CN105586135A - Urea-based lubricating grease composition with excellent antifriction property and preparation method therefor - Google Patents
Urea-based lubricating grease composition with excellent antifriction property and preparation method therefor Download PDFInfo
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- 0 SC1=SC(Sc(cc2)ccc2Ns2nc3ccccc3[s]2)=N*1 Chemical compound SC1=SC(Sc(cc2)ccc2Ns2nc3ccccc3[s]2)=N*1 0.000 description 1
- MHLMJBQJKZOTNJ-UHFFFAOYSA-N Sc1nnc(Sc(cc2)ccc2Ns2nc3ccccc3[s]2)[s]1 Chemical compound Sc1nnc(Sc(cc2)ccc2Ns2nc3ccccc3[s]2)[s]1 MHLMJBQJKZOTNJ-UHFFFAOYSA-N 0.000 description 1
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Abstract
The invention discloses a urea-based lubricating grease composition with excellent antifriction property. The lubricating grease composition contains the following ingredients in percentage by weight: 65-95wt% of lubricating base oil, 5-35wt% of urea-based thickener and 0.1-15wt% of additive, wherein the additive contains a compound with a structure represented by a formula (I) shown in the description. The invention further provides a preparation method for the urea-based lubricating grease composition with excellent antifriction property. The urea-based lubricating grease composition disclosed by the invention contains the multipurpose additive, so that the antifriction capability and oxidation resistance of lubricating grease are greatly improved. The lubricating grease disclosed by the invention has excellent high-temperature properties, mechanical stability, oxidation resistance, colloid stability, waterproofing performance, bearing capacity, antifriction property and the like and can be adequate to harsh working conditions, such as high-temperature, high-speed, high-load and watery.
Description
Technical field
The present invention relates to lubricating grease field, particularly, relate to a kind of Wear vesistance that contains special additiveExcellent urea-based lubricating grease composition and preparation method thereof.
Background technology
Urea-base grease is to be obtained by organic compound urea multiviscosisty mineral oil or artificial oil, and thickening agent is containing goldBelong to ion, avoided the catalytic action of metal ion to base oil oxidation, urea-base grease has goodOxidation stability, thermostability and other various premium properties, also have long especially service life, isA kind of multipurpose grease, can prepare various lubricating grease and meet different instructions for uses, be applicable to high temperature,Low temperature, high load capacity, wide velocity interval and the occasion contacting with impedance dielectric, be widely used in electrical equipment, smeltingThe industries such as gold, food, automobile, papermaking.
Urea-base grease generally selects mineral oil or artificial oil to make base oil, but mineral oil is at natural environmentIn biodegradable ability, in environment, gather and to environment. Therefore Green LubricantsDemand is ascendant trend year by year, and Green Lubricants generally has polyethers, synthetic ester and crude vegetal. ItsMiddle vegetable oil is with low cost, good greasy property is enriched, had in source, and viscosity index (VI) is high, biology fallsSolution is good, but contains a large amount of two keys in general vegetable oil molecule, and oxidation stability is poor.CN101407746A mixes alcohol, metatitanic acid, four butyl esters and vegetable oil, at 20-80 DEG C of temperature, reacts,React the remaining alcohol of complete separation, obtain modified vegetable oil, the oxidation that has greatly improved vegetable oil is stableProperty, extreme pressure anti-wear.
There are in recent years a large amount of patents to inquire into the performance of urea-base grease, if US5158694 is by two isocyanidesAcid esters reacts and prepares polyurea grease with water and amine, but the dropping point of its product is between 230-260 DEG C;CN1272530, under the existence of base oil, makes C8-C24 fatty amine and excessive di-isocyanate reaction,Water neutralizes unreacted vulcabond, continue to react to temperature be 130-200 DEG C, this legal system is standbyTwo urea grease dropping points reach 260-330 DEG C; CN1580211 mixes organic amine and isocyanates alsoReaction, is elevated to after 100-150 DEG C until temperature of charge, adds quench oil to make material cooling rapidly, grindsBecome fat, the standby urea-base grease of this legal system has stable vibration values; CN1408825 will at 50-120 DEG CBase oil, alkylamine and excessive vulcabond mix, and react, and add excessive water neutralization not anti-The vulcabond of answering, is warming up to melting, adds quench oil, cooling go out still obtain the lubricated of appearance transparentFat; CN101368129 has boratory extreme pressure anti-wear additives to having added in system, improved lubricating greaseCombination property, has reduced cost; CN1657599 by adding calcium containing compound in polyurea greaseImprove the oxidation stability of lubricating grease, its complex process; CN101111591A relates to four urea greases,But preparation technology's more complicated, but also introduced metal ion, this will affect the oxygen of polyurea greaseChange stability; CN101693851A adopts the mixture of two ureas, triuret, four ureas and introduces amidic-salt thickThe fat that agent makes, has excellent high-temperature behavior, resistance leachability, good extreme pressure anti-wear;CN1056313 thickening agent used is two ureas and four urea mixtures, and this fat has more in the machinery of long-term runningThere is good performance.
In recent years along with the development of modern industry, bearing, automobile, printing and dyeing, mine, metallurgy, aerospace etc.Industrial department has proposed more and more harsher requirement to the quality of lubricating grease, and many lubricant housings are all onceProperty fill fat, in running, no longer supplement or change, so require higher to the abrasion resistance of fat.
Summary of the invention
The object of the invention is the high request in order to meet the abrasion resistance to lubricating grease, a kind of anti-attrition is providedUrea-based lubricating grease composition of excellent performance and preparation method thereof.
The present inventor finds under study for action, and the additive in lubricant composition contains formula (I)Shown in the multipurpose additive of structure:
Can make lubricant composition there is the performances such as good anti-attrition is anti-oxidant.
Therefore, to achieve these goals, on the one hand, the invention provides a kind of Wear vesistance excellenceUrea-based lubricating grease composition, taking the weight of lubricant composition as benchmark, described lubricant composition comprisesFollowing component: the lubricating base oil of 65-95 % by weight, carbamido thickening agent and the 0.1-15 of 5-35 % by weightThe additive of % by weight, the compound that described additive contains structure shown in formula (I):
Preferably, taking the weight of lubricant composition as benchmark, described lubricant composition comprises following groupPoint: the lubricating base oil of 70-90 % by weight, the carbamido thickening agent of 8-30 % by weight and 0.5-10 % by weightAdditive.
Preferably, taking the weight of lubricant composition as benchmark, the compound of structure shown in formula (I)Content is 0.1-10 % by weight, more preferably 1-5 % by weight.
On the other hand, the invention provides a kind of preparation of urea-based lubricating grease composition of Wear vesistance excellenceMethod, described method comprises:
(1) part lubricating base oil, vulcabond, amine hybrid reaction are generated to carbamido thickening agent;
(2) step (1) reaction gained system is warming up to 180-210 DEG C, keeps 5-25min, then addEnter to remain lubricating base oil, stir and be cooled to 90-130 DEG C, add additive, mix;
(3) grind 2-3 time by three-roller;
Wherein, taking the weight of lubricant composition as benchmark, the consumption of lubricating base oil is that 65-95 is heavyThe consumption of the carbamido thickening agent of measure %, being prepared by vulcabond, amine is 5-35 % by weight, additiveConsumption is 0.1-15 % by weight, the compound that described additive contains structure shown in formula (I):
Preferably, taking the weight of lubricant composition as benchmark, the consumption of lubricating base oil is that 70-90 is heavyThe consumption of the carbamido thickening agent of measure %, being prepared by vulcabond, amine is 8-30 % by weight, additiveConsumption is 0.5-10 % by weight.
Preferably, taking the weight of lubricant composition as benchmark, the compound of structure shown in formula (I)Consumption is 0.1-10 % by weight, more preferably 1-5 % by weight.
Urea-based lubricating grease composition of the present invention, owing to containing multipurpose additive, has greatly improved lubricatedAnti-attrition ability and the oxidation resistance of fat. Lubricating grease of the present invention has splendid high-temperature behavior, machinery peaceQualitative, non-oxidizability, colloid stability, water proofing property, bearing capacity and antifriction performance etc., can be competent atIn high temperature, at a high speed, the harsh working condition such as high load capacity, many water.
Other features and advantages of the present invention are described in detail the detailed description of the invention part subsequently.
Brief description of the drawings
Fig. 1 is the reaction equation of the step (a) of preparing multipurpose additive.
Fig. 2 is the reaction equation of the step (b) of preparing multipurpose additive.
Fig. 3 is the hydrogen spectrum spectrogram of the multipurpose additive prepared of preparation example.
Fig. 4 is the carbon spectrum spectrogram of the multipurpose additive prepared of preparation example.
Fig. 5 is the mass spectrogram of the multipurpose additive prepared of preparation example.
Detailed description of the invention
Below the specific embodiment of the present invention is elaborated. Should be understood that, retouch in this placeThe detailed description of the invention of stating only, for description and interpretation the present invention, is not limited to the present invention.
The invention provides a kind of urea-based lubricating grease composition of Wear vesistance excellence, with lubricant compositionWeight be benchmark, lubricant composition comprises following component: the lubricating base oil of 65-95 % by weight,The additive of the carbamido thickening agent of 5-35 % by weight and 0.1-15 % by weight, additive contains shown in formula (I)The compound of structure:
In the present invention, what multipurpose additive referred to is the compound of structure shown in formula (I).
In the present invention, preferably, taking the weight of lubricant composition as benchmark, described lubricant compositionComprise following component: the lubricating base oil of 70-90 % by weight, carbamido thickening agent and the 0.5-10 of 8-30 % by weightThe additive of % by weight.
In the present invention, taking the weight of lubricant composition as benchmark, the compound of structure shown in formula (I)Content be preferably 0.1-10 % by weight, more preferably 1-5 % by weight.
The present invention is intended to contain structure shown in formula (I) by the additive in urea-based lubricating grease compositionCompound and realize goal of the invention, even if urea-based lubricating grease composition has the property such as good anti-attrition is anti-oxidantEnergy. Therefore, for the selection of each conventional component in urea-base grease, all less than specific restriction.
In the present invention, lubricating base oil can be the conventional lubricating base oil using in this area, for example canFor at least one in mineral oil, vegetable oil and artificial oil. 100 DEG C of kinematic viscosity of lubricating base oil are preferredFor 4-60mm2/ s, more preferably 5-32mm2/ s. For the concrete kind of mineral oil, vegetable oil and artificial oilAlso there is no particular limitation for class, can adopt the conventional mineral oil in this area, vegetable oil and artificial oil, exampleAs, mineral oil can be selected paraffinic base, cycloalkyl series, vegetable oil can be castor oil, rapeseed oil,At least one in peanut oil and soybean wet goods, artificial oil can be poly-a-olefin oil (PAO), ester class oil,At least one in fluorocarbon oil and silicone oil etc.
In the present invention, carbamido thickening agent is preferably the product of amine and vulcabond, for example, and urea groupsThickening agent can be two carbamido thickening agents, four carbamido thickening agents, six carbamido thickening agents and eight carbamido thickening agentsIn at least one.
The structure of two carbamido thickening agents is preferably:
The structure of four carbamido thickening agents is preferably:
The structure of six carbamido thickening agents is preferably:
The structure of eight carbamido thickening agents is preferably:
In the structural formula of above-mentioned two, four, six, eight carbamido thickening agents, R1、R1’Can be identical also passableDifference, can be alkyl, cycloalkyl or aryl, and the carbon number of alkyl or cycloalkyl can be 8-24, preferably10-18, aryl can be the phenyl of phenyl or replacement, preferably phenyl or C1-C3 alkyl or halogen replacePhenyl.
Wherein, R2Can be alkylidene or arlydene, the carbon number of alkylidene can be 2-12, preferably 2-8,Arlydene can be phenylene or biphenylene.
Wherein, R3Can be arlydene, alkylidene or cycloalkylidene, arlydene, alkylidene or sub-cycloalkanesThe carbon number of base can be 6-30, preferably 6-20, R3More preferably InAt least one.
Above-mentioned carbamido thickening agent can adopt the thinkable the whole bag of tricks of those skilled in the art institute to obtain.
In the present invention, because multipurpose additive and other additives of structure shown in formula (I) have betterCompatibility, therefore, according to the use needs of lubricating grease, additive of the present invention can also contain otherAntioxidant, extreme pressure anti-wear additives and antirust agent at least one.
In the present invention, for other the kind of antioxidant, extreme pressure anti-wear additives, antirust agent and content without spyDifferent requirement, can adopt kind and the content of this area routine. For example, antioxidant can be anti-for arylamine classOxygen agent, is preferably at least one in diphenylamines, PA and di-iso-octyldiphenylamine, more preferablyFor di-iso-octyldiphenylamine, the 0.01-5 that the content of antioxidant can account for lubricant composition gross weight is heavyAmount %, preferably 0.1-2.5 % by weight; Extreme pressure anti-wear additives can be two sulfo-Acidic phosphates zinc, two sulfo-sDialkyl amido formic acid molybdenum, two sulfo-dialkyl amido lead formates, molybdenum bisuphide, polytetrafluoroethylene (PTFE), twoButyl antimony dithiocarbamate, tungsten disulfide, selenium disulfide, fluorographite, calcium carbonate and zinc oxideIn at least one, the 0.5-12 that the content of extreme pressure anti-wear additives can account for lubricant composition gross weight is heavyAmount %, is preferably 0.5-5 % by weight; Antirust agent can be barium mahogany sulfonate, petroleum sodium sulfonate, benzo thiopheneAt least one in azoles, BTA, zinc naphthenate and alkenyl succinic acid, the content of antirust agent canThe 0.01-4.5 % by weight that accounts for lubricant composition gross weight, is preferably 0.1-2 % by weight.
In the present invention, shown in formula (I), the preparation method of the compound of structure preferably includes:
(a) aniline, sulfur chloride and 4-chloroaniline are reacted to the intermediate shown in production (II)M，
(b) intermediate M step (a) being obtained and dimercapto-1,3,4-thiadiazole are under alkali conditionCarry out nucleophilic substitution, the multipurpose additive shown in production (I),
In step of the present invention (a), the concrete mode that aniline, sulfur chloride and 4-chloroaniline are reactedPreferably include:
(i) under inert atmosphere, in the first solvent, by aniline and sulfur chloride at-20-0 DEG C fullyReact;
(ii) 4-chloroaniline is added in the reaction system of step (i), at 15-30 DEG C, react 1-3h.
In the present invention, inert atmosphere can be the inert atmosphere of this area routine, for example can by nitrogen,The gases such as argon gas provide.
In step of the present invention (i), the first solvent be preferably selected from carrene, oxolane, toluene,At least one in dimethylbenzene and dioxane, more preferably carrene and/or oxolane, more enters oneStep is preferably carrene.
In step in the present invention (i), fully react and refer to and react completely, reaction raw materials is completeEntirely react. Can adopt the conventional method in this area to monitor reaction, react completely confirming,For example can adopt the methods such as TLC (TLC) or gas-chromatography to monitor.
In step of the present invention (ii), at 15-30 DEG C, react 1-3h, preferably fully anti-in step (i)Ying Hou, rises to 15-30 DEG C gradually by the temperature of reaction system, then adds 4-chloroaniline to react 1-3h.Under this preferable case, can further improve reaction yield.
In step of the present invention (ii), the mode that adds of 4-chloroaniline is preferably gradation and adds, and for example canDivide and add for 3-4 time. Under this preferable case, can further improve reaction yield. Add for gradationTime, each addition can be identical, also can be different, and for easy to operate, preferably each addingMeasure identical.
In step of the present invention (ii), reaction 1-3h, the mode that stops reaction can be art technology peopleThe thinkable variety of way of member, for example, can add quencher to carry out cancellation, and quencher can be thisThe quencher that field is conventional can be for example saturated aqueous common salt.
In the present invention, the consumption of aniline, sulfur chloride and 4-chloroaniline is essentially equimolar amounts, but anilineWith sulfur chloride can be suitably excessive. The mol ratio of aniline, sulfur chloride and 4-chloroaniline is preferably 0.9-1.5:0.9-1.5：0.8-1.2。
It will be understood by those skilled in the art that in step of the present invention (a), purer in order to obtainIntermediate M, also need reacted system to carry out post processing, the mode of post processing can comprise washesWash, be dried, removal of solvent under reduced pressure, for example, the reaction system after cancellation is used respectively to distilled water and saturatedSaline solution washing then adds the drier such as anhydrous calcium chloride or anhydrous sodium sulfate at 15-30 DEG C,Keep 10-60min. Remove by filter after drier, at 0.01-0.05MPa, 40-60 DEG C, remove desolventizing,To obtain intermediate M.
In step of the present invention (a), the reaction equation that aniline, sulfur chloride and 4-chloroaniline reactAs shown in Figure 1, in Fig. 1, what the first solvent adopted is carrene, only for purposes of illustration,Scope of the present invention is not construed as limiting.
In step of the present invention (b), the condition of nucleophilic substitution preferably includes: under inert atmosphere,In the second solvent, dimercapto-1,3,4-thiadiazole, alkaline reagent and catalyst are mixed at 15-30 DEG C10-30min, then adds intermediate M, fully reacts. Be that alkali condition is provided by alkaline reagent.
" inert atmosphere ", " fully reacting " as previously mentioned, do not repeat them here.
In the present invention, intermediate M preferably slowly adds, for example, can gradation add, and generally can divideAdd for 3-4 time. Under this preferable case, can further improve reaction yield. Add for gradation fashionable,Each addition can be identical, also can be different, and for easy to operate, preferably each addition phaseWith.
In the present invention, the second solvent is preferably selected from carrene, oxolane, toluene, dimethylbenzene, N, N-At least one in dimethyl formamide, more preferably carrene and/or DMF,Further be preferably DMF.
In the present invention, alkaline reagent is preferably selected from the inorganic bases such as potash, sodium carbonate, sodium methoxide extremelyFew a kind of.
In the present invention, catalyst is preferably potassium sulfate.
In step of the present invention (b), the use of dimercapto-1,3,4-thiadiazole, alkaline reagent and intermediate MAmount is essentially equimolar amounts, but dimercapto-1,3,4-thiadiazole and alkaline reagent can be suitably excessive. TwoSulfydryl-1, the mol ratio of 3,4-thiadiazoles, alkaline reagent and intermediate M is preferably 0.9-3.0:0.9-5.0:0.8-1.5。
In step of the present invention (b), the consumption of catalyst can be catalytic amount, with dimercapto-1, and 3,4-thiophene twoThe molal quantity of azoles is benchmark, and the consumption of catalyst is preferably 5-100 % by mole, and more preferably 10-50 rubsYou are %.
In step of the present invention (b), the reaction that dimercapto-1,3,4-thiadiazole and intermediate M reactAs shown in Figure 2, in Fig. 2, what alkaline reagent adopted is potash to equation, is only illustrational order, scope of the present invention is not construed as limiting.
It will be understood by those skilled in the art that in order to obtain purer end product, i.e. the present inventionMultipurpose additive, the method that the present invention prepares multipurpose additive preferably also comprises reacted system is enteredRow post processing, the mode of post processing can comprise washing, dry, removal of solvent under reduced pressure, for example, will fillDivide reacted system to pour in the ethyl acetate (or carrene) of 1-10 times of volume, respectively with steamingHeat up in a steamer water and saturated common salt water washing, then at 15-30 DEG C, add anhydrous calcium chloride or anhydrous sodium sulfateIn drier, keep 10-60min. Remove by filter after drier, at 0.01-0.05MPa, 40-60 DEG CDown except desolventizing, to obtain end product.
Each step of the method for the compound of structure shown in preparation formula in the present invention (I) preferably under agitationCarrying out, without particular/special requirement, can be the mixing speed of this area routine for mixing speed, for example, stirsThe speed of mixing can be 100-800rpm.
In the present invention, without particular/special requirement, can be that this area is normal for the amount of the first solvent and the second solventThe solvent load of rule, this is conventionally known to one of skill in the art, does not repeat them here.
As mentioned above, the present invention is intended to contain formula (I) by the additive in urea-based lubricating grease compositionShown in structure compound and realize goal of the invention, even if lubricant composition has good anti-attrition antioxygenThe performances such as change. Therefore, without particular/special requirement, can adopt this area for the preparation method of urea-base greaseThe conventional method using, for example, second aspect, the present invention also provides a kind of urea of Wear vesistance excellenceThe preparation method of base grease composition, the method comprises:
(1) part lubricating base oil, vulcabond, amine hybrid reaction are generated to carbamido thickening agent;
(2) step (1) reaction gained system is warming up to 180-210 DEG C, keeps 5-25min, then addEnter to remain lubricating base oil, stir and be cooled to 90-130 DEG C, add additive, mix;
(3) grind 2-3 time by three-roller;
Wherein, taking the weight of lubricant composition as benchmark, the consumption of lubricating base oil is that 65-95 is heavyThe consumption of the carbamido thickening agent of measure %, being prepared by vulcabond, amine is 5-35 % by weight, additiveConsumption is 0.1-15 % by weight, the compound that additive contains structure shown in formula (I):
It will be understood by those skilled in the art that in the inventive method, the consumption of lubricating base oil is portionDivide the consumption sum of consumption with the residue lubricating base oil of lubricating base oil.
In the inventive method, preferably, taking the weight of lubricant composition as benchmark, lubricating base oilThe consumption of the carbamido thickening agent that consumption is 70-90 % by weight, prepared by vulcabond, amine is that 8-30 is heavyAmount %, the consumption of additive is 0.5-10 % by weight.
In the inventive method, taking the weight of lubricant composition as benchmark, the change of structure shown in formula (I)The consumption of compound is preferably 0.1-10 % by weight, more preferably 1-5 % by weight.
In the present invention, for step (1), part lubricating base oil, vulcabond, amine are mixed anti-The method of carbamido thickening agent should be generated without particular/special requirement, the conventional the whole bag of tricks in this area can be adopted, exampleAs:
In the time of preparation two carbamido thickening agent, method can comprise: the base oil of monoamine and 1/5-2/5 is mixedClose and be heated to 50-80 DEG C, stir 2-8 minute, organic amine is melted completely; Again by the basis of 1/5-2/5Oil to 50-80 DEG C, stirs 2-8 minute with vulcabond Hybrid Heating, and vulcabond is melted completelyChange; Then above-mentioned two groups of solution are mixed, at 80-100 DEG C, reaction 20-60min. Vulcabond withThe mol ratio of monoamine is 1:2.
When preparation is when four carbamido thickening agents, method can comprise: first by the base oil of 1/5-2/5 and two differentCyanate Hybrid Heating, to 50-60 DEG C, adds diamines, is warming up to 80-100 DEG C, reaction 20-60min;The base oil of 1/5-2/5 and individual palpation Hybrid Heating are arrived to 50-60 DEG C; Above-mentioned two kinds of solution are mixed,80-100 DEG C, reaction 20-60min. The mol ratio of vulcabond, diamines and monoamine is 2:1:2.
In the time of preparation six carbamido thickening agent, method can comprise: first by the base oil of 1/5-1/3 and partVulcabond Hybrid Heating is to 50-70 DEG C; Again the base oil of 1/5-1/3 and monoamine Hybrid Heating are arrived50-70 DEG C, slowly joins in said mixture, is warming up to 80-100 DEG C, reaction 20-60min, Xiang QiIn add diamines, constant temperature 80-100 DEG C, reaction 20-60min; Again by the base oil of 1/5-1/3 and remainderVulcabond Hybrid Heating to 50-70 DEG C, slowly join in said mixture, constant temperature 80-100 DEG C,Reaction 20-60min. The mol ratio of added vulcabond, monoamine, diamines and vulcabond successivelyFor 2:2:2:1.
In the time of preparation eight carbamido thickening agent, method can comprise: by the lubricating base oil of 1/5-2/5 and twoIsocyanates Hybrid Heating, to 50-70 DEG C, adds diamines, is warming up to 80-100 DEG C, reaction 20-60min,Again add diamines, constant temperature 80-100 DEG C, reaction 20-60min; By the lubricating base oil of 1/5-2/5 withMonoamine Hybrid Heating, to 50-70 DEG C, joins in said mixture, constant temperature 80-100 DEG C, reaction20-60min. The mol ratio of added vulcabond, diamines, diamines and monoamine is 4:2:1:2 successively.
In the present invention, the lubricating base oil of 1/5-2/5,1/5-1/3 refers to respectively to account for prepares urea-base grease group1/5-2/5, the 1/5-1/3 of compound lubricating base oil total amount used.
The inventive method is all preferably under agitation carried out, and, for example can without particular/special requirement for the speed stirringThink 20-400rpm.
It will be understood by those skilled in the art that according to the urea groups multiviscosisty of being prepared by vulcabond, amineThe consumption of agent, can instead release the consumption of vulcabond, amine, and this is conventionally known to one of skill in the art,Do not repeat them here.
In the inventive method, vulcabond structure is OCN-R3-NCO，R3Can be that carbon number is 6-30,Preferably arlydene, alkylidene or the cycloalkylidene of 6-20, more preferably Deng.Preferred vulcabond can be toluene di-isocyanate(TDI) (TDI), methyldiphenyl group diisocyanate(MDI), 1,6-hexylidene diisocyanate (HDI), dicyclohexyl methyl vulcabond (HMDI)With at least one in xyxylene vulcabond (XDI) etc.
Monoamine can be fatty amine, aliphatic cyclic amine or arylamine, and structural formula is R1-NH2, wherein, R1CanBe alkyl, cycloalkyl or aryl, the carbon number of alkyl or cycloalkyl can be 8-24, preferably 10-18, virtueBase can be the phenyl of phenyl or replacement, the phenyl that preferably phenyl or C1-C3 alkyl or halogen replace. ExcellentThe monoamine of choosing can be the arylamine that is selected from aniline, m-chloroaniline, parachloroanilinum, para-totuidine, and/or choosingFrom the fatty amine of lauryl amine, tetradecy lamine, cetylamine, octadecylamine, cyclohexylamine.
Diamines can be fatty amine or arylamine, and structural formula is NH2-R2-NH2, wherein, R2Can be sub-Alkyl or arlydene, the carbon number of alkylidene can be 2-12, preferably 2-8, arlydene can be phenyleneOr biphenylene. Preferred diamines can be to be selected from p-phenylenediamine (PPD), o-phenylenediamine, 4,4-benzidineAromatic amine, and/or be selected from ethylenediamine, propane diamine, 1, the straight-chain fatty amine of 6-hexamethylene diamine.
Lubricating base oil, additive as previously mentioned, do not repeat them here.
Embodiment
The present invention is further illustrated for following embodiment, but therefore do not limit the present invention.
In the following Examples and Comparative Examples:
The method that monitoring reacts completely: thin-layer chromatography chromatogram (TLC) fluorescence developing method.
Gross production rate=end product mole/aniline mole × 100%
The physico-chemical analysis method of product: by inductively coupled plasma emission of ions spectrographic determination elementContent.
Structure characterization methods: nuclear magnetic resonance method (1H hydrogen spectrum,13C carbon spectrum), high resolution mass spectrum.
Each indication test method: dropping point: GB/T3498; Drawing cone in-degree: GB/T269; Extend workMake cone penetration: GB2360-1980; Oxidation initial temperature: PDSC; Stencil oil-dividing: SH/T0324;Anticorrosive property: GB/T5018; Water drenches number of dropouts: SH/T0109; Tetra-ball machine test PB, PD:SH/T0202; Copper corrosion: GB/T7326; Coefficient of friction: SH/T0847.
Preparation example
In the 500ml flask with electromagnetic agitation (mixing speed is 300rpm), being filled with nitrogen protectsProtect, add the carrene of 150ml, then add the sulfur chloride of 0.2mol, abundant in ice-water bathAfter cooling, add the aniline of 0.2mol. Monitoring is removed ice-water bath after reacting completely, and is placed in 25 DEG C of chambersUnder temperature, question response system rises to after 25 DEG C gradually, divides and adds for 3 times 4-chloroaniline to react, eachAddition is identical, adds altogether 4-chloroaniline 0.15mol. Sustained response adds the saturated food of 30ml after 2 hoursSalt solution cancellation reaction, then proceeds to reaction system in separatory funnel, uses respectively 50ml distilled water and 50mlSaturated common salt water washing, and add 10g anhydrous sodium sulfate dry 20min at 25 DEG C. Filter after filtrationLiquid, at 40 DEG C, steams and desolventizes under 0.05MPa, obtains intermediate M1.
In the 500ml flask with electromagnetic agitation (mixing speed is 400rpm), being filled with nitrogen protectsProtect, add the DMF (DMF) of 150ml, then add 0.2mol dimercapto-1,3,4-The potash of thiadiazoles and 0.2mol, the potassium sulfate of 0.05mol, stir 20 minutes at 25 DEG C, and points 3Inferiorly add above-mentioned intermediate M1, each addition is identical, adds altogether intermediate M10.12mol. MonitoringTo reacting completely, then reaction system is added to 250ml ethyl acetate, and proceed in separatory funnel, pointDo not use 100ml distilled water (twice) and the water washing of 50ml saturated common salt, and add 15g anhydrous slufuric acidSodium is dry 20min at 25 DEG C. Filtrate after filtration is steamed and is desolventized under 40 DEG C, 0.03MPa, obtainsEnd product S1. Calculating gross production rate is 76%.
The physico-chemical analysis data of product are as follows: sulfur content, 41.3%; Nitrogen content, 13.9%.
S1 is carried out to structural characterization, obtain respectively hydrogen spectrum, carbon spectrum and high resolution mass spec spectrogram, respectivelySee Fig. 3, Fig. 4 and Fig. 5.
Can find out from physico-chemical analysis data, Fig. 3, Fig. 4 and Fig. 5 of above-mentioned preparation example, S1 has formula(I) structure shown in.
Embodiment 1
The present embodiment is used for illustrating two urea-based lubricating grease compositions of the present invention and preparation method thereof.
(1) 54.5 grams of octadecylamines and 21 grams of para-totuidine are joined to 475 grams of 500SN base oils(100 DEG C of viscosity are 10mm2/ s, lower same) in, be heated to 60 DEG C, stir 6 minutes, make organic amineMelt completely;
(2) in 475 grams of 500SN base oils, add 50.8 grams of MDI, be heated to 60 DEG C, stir 6Minute, MDI is melted completely;
(3) two groups of solution of step (1) and step (2) are mixed, at 90 DEG C, at 200rpmLower reaction 40min;
(4) while being warming up to 180 DEG C, constant temperature refining 20min;
(5) add 471 grams of 500SN base oils, stir and be cooled to 110 DEG C, add 31.6 grams of S1,Under 200rpm, stir;
(6) grind 2 times by three-roller and become fat. Properties of product are as shown in table 1.
In the lubricating grease that the present embodiment obtains, taking lubricating grease weight as benchmark, consist of: S12 % by weight,Two carbamido thickening agent 8 % by weight, base oil 90 % by weight.
Embodiment 2
The present embodiment is used for illustrating two urea-based lubricating grease compositions of the present invention and preparation method thereof.
(1) 62.1 grams of octadecylamines and 23.7 grams of para-totuidine are joined to 103.5 grams of 150BS base oils(100 DEG C of viscosity are 31mm2/ s, lower same) in, be heated to 50 DEG C, stir 8 minutes, make organic amineMelt completely;
(2) in 100 grams of 150BS base oils, add 40 grams of TDI, be heated to 50 DEG C, stir 8Minute, TDI is melted completely;
(3) two groups of solution of step (1) and step (2) are mixed, at 80 DEG C, at 180rpmLower reaction 60min;
(4) while being warming up to 190 DEG C, constant temperature refining 15min;
(5) add 100 grams of 150BS base oils, stir and be cooled to 90 DEG C, add 4.3 grams of S1,Under 180rpm, stir;
(6) grind 3 times by three-roller and become fat. Properties of product are as shown in table 1.
In the lubricating grease that the present embodiment obtains, taking lubricating grease weight as benchmark, consist of: S11 % by weight,Two carbamido thickening agent 29 % by weight, base oil 70 % by weight.
Embodiment 3
The present embodiment is used for illustrating two urea-based lubricating grease compositions of the present invention and preparation method thereof.
(1) 54.7 grams of lauryl amines and 26.5 grams of para-totuidine are joined to 157 grams of PAO6 synthetic hydrocarbon oils(100 DEG C of viscosity are 5.8mm2/ s, lower same) in, be heated to 70 DEG C, stir 4 minutes, make organic amineMelt completely;
(2) in 165 grams of PAO6 synthetic hydrocarbon oils, add 44.7 grams of TDI, be heated to 70 DEG C, stir4 minutes, TDI is melted completely;
(3) two groups of solution of step (1) and step (2) are mixed, at 100 DEG C, at 300rpmLower reaction 20min;
(4) while being warming up to 200 DEG C, constant temperature refining 10min;
(5) add 150 grams of PAO6 synthetic hydrocarbon oils, stir and be cooled to 120 DEG C, add 31.5 grams of S1,Under 300rpm, stir;
(6) grind 2 times by three-roller and become fat. Properties of product are as shown in table 1.
In the lubricating grease that the present embodiment obtains, taking lubricating grease weight as benchmark, consist of: S15 % by weight,Two carbamido thickening agent 20 % by weight, base oil 75 % by weight.
Embodiment 4
The present embodiment is used for illustrating two urea-based lubricating grease compositions of the present invention and preparation method thereof.
(1) 47.5 grams of lauryl amines and 23.1 grams of para-totuidine are joined to 240 grams of 500SN and 150BSMiscella (100 DEG C of viscosity are 13mm2/ s, lower same) in, be heated to 80 DEG C, stir 2 minutes,Organic amine is melted completely;
(2) in the miscella of 240 grams of 500SN and 150BS, add 55.5 grams of MDI, be heated to80 DEG C, stir 2 minutes, MDI is melted completely;
(3) two groups of solution of step (1) and step (2) are mixed, at 90 DEG C, at 230rpmLower reaction 40min;
(4) while being warming up to 210 DEG C, constant temperature refining 5min;
(5) add the miscella of 209 grams of 500SN and 150BS, stir and be cooled to 130 DEG C, add25.2 grams of S1 stir under 230rpm;
(6) grind 3 times by three-roller and become fat. Properties of product are as shown in table 1.
In the lubricating grease that the present embodiment obtains, taking lubricating grease weight as benchmark, consist of: S13 % by weight,Two carbamido thickening agent 15 % by weight, base oil 82 % by weight.
Comparative example 1
Prepare two urea-base greases according to the method for embodiment 4, different, do not add S1. ProductPerformance is as shown in table 1.
In the lubricating grease that this comparative example obtains, taking lubricating grease weight as benchmark, consist of: two urea groups multiviscosistyAgent 15.5 % by weight, base oil 84.5 % by weight.
Embodiment 5
The present embodiment is used for illustrating four urea-based lubricating grease compositions of the present invention and preparation method thereof.
(1) by 400 grams of 500SN base oils, (100 DEG C of viscosity are 10mm2/ s, lower same) with 40.3Gram TDI Hybrid Heating to 60 DEG C, adds 7.1 grams of ethylenediamines, is warming up to 80 DEG C, reaction 20min;
(2) by 352.5 grams of 500SN base oils and 50.6 grams of lauryl amine Hybrid Heating to 60 DEG C;
(3) two groups of solution of step (1) and step (2) are mixed, at 80 DEG C, react 20min;
(4) be warming up to 180 DEG C, constant temperature refining 25min; Add wherein 350 grams of 500SN basesOil, stirs and is cooled to 130 DEG C, adds 24.5 grams of S1, under 200rpm, stirs;
(5) grind 2 times by three-roller and become fat. Properties of product are as shown in table 2.
In the lubricating grease that the present embodiment obtains, taking lubricating grease weight as benchmark, consist of: S12 % by weight,Four carbamido thickening agent 8 % by weight, base oil 90 % by weight.
Embodiment 6
The present embodiment is used for illustrating four urea-based lubricating grease compositions of the present invention and preparation method thereof.
(1) by 80.5 grams of 150BS base oils, (100 DEG C of viscosity are 30mm2/ s, lower same) with 50.5Gram MDI Hybrid Heating to 50 DEG C, adds 6 grams of ethylenediamines, is warming up to 100 DEG C, reaction 60min;
(2) by 78 grams of 150BS base oils and 41.5 grams of lauryl amine Hybrid Heating to 50 DEG C;
(3) two groups of solution of step (1) and step (2) are mixed, at 100 DEG C, react 60min;
(4) be warming up to 210 DEG C, constant temperature refining 10min; Add wherein 78 grams of 150BS base oils,Stirring is cooled to 90 DEG C, adds 3.4 grams of S1, under 180rpm, stirs;
(5) grind 3 times by three-roller and become fat. Properties of product are as shown in table 2.
In the lubricating grease that the present embodiment obtains, taking lubricating grease weight as benchmark, consist of: S11 % by weight,Four carbamido thickening agent 29 % by weight, base oil 70 % by weight.
Embodiment 7
The present embodiment is used for illustrating four urea-based lubricating grease compositions of the present invention and preparation method thereof.
(1) by 172 grams of PAO6 synthetic hydrocarbon oils, (100 DEG C of viscosity are 5.8mm2/ s, lower same) with 36.5Gram TDI Hybrid Heating to 55 DEG C, adds 6.3 grams of ethylenediamines, is warming up to 95 DEG C, reaction 50min;
(2) by 100 grams of PAO6 synthetic hydrocarbon oils and 56.5 grams of octadecylamine Hybrid Heating to 55 DEG C;
(3) two groups of solution of step (1) and step (2) are mixed, at 90 DEG C, react 30min;
(4) be warming up to 190 DEG C, constant temperature refining 15min; Add wherein 100 grams of PAO6 to synthesize hydrocarbonOil, stirs and is cooled to 110 DEG C, adds 24.8 grams of S1, under 230rpm, stirs;
(5) grind 2 times by three-roller and become fat. Properties of product are as shown in table 2.
In the lubricating grease that the present embodiment obtains, taking lubricating grease weight as benchmark, consist of: S15 % by weight,Four carbamido thickening agent 20 % by weight, base oil 75 % by weight.
Embodiment 8
The present embodiment is used for illustrating four urea-based lubricating grease compositions of the present invention and preparation method thereof.
(1) by the miscella of 202 grams of 500SN and 150BS, (100 DEG C of viscosity are 13mm2/ s, underWith) and 45.1 grams of MDI Hybrid Heating to 60 DEG C, add 5.5 grams of ethylenediamines, be warming up to 90 DEG C, anti-Answer 30min;
(2) miscella of 180 grams of 500SN and 150BS and 48.5 grams of octadecylamine Hybrid Heating are arrived60℃；
(3) two groups of solution of step (1) and step (2) are mixed, at 85 DEG C, react 40min;
(4) be warming up to 200 DEG C, constant temperature refining 10min; Add wherein 160 grams of 500SN and 150BSMiscella, stir be cooled to 120 DEG C, add 19.8 grams of S1, under 300rpm, stir;
(5) grind 3 times by three-roller and become fat. Properties of product are as shown in table 2.
In the lubricating grease that the present embodiment obtains, taking lubricating grease weight as benchmark, consist of: S13 % by weight,Four carbamido thickening agent 15 % by weight, base oil 82 % by weight.
Comparative example 2
Prepare four urea-base greases according to the method for embodiment 8, different, do not add S1. ProductPerformance is as shown in table 2.
In the lubricating grease that this comparative example obtains, taking lubricating grease weight as benchmark, consist of: four urea groups multiviscosistyAgent 15.5 % by weight, base oil 84.5 % by weight.
Embodiment 9
The present embodiment is used for illustrating six urea-based lubricating grease compositions of the present invention and preparation method thereof.
(1) by 315 grams of 500SN base oils, (100 DEG C of viscosity are 10mm2/ s, lower same) and 42 gramsMDI Hybrid Heating to 50 DEG C;
(2) by 300 grams of 500SN base oils and 35.5 grams of lauryl amine Hybrid Heating to 50 DEG C, slowlyJoin in the system of step (1), be warming up to 80 DEG C of reaction 60min, slowly add 10 grams of ethylenediamines,80 DEG C of reaction 60min of constant temperature;
(3) by 300 grams of 500SN base oils and 20.5 grams of MDI Hybrid Heating to 50 DEG C, slowly addEnter in above-mentioned system 80 DEG C of reaction 30min of constant temperature;
(4) be warming up to 180 DEG C, constant temperature refining 20min; Add wherein 300 grams of 500SN basesOil, stirs and is cooled to 130 DEG C, adds 27 grams of S1, under 200rpm, stirs;
(5) grind 2 times by three-roller and become fat. Properties of product are as shown in table 3.
In the lubricating grease that the present embodiment obtains, taking lubricating grease weight as benchmark, consist of: S12 % by weight,Six carbamido thickening agent 8 % by weight, base oil 90 % by weight.
Embodiment 10
The present embodiment is used for illustrating six urea-based lubricating grease compositions of the present invention and preparation method thereof.
(1) by 61 grams of 150BS base oils, (100 DEG C of viscosity are 30mm2/ s, lower same) and 35 gramsTDI Hybrid Heating to 70 DEG C;
(2) by 60 grams of 150BS base oils and 43 grams of lauryl amine Hybrid Heating to 70 DEG C, slowly addIn the system of step (1), be warming up to 100 DEG C of reaction 20min, slowly add 12.2 grams of ethylenediamines,100 DEG C of reaction 20min of constant temperature;
(3) by 60 grams of 150BS base oils and 18 grams of TDI Hybrid Heating to 70 DEG C, slowly joinIn above-mentioned system, 100 DEG C of reaction 20min of constant temperature;
(4) be warming up to 210 DEG C, constant temperature refining 5min; Add wherein 60 grams of 150BS base oils,Stirring is cooled to 90 DEG C, adds 3.7 grams of S1, under 180rpm, stirs;
(5) grind 3 times by three-roller and become fat. Properties of product are as shown in table 3.
In the lubricating grease that the present embodiment obtains, taking lubricating grease weight as benchmark, consist of: S11 % by weight,Six carbamido thickening agent 29 % by weight, base oil 70 % by weight.
Embodiment 11
The present embodiment is used for illustrating six urea-based lubricating grease compositions of the present invention and preparation method thereof.
(1) by 104 grams of PAO6 synthetic hydrocarbon oils, (100 DEG C of viscosity are 5.8mm2/ s, lower same) with 40Gram MDI Hybrid Heating to 60 DEG C;
(2) by 100 grams of PAO6 synthetic hydrocarbon oils and 41 grams of octadecylamine Hybrid Heating to 60 DEG C, slowly addEnter in the system of step (1), be warming up to 95 DEG C of reaction 40min, slowly add 9.2 grams of ethylenediamines,95 DEG C of reaction 40min of constant temperature;
(3) by 100 grams of PAO6 synthetic hydrocarbon oils and 17.5 grams of MDI Hybrid Heating to 60 DEG C, slowlyJoin in above-mentioned system 95 DEG C of reaction 40min of constant temperature;
(4) be warming up to 190 DEG C, constant temperature refining 15min; Add wherein 100 grams of PAO6 to synthesize hydrocarbonOil, stirs and is cooled to 100 DEG C, adds 26.9 grams of S1, under 230rpm, stirs;
(5) grind 2 times by three-roller and become fat. Properties of product are as shown in table 3.
In the lubricating grease that the present embodiment obtains, taking lubricating grease weight as benchmark, consist of: S15 % by weight,Six carbamido thickening agent 20 % by weight, base oil 75 % by weight.
Embodiment 12
The present embodiment is used for illustrating six urea-based lubricating grease compositions of the present invention and preparation method thereof.
(1) by the miscella of 149 grams of 500SN and 150BS, (100 DEG C of viscosity are 13mm2/ s, underWith) and 32 grams of TDI Hybrid Heating to 55 DEG C;
(2) miscella of 148 grams of 500SN and 150BS and 49.5 grams of octadecylamine Hybrid Heating are arrived55 DEG C, slowly join in the system of step (1), be warming up to 90 DEG C of reaction 30min, slowly add11 grams of ethylenediamines, 90 DEG C of reaction 30min of constant temperature;
(3) by the miscella of 148 grams of 500SN and 150BS and 16 grams of TDI Hybrid Heating to 55 DEG C,Slowly join in above-mentioned system 90 DEG C of reaction 30min of constant temperature;
(4) be warming up to 200 DEG C, constant temperature refining 10min; Add wherein 148 grams of 500SN and 150BSMiscella, stir be cooled to 120 DEG C, add 21.7 grams of S1, under 300rpm, stir;
(5) grind 3 times by three-roller and become fat. Properties of product are as shown in table 3.
In the lubricating grease that the present embodiment obtains, taking lubricating grease weight as benchmark, consist of: S13 % by weight,Six carbamido thickening agent 15 % by weight, base oil 82 % by weight.
Comparative example 3
Prepare six urea-base greases according to the method for embodiment 12, different, do not add S1. ProductPerformance is as shown in table 3.
In the lubricating grease that this comparative example obtains, taking lubricating grease weight as benchmark, consist of: six urea groups multiviscosistyAgent 15.5 % by weight, base oil 84.5 % by weight.
Embodiment 13
The present embodiment is used for illustrating eight urea-based lubricating grease compositions of the present invention and preparation method thereof.
(1) by 450 grams of 500SN base oils, (100 DEG C of viscosity are 10mm2/ s, lower same) with 62.5Gram TDI Hybrid Heating to 50 DEG C, adds 11 grams of ethylenediamines, is warming up to 80 DEG C, react 60 minutes withAfter, then adding 5 grams of ethylenediamines, 80 DEG C of constant temperature, react 60 minutes;
(2) by 450 grams of 500SN base oils and 38 grams of lauryl amine Hybrid Heating to 50 DEG C, joinIn the reacted system of step (1), 80 DEG C of constant temperature, react 60 minutes;
(3) be warming up to 210 DEG C, keep 5 minutes, then add 410.5 grams of 500SN base oils, stirMix and be cooled to 130 DEG C, add 29.1 grams of S1, under 200rpm, stir;
(4) grind 3 times by three-roller and become fat. Properties of product are as shown in table 4.
In the lubricating grease that the present embodiment obtains, taking lubricating grease weight as benchmark, consist of: S12 % by weight,Eight carbamido thickening agent 8 % by weight, base oil 90 % by weight.
Embodiment 14
The present embodiment is used for illustrating eight urea-based lubricating grease compositions of the present invention and preparation method thereof.
(1) by 102.5 grams of 150BS base oils, (100 DEG C of viscosity are 30mm2/ s, lower same) with 68Gram MDI Hybrid Heating to 70 DEG C, adds 8 grams of ethylenediamines, is warming up to 100 DEG C, react 20 minutes withAfter, then adding 4.5g ethylenediamine, 100 DEG C of constant temperature, react 20 minutes;
(2) by 90 grams of 150BS base oils and 36.5 grams of octadecylamine Hybrid Heating to 70 DEG C, joinIn the reacted system of step (1), 100 DEG C of constant temperature, react 20 minutes;
(3) be warming up to 180 DEG C, keep 20 minutes, then add 90 grams of 150BS base oils, stirBe cooled to 90 DEG C, add 4.8 grams of S1, under 300rpm, stir;
(4) grind 2 times by three-roller and become fat. Properties of product are as shown in table 4.
In the lubricating grease that the present embodiment obtains, taking lubricating grease weight as benchmark, consist of: S11 % by weight,Eight carbamido thickening agent 29 % by weight, base oil 70 % by weight.
Embodiment 15
The present embodiment is used for illustrating eight urea-based lubricating grease compositions of the present invention and preparation method thereof.
(1) by 148.5 grams of PAO6 synthetic hydrocarbon oils, (100 DEG C of viscosity are 10mm2/ s, lower same) with 73Gram MDI Hybrid Heating to 55 DEG C, adds 9 grams of ethylenediamines, is warming up to 90 DEG C, react 40 minutes withAfter, then adding 4 grams of ethylenediamines, 90 DEG C of constant temperature, react 40 minutes;
(2) by 145 grams of PAO6 synthetic hydrocarbon oils and 31 grams of lauryl amine Hybrid Heating to 55 DEG C, joinIn the reacted system of step (1), 90 DEG C of constant temperature, react 40 minutes;
(3) be warming up to 190 DEG C, keep 15 minutes, then add 145 grams of PAO6 synthetic hydrocarbon oils, stirMix and be cooled to 110 DEG C, add 29.3 grams of S1, under 180rpm, stir;
(4) grind 3 times by three-roller and become fat. Properties of product are as shown in table 4.
In the lubricating grease that the present embodiment obtains, taking lubricating grease weight as benchmark, consist of: S15 % by weight,Eight carbamido thickening agent 20 % by weight, base oil 75 % by weight.
Embodiment 16
The present embodiment is used for illustrating eight urea-based lubricating grease compositions of the present invention and preparation method thereof.
(1) by the miscella of 242 grams of 500SN and 150BS, (100 DEG C of viscosity are 13mm2/ s, underWith) and 58 grams of TDI Hybrid Heating to 60 DEG C, add 10 grams of ethylenediamines, be warming up to 95 DEG C, reactionAfter 30 minutes, then add 5 grams of ethylenediamines, 95 DEG C of constant temperature, react 30 minutes;
(2) miscella of 200 grams of 500SN and 150BS and 44.5 grams of octadecylamine Hybrid Heating are arrived60 DEG C, join in the reacted system of step (1), 95 DEG C of constant temperature, react 30 minutes;
(3) be warming up to 200 DEG C, keep 10 minutes, then add mixing of 200 grams of 500SN and 150BSClose oil, stir and be cooled to 100 DEG C, add 23.5 grams of S1, under 230rpm, stir;
(4) grind 2 times by three-roller and become fat. Properties of product are as shown in table 4.
In the lubricating grease that the present embodiment obtains, taking lubricating grease weight as benchmark, consist of: S13 % by weight,Eight carbamido thickening agent 15 % by weight, base oil 82 % by weight.
Comparative example 4
Prepare eight urea-base greases according to the method for embodiment 16, different, do not add S1. ProductPerformance is as shown in table 4.
In the lubricating grease that this comparative example obtains, taking lubricating grease weight as benchmark, consist of: eight urea groups multiviscosistyAgent 15.5 % by weight, base oil 84.5 % by weight.
Table 1
Table 2
Table 3
Table 4
It will be understood by those skilled in the art that dropping point is higher, the high-temperature behavior of lubricating grease is better; WorkMake cone penetration less, the multiviscosisty performance of grease thickener is better; Extend Drawing cone in-degree less, lubricatedThe mechanical stability of fat is better; Oxidation initial temperature is higher, and the antioxygenic property of lubricating grease is better; Steel meshDivide oil value less, the colloid stability of lubricating grease is better; Water pouring number of dropouts is less, the water proofing property of lubricating greaseCan be better; PB, PD value are larger, and the bearing capacity of lubricating grease is better; Coefficient of friction is less, lubricating greaseAntifriction performance better.
Respectively embodiment 4 is compared with comparative example 1, embodiment 8 is compared with comparative example 2,Embodiment 12 is compared with comparative example 3, embodiment 16 is compared with comparative example 4, canFind out, lubricating grease of the present invention has better high-temperature behavior, mechanical stability, non-oxidizability, colloidStability, water proofing property, bearing capacity and antifriction performance.
Urea-based lubricating grease composition of the present invention, owing to containing multipurpose additive, has greatly improved lubricatedAnti-attrition ability and the oxidation resistance of fat. Lubricating grease of the present invention has splendid high-temperature behavior, machinery peaceQualitative, non-oxidizability, colloid stability, water proofing property, bearing capacity and antifriction performance etc., can be competent atIn high temperature, at a high speed, the harsh working condition such as high load capacity, many water.
Below describe by reference to the accompanying drawings the preferred embodiment of the present invention in detail, still, the present invention does not limitDetail in above-mentioned embodiment, within the scope of technical conceive of the present invention, can be to the present inventionTechnical scheme carry out multiple simple variant, these simple variant all belong to protection scope of the present invention.
It should be noted that in addition each the concrete technology spy described in above-mentioned detailed description of the inventionLevy, in reconcilable situation, can combine by any suitable mode, for fear of needn'tThe repetition of wanting, the present invention is to the explanation no longer separately of various possible combinations.
In addition, between various embodiment of the present invention, also can be combined, as long as itsWithout prejudice to thought of the present invention, it should be considered as content disclosed in this invention equally.
Claims (14)
1. a urea-based lubricating grease composition for Wear vesistance excellence, taking the weight of lubricant composition asBenchmark, described lubricant composition comprises following component: the lubricating base oil of 65-95 % by weight, 5-35The additive of the carbamido thickening agent of % by weight and 0.1-15 % by weight, is characterized in that, described additive containsThere is the compound of structure shown in formula (I):
2. lubricant composition according to claim 1, wherein, with the weight of lubricant compositionAmount is for benchmark, and described lubricant composition comprises following component: the lubricating base oil of 70-90 % by weight,The additive of the carbamido thickening agent of 8-30 % by weight and 0.5-10 % by weight.
3. lubricant composition according to claim 1 and 2, wherein, with lubricant compositionWeight be benchmark, shown in formula (I), the content of the compound of structure is 0.1-10 % by weight.
4. lubricant composition according to claim 3, wherein, with the weight of lubricant compositionAmount is benchmark, and shown in formula (I), the content of the compound of structure is 1-5 % by weight.
5. lubricant composition according to claim 1 and 2, wherein, described lubricating base oilFor at least one in mineral oil, vegetable oil and artificial oil.
6. lubricant composition according to claim 1 and 2, wherein, described carbamido thickening agentFor the product of amine and vulcabond, described carbamido thickening agent is that two carbamido thickening agents, four urea groups are thickAt least one in agent, six carbamido thickening agents and eight carbamido thickening agents.
7. lubricant composition according to claim 1 and 2, wherein, described additive also containsThere is at least one in other antioxidant, extreme pressure anti-wear additives and antirust agent.
8. lubricant composition according to claim 7, wherein, described antioxidant is arylamine classAntioxidant, is preferably at least one in diphenylamines, PA and di-iso-octyldiphenylamine, more excellentElect di-iso-octyldiphenylamine as.
9. lubricant composition according to claim 7, wherein, described extreme pressure anti-wear additives is twoSulfo-Acidic phosphates zinc, two sulfo-dialkyl amido formic acid molybdenums, two sulfo-dialkyl amido lead formates,Molybdenum bisuphide, polytetrafluoroethylene (PTFE), dibutyl dithiocaarbamate antimony, tungsten disulfide, selenium disulfide,At least one in fluorographite, calcium carbonate and zinc oxide.
10. lubricant composition according to claim 7, wherein, described antirust agent is oil sulphurIn acid barium, petroleum sodium sulfonate, benzothiazole, BTA, zinc naphthenate and alkenyl succinic acid extremelyFew a kind of.
The preparation method of the urea-based lubricating grease composition of 11. 1 kinds of Wear vesistance excellences, described method comprises:
(1) part lubricating base oil, vulcabond, amine hybrid reaction are generated to carbamido thickening agent;
(2) step (1) reaction gained system is warming up to 180-210 DEG C, keeps 5-25min, then addEnter to remain lubricating base oil, stir and be cooled to 90-130 DEG C, add additive, mix;
(3) grind 2-3 time by three-roller;
Wherein, taking the weight of lubricant composition as benchmark, the consumption of lubricating base oil is that 65-95 is heavyThe consumption of the carbamido thickening agent of measure %, being prepared by vulcabond, amine is 5-35 % by weight, additiveConsumption is 0.1-15 % by weight, it is characterized in that, the chemical combination that described additive contains structure shown in formula (I)Thing:
12. methods according to claim 11, wherein, taking the weight of lubricant composition as baseStandard, the urea groups multiviscosisty that the consumption of lubricating base oil is 70-90 % by weight, prepared by vulcabond, amineThe consumption of agent is 8-30 % by weight, and the consumption of additive is 0.5-10 % by weight.
13. according to the method described in claim 11 or 12, wherein, and with the weight of lubricant compositionFor benchmark, shown in formula (I), the consumption of the compound of structure is 0.1-10 % by weight.
14. methods according to claim 13, wherein, taking the weight of lubricant composition as baseStandard, shown in formula (I), the consumption of the compound of structure is 1-5 % by weight.
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| CN110408457A (en) * | 2019-07-19 | 2019-11-05 | 中国科学院兰州化学物理研究所 | A kind of preparation method of poly- four urea grease |
| CN110499202A (en) * | 2018-05-18 | 2019-11-26 | 天津科技大学 | A kind of preparation method of polyurea grease thickening agent powder |
| CN112521997A (en) * | 2019-09-17 | 2021-03-19 | 中国石油化工股份有限公司 | Lubricating grease composition for metallurgical sintering machine and preparation method thereof |
| CN115960650A (en) * | 2021-10-12 | 2023-04-14 | 中国石油化工股份有限公司 | Lubricating oil composition for air compressor and preparation method thereof |
| CN115960649A (en) * | 2021-10-11 | 2023-04-14 | 中国石油化工股份有限公司 | Lubricating grease and preparation method thereof |
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| CN110408457A (en) * | 2019-07-19 | 2019-11-05 | 中国科学院兰州化学物理研究所 | A kind of preparation method of poly- four urea grease |
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