nano silicons, ultrasonic disperse 30min are added, 5g is sequentially added
N- (2- aminoethyls) -3- aminopropyl trimethoxysilanes, 1g 3- Mercaptopropyltriethoxysilanes, the back flow reaction at 100 DEG C
5h, filtering, ethanol is washed 3 times, and silane coupler modified nano silicon is obtained after drying.
The preparation method of the High-performance graphene complex grease, at least comprises the following steps：
(1) lubricating base oil of corresponding parts by weight, calcium lignosulfonate, graphene mixture are added in reactor,
Stirred at 100 DEG C 1 hour, be then incubated 3 hours at 70 DEG C；
(2) dispersant, thickening agent, the antiwear additive of corresponding parts by weight are added into step (1), at 120 DEG C, continues to stir
1 hour, nano silicon is then added, 150 DEG C are warming up to, refining continues to be incubated 100 minutes；
(3) cool, after temperature drops to 20 DEG C, High-performance graphene complex grease is obtained after grinding homogenizing.
Comparative example 1
The be the same as Example 3 of comparative example 1, difference is, the graphene is only graphene oxide.
Comparative example 2
The be the same as Example 3 of comparative example 2, difference is, the graphene is only ammonification graphene.
Comparative example 3
The be the same as Example 3 of comparative example 3, difference is, the graphene is only sulfonated graphene.
Comparative example 4
The be the same as Example 5 of comparative example 4, difference is, the silane coupler is only N- (2- aminoethyls) -3- aminopropyls three
Methoxy silane.
Comparative example 5
The be the same as Example 5 of comparative example 5, difference is, the silane coupler is only 3- Mercaptopropyltriethoxysilanes.
Comparative example 6
The be the same as Example 5 of comparative example 6, difference is, the silane coupler is only 3- (2,3- the third oxygen of epoxy) propyl group three
Methoxy silane.
Comparative example 7
The be the same as Example 5 of comparative example 7, difference is, not including graphene.
Comparative example 8
The be the same as Example 5 of comparative example 8, difference is, not including nano silicon.
Method of testing
1st, maximum nonseizure load PB：Maximum nonseizure load test is tested using GB/T 3142-1982 standards；
This indicator measurements is higher, illustrates that oil lubrication performance is better.
2nd, sintering load PD：Sintering load test is using GB/T 3142-1982；Sintering load is higher, illustrates lubricating oil
Extreme boundary lubrication performance is better.
3rd, wear scar diameter d：Wear scar diameter d tests are using SH/T 0189-1992 (292N, 60min, 75 DEG C, 1200r/
min)；Wear scar diameter is smaller, illustrates the antiwear property of lubricating oil.
4th, decay resistance：Decay resistance test is using GB/T 5018 (52 DEG C, 48h).
The performance test of table 1
From table 1 it follows that the graphene complex grease of the application has good greasy property.
Foregoing example is merely illustrative, some features of the feature for explaining the disclosure.Appended claim
The scope as wide as possible for requiring to be contemplated that is intended to, and embodiments as presented herein is only according to all possible embodiment
Combination selection embodiment explanation.Therefore, the purpose of applicant is appended claim not by the explanation present invention
Feature example selectional restriction.And the progress in science and technology by formed language performance it is inaccurate due to and not
The possible equivalent or son being presently considered are replaced, and these changes should also be interpreted by appended in the conceived case
Claim is covered.
Claims (10)
1. a kind of High-performance graphene complex grease, it is characterised in that in parts by weight, at least including following components,
100 parts of lubricating base oil；
1~5 part of dispersant；
5~15 parts of thickening agent；
10~30 parts of antiwear additive；
0.1~3 part of graphene mixture；
10~40 parts of calcium lignosulfonate；
1~5 part of nano-particle；
The graphene mixture is graphene oxide, ammonification graphene, the mixing of sulfonated graphene.
2. High-performance graphene complex grease as claimed in claim 1, it is characterised in that the lubricating base oil is selected from：
Mineral oil, hydrocarbon system artificial oil, ester system oil, ether system oil in any one.
3. High-performance graphene complex grease as claimed in claim 2, it is characterised in that the lubricating base oil is at 40 DEG C
Under kinematic viscosity be 50~200mm2/s。
4. High-performance graphene complex grease as claimed in claim 1, it is characterised in that the dispersant is selected from：It is poly- different
Any one in butylene succimide, acetone, propene carbonate.
5. High-performance graphene complex grease as claimed in claim 1, it is characterised in that the thickening agent is selected from：Vulcanization
The mixing of any one or more in alkyl phenol calcium, carbamido thickening agent.
6. High-performance graphene complex grease as claimed in claim 1, it is characterised in that the antiwear additive is selected from：Two sulphur
For Acidic phosphates zinc, two thio dialkyl amido formic acid molybdenums, two thio dialkyl amido lead formates, molybdenum disulfide, polytetrafluoro
The mixing of any one or more in ethene, dibutyl dithiocaarbamate antimony, tungsten disulfide, selenium disulfide.
7. High-performance graphene complex grease as claimed in claim 1, it is characterised in that in the graphene mixture,
Weight ratio between graphene oxide, ammonification graphene, sulfonated graphene is 100：1：12.
8. High-performance graphene complex grease as claimed in claim 1, it is characterised in that the nano-particle is selected from：Receive
Rice silica, nano aluminium oxide, nanometer sulfoacid calcium, nano-calcium carbonate, nano molybdenum disulfide, nano aluminum nitride, nano-silica
Change any one or a few the mixing in titanium.
9. High-performance graphene complex grease as claimed in claim 8, it is characterised in that the High-performance graphene is combined
Lubricating grease also includes antioxidant, antirust agent, oiliness improver, viscosity index improving agent, pour-point depressant, defoamer, emulsifying agent, metallic blunt
The mixing of any one or more in agent, detergent-dispersant additive.
10. the preparation method of High-performance graphene complex grease described in claim 1~9, it is characterised in that at least including with
Lower step：
(1) lubricating base oil, calcium lignosulfonate, graphene of corresponding parts by weight are added in reactor, at 50~100 DEG C
Stirring 1~2 hour, is then incubated 1~5 hour at 70~80 DEG C；
(2) dispersant, thickening agent, the antiwear additive of corresponding parts by weight are added into step (1), at 70~120 DEG C, continues to stir
1~3 hour, nano silicon is then added, 150~200 DEG C are warming up to, refining continues to be incubated 30~100 minutes；
(3) cool, after temperature drops to 20~40 DEG C, High-performance graphene complex grease is obtained after grinding homogenizing.
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| CN110643412B (en) * | 2019-08-30 | 2022-03-29 | 无锡市惠山区川大石墨烯应用研究中心 | High-temperature graphene fluorine-based lubricating grease and preparation method thereof |
| CN110643412A (en) * | 2019-08-30 | 2020-01-03 | 无锡市惠山区川大石墨烯应用研究中心 | High-temperature graphene fluorine-based lubricating grease and preparation method thereof |
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| US11332688B2 (en) | 2020-07-13 | 2022-05-17 | Guangxi Liugong Machinery Co., Ltd. | Lubricating oil or grease with anti-wear, anti-friction and stable dispersion and preparation method thereof |
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