CN106032477B - Lubricant composition and preparation method thereof - Google Patents

Lubricant composition and preparation method thereof Download PDF

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CN106032477B
CN106032477B CN201510105336.9A CN201510105336A CN106032477B CN 106032477 B CN106032477 B CN 106032477B CN 201510105336 A CN201510105336 A CN 201510105336A CN 106032477 B CN106032477 B CN 106032477B
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calcium
newtonian fluid
weight
content
added
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CN106032477A (en
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何懿峰
孙洪伟
段庆华
张建荣
郑会
刘中其
姜靓
陈政
孔锡奎
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Sinopec Research Institute of Petroleum Processing
China Petroleum and Chemical Corp
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Sinopec Research Institute of Petroleum Processing
China Petroleum and Chemical Corp
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Abstract

Lubricant composition and preparation method thereof.The present invention relates to lubricating grease fields, disclose a kind of lubricant composition, the lubricant composition contains base oil and thickening agent, the thickening agent contains non-newtonian fluid sulfurized alkylphenol calcium-sulfoacid calcium and polyurea compound, the thickening agent also optionally contains one of non-newtonian fluid calcium naphthenate, non-newtonian fluid calcium salicylate and non-newtonian fluid calcium oleate or a variety of, on the basis of lubricating grease weight, non-newtonian fluid sulfurized alkylphenol calcium-sulfoacid calcium content is 10-70 weight %；The content of non-newtonian fluid calcium naphthenate is 0-70 weight %；The content of non-newtonian fluid calcium salicylate is 0-70 weight %；The content of non-newtonian fluid calcium oleate is 0-70 weight %；The content of polyurea compound is 0.5-30 weight %；The content of base oil is 10-80 weight %.Also disclose the preparation method of lubricant composition.Lubricant composition of the invention has excellent performance, and preparation process is simple and environmentally-friendly, stable product quality.

Description

Lubricant composition and preparation method thereof
Technical field
The present invention relates to a kind of lubricant compositions and preparation method thereof.
Background technique
SULFURIZED CALCIUM ALKYL PHENATE WITH HIGH BASE NUMBER has preferable detergent-dispersant performance, good acid neutralization capacity and excellent diffusion Property, it is used as the detersive of lubricating oil, is widely used in modulation medium and high classes I. C. engine oil, is particularly suitable for supercharged diesel engine For oil to reduce the carbon deposit of top land and the additive of marine cylinder oil, technology development mainly makes its height alkalization, be exactly Calcium carbonate, which is distributed in flux oil with the sulfurized alkylphenol calcium with surface-active, becomes a kind of colloidal dispersion system.High base number Sulfurized alkylphenol calcium is that alkyl phenol is reacted with CaO, vulcanized, carbonated contour alkalization technology and obtain, and the correlation in relation to preparation is specially Benefit has CN101423483 etc..
It is that raw material produces lubricating grease using calcium sulfonate with high base number, because it is with excellent antirust and anticorrosive property, from investment Since market, the extensive concern of domestic and international lubricating grease industry is caused, however, although high base number composite calcium sulfonate base grease has Very excellent antirust and anticorrosive property, but hardening is easy in storage process, and its raw materials for production calcium sulfonate with high base number is high Price and complicated preparation process itself cause it not promoted rapidly, meanwhile, the requirement with people to environmental protection is got over Come higher, necessary sulfonation process is also increasingly subject to the concern of people to the pollution of environment in calcium sulfonate with high base number production process. It finds a kind of antirust and anticorrosive property is similar with high base number composite calcium sulfonate base grease but can reduce the lubrication of the above problem Rouge becomes the big problem that people face at present.
Summary of the invention
The object of the present invention is to provide one kind to have good antirust and anticorrosive property, storage good security and its raw material system Standby simple process, lubricating grease of environmental protection and preparation method thereof.
The present inventor has found that sulfurized alkylphenol calcium may hold at high temperature due to containing active sulfur under study for action Elemental sulfur easily is precipitated and generates corrosion, therefore, when as detersive, the antirust and anticorrosive property of sulfurized alkylphenol calcium are far below Sulfoacid calcium, but when sulfurized alkylphenol calcium is prepared lubricating grease as thickening agent, but it can get and sulfonate with high base number calcium-base grease Quite even preferably antirust and anticorrosive property, and storage good security.
Therefore, to achieve the goals above, on the one hand, the present invention provides a kind of lubricant composition, the lubricating grease Composition contains base oil and thickening agent, and the thickening agent contains non-newtonian fluid sulfurized alkylphenol calcium-sulfoacid calcium and polyureas chemical combination Object, the thickening agent is also optionally containing in non-newtonian fluid calcium naphthenate, non-newtonian fluid calcium salicylate and non-newtonian fluid calcium oleate It is one or more, on the basis of the weight of lubricant composition, non-newtonian fluid sulfurized alkylphenol calcium-sulfoacid calcium content is 10-70 weight %；The content of non-newtonian fluid calcium naphthenate is 0-70 weight %；The content of non-newtonian fluid calcium salicylate is 0-70 weight Measure %；The content of non-newtonian fluid calcium oleate is 0-70 weight %；The content of polyurea compound is 0.5-30 weight %；Base oil Content is 10-80 weight %.
Preferably, on the basis of the weight of lubricant composition, non-newtonian fluid sulfurized alkylphenol calcium-sulfoacid calcium content For 20-65 weight %；The content of non-newtonian fluid calcium naphthenate is 0-50 weight %；The content of non-newtonian fluid calcium salicylate is 0-50 Weight %；The content of non-newtonian fluid calcium oleate is 0-50 weight %；The content of polyurea compound is 1-20 weight %；Base oil Content is 20-70 weight %.
Second aspect, the present invention provides the preparation methods of lubricant composition as described above, this method comprises: by thick Agent and part basis oil are uniformly mixed, and refine in 180-230 DEG C of constant temperature, surplus base oil is added, necessary additive is added, Finished product is obtained, the thickening agent contains non-newtonian fluid sulfurized alkylphenol calcium-sulfoacid calcium and polyurea compound, and the thickening agent is also Optionally contain one of non-newtonian fluid calcium naphthenate, non-newtonian fluid calcium salicylate and non-newtonian fluid calcium oleate or a variety of.
The third aspect, the present invention provides a kind of preparation methods of lubricant composition, this method comprises:
(1) will contain newton body sulfurized alkylphenol calcium, newton body and/or non-newtonian fluid sulfoacid calcium, or containing newton body and/ Or non-newtonian fluid sulfurized alkylphenol calcium, the high base number material of newton body sulfoacid calcium and the mixing of part basis oil, mixture is obtained, The high base number material also optionally contains newton body and/or non-newtonian fluid calcium naphthenate, newton body and/or non-newtonian fluid bigcatkin willow Sour calcium and one of newton body and/or non-newtonian fluid calcium oleate or a variety of；
(2) it optionally carries out the reaction of at least partly polyurea compound: part basis oil and monoamine is added, or is additionally added two Amine is added diisocyanate and is reacted；
(3) transforming agent is added, heats up to material retrogradation, further heats up dehydration；
(4) reaction of remaining polyurea compound is carried out；
(5) 180-230 DEG C of constant temperature refinings are warming up to, surplus base oil is added, necessary additive is added, obtains finished product.
Preferably, in step (2), the reaction of at least partly polyurea compound is carried out.
Fourth aspect, the present invention provides the lubricant compositions as made from method as described above.
Lubricant composition of the invention with the antirust quite even more excellent with sulfoacid calcium base polyurea grease and is prevented Corrosivity, and there is excellent storage stability, also have the viscous resistance better than sulfoacid calcium base polyurea grease, machinery stable Property, water-resistance, colloid stability, abrasion resistance, extreme pressure anti-wear and bearing lubrication service life, and also there is excellent heat-resisting quantity Etc. performances.The feed preparation process of lubricating grease of the invention is simple and environmentally-friendly, stable product quality.
Other features and advantages of the present invention will the following detailed description will be given in the detailed implementation section.
Specific embodiment
Detailed description of the preferred embodiments below.It should be understood that described herein specific Embodiment is merely to illustrate and explain the present invention, and is not intended to restrict the invention.
The present invention provides a kind of lubricant composition, this lubricant composition uses calcium mahogany sulfonate and/or conjunction At sulfoacid calcium, synthesis sulfurized alkylphenol calcium, optional petroleum naphthenic acid calcium and/or synthesis calcium naphthenate, optional synthesis bigcatkin willow Sour calcium, optional natural calcium oleate and/or synthesis calcium oleate are raw material, the polyureas generated simultaneously containing isocyanates and amine reaction Compound.
The present invention also provides the preparation methods of foregoing grease composition.
On the one hand, the present invention provides a kind of lubricant composition, lubricant composition contains base oil and thickening agent, thick Agent contains non-newtonian fluid sulfurized alkylphenol calcium-sulfoacid calcium and polyurea compound, and thickening agent also optionally contains non-newtonian fluid ring One of alkanoic acid calcium, non-newtonian fluid calcium salicylate and non-newtonian fluid calcium oleate are a variety of, are with the weight of lubricant composition Benchmark, non-newtonian fluid sulfurized alkylphenol calcium-sulfoacid calcium content are 10-70 weight %；The content of non-newtonian fluid calcium naphthenate is 0-70 weight %；The content of non-newtonian fluid calcium salicylate is 0-70 weight %；The content of non-newtonian fluid calcium oleate is 0-70 weight Measure %；The content of polyurea compound is 0.5-30 weight %；The content of base oil is 10-80 weight %.
Preferably, on the basis of the weight of lubricant composition, non-newtonian fluid sulfurized alkylphenol calcium-sulfoacid calcium content For 20-65 weight %；The content of non-newtonian fluid calcium naphthenate is 0-50 weight %；The content of non-newtonian fluid calcium salicylate is 0-50 Weight %；The content of non-newtonian fluid calcium oleate is 0-50 weight %；The content of polyurea compound is 1-20 weight %；Base oil Content is 20-70 weight %.
In the present invention, " optionally containing " refers to can be containing the component or without containing the component, that is, non-newtonian fluid One of calcium naphthenate, non-newtonian fluid calcium salicylate and non-newtonian fluid calcium oleate or it is a variety of be optional component, profit of the invention It may include the component in grease composition, can not also include the component.
Non-newtonian fluid sulfurized alkylphenol calcium-sulfoacid calcium, non-newtonian fluid calcium naphthenate, non-newtonian fluid calcium salicylate, non newtonian Body calcium oleate or combinations thereof object is in infrared spectrum 873cm–1–886cm–1There is crystal form calcium carbonate characteristic absorption peak in place.Non-newtonian fluid Sulfurized alkylphenol calcium-sulfoacid calcium is to convert to obtain by transforming agent by newton body sulfoacid calcium and newton body sulfurized alkylphenol calcium, non- Newton body sulfurized alkylphenol calcium-sulfoacid calcium total base number is 250-450mgKOH/g, preferably 300-400mgKOH/g；Non- ox The body calcium naphthenate that pauses is converted by newton body calcium naphthenate, and the total base number of non-newtonian fluid calcium naphthenate is 250- 450mgKOH/g, preferably 300-400mgKOH/g；Non-newtonian fluid calcium salicylate is converted by newton body calcium salicylate, The total base number of non-newtonian fluid calcium salicylate is 250-450mgKOH/g, preferably 300-400mgKOH/g；Non-newtonian fluid calcium oleate It is to be converted by newton body calcium oleate, the total base number of non-newtonian fluid calcium oleate is 250-450mgKOH/g, preferably 300- 400mgKOH/g.And newton body sulfoacid calcium, newton body sulfurized alkylphenol calcium, newton body calcium naphthenate, newton body calcium salicylate, ox Contain unformed calcium carbonate in body calcium oleate, in infrared spectrum 860cm–1–865cm–1There is unformed calcium carbonate feature and inhales in place Receive peak.Newton body sulfurized alkylphenol calcium is synthesis sulfurized alkylphenol calcium, total base number 250-450mgKOH/g, preferably 300- 400mgKOH/g；Newton body sulfoacid calcium is calcium mahogany sulfonate and/or calcium alkylbenzenesulfonate, total base number 250-450mgKOH/g, Preferably 300-400mgKOH/g；Newton body calcium naphthenate is petroleum naphthenic acid calcium and/or synthesis calcium naphthenate, total base number are 250-450mgKOH/g, preferably 300-400mgKOH/g；Newton body calcium salicylate is salicylate calcium, and total base number is 250-450mgKOH/g, preferably 300-400mgKOH/g；Newton body calcium oleate be natural calcium oleate and/or synthesis calcium oleate, Its total base number is 250-450mgKOH/g, preferably 300-400mgKOH/g.It is non-newtonian fluid sulfurized alkylphenol calcium-sulfoacid calcium, non- The base number of newton body calcium naphthenate, non-newtonian fluid calcium salicylate and the mixing of non-newtonian fluid calcium oleate is the weight of the base number of each component Weighted average.
In the present invention, polyurea compound can be polyurea compound commonly used in the art, for example, polyureas without particular/special requirement The structural formula of compound can be
Wherein, n is preferably 0-3 integer.
Wherein, R1、R4It can be the same or different, can be alkyl, naphthenic base or aryl, the carbon of alkyl or cycloalkyl Number can be 8-24, preferably 10-18, and aryl can be phenyl or substituted phenyl, preferably the alkyl of phenyl or C1-C3 or The phenyl that halogen replaces.
Wherein, R2It can be alkylidene or arlydene, the carbon number of alkylidene can be 2-12, preferably 2-8, and arlydene can To be phenylene or biphenylene.
Wherein, R3It can be arlydene, alkylidene or cycloalkylidene, the carbon number of arlydene, alkylidene or cycloalkylidene can Think 6-30, preferably 6-20, R3More preferably WithIn At least one.
In the present invention, single polyureas can be used, mixing polyureas also can be used, for example, polyurea compound can be two At least one of polyurea compound, four polyurea compounds, six polyurea compounds and eight polyurea compounds.
Above-mentioned polyurea compound can be obtained using the thinkable various methods of those skilled in the art institute, such as can be by The method preparation recorded according to CN103060069A, CN103060070A, CN103060068A, CN103060067A, US3243372 It obtains.
The lubricating base oil can be mineral oil, synthetic oil, vegetable oil or their mixture, 100 DEG C of dynamic viscosities For 4-150mm2/ s, preferably 10-60mm2/s.Synthetic oil can be poly-a-olefin oil (PAO), Esters oil, alkyl-silicone oil, Fischer-Tropsch Synthetic oil etc..
Various additives can also be contained in lubricant composition of the invention, such as antioxidant, extreme pressure anti-wear additives, antirust agent Etc..Wherein, the preferred arylamine kind antioxidant of antioxidant, accounts for the 0.01-5% of lubricating grease total weight, preferably 0.1-2.5%, can be with It is diphenylamines, phenyl-α-at least one of naphthylamines and di-iso-octyldiphenylamine, preferably di-iso-octyldiphenylamine.Extreme-pressure anti-wear Agent accounts for the 0.5-12% of lubricating grease total weight, preferably 0.8-8%, can be two thio Acidic phosphates zinc, two thio dialkyl group Carbamic acid molybdenum, two thio dialkyl amido lead formates, triphenylphosphorothionate, organic molybdenum complex compound, olefine sulfide, two sulphur Change molybdenum, polytetrafluoroethylene (PTFE), thiophosphoric acid molybdenum, chlorinated paraffin, dibutyl dithiocaarbamate antimony, tungsten disulfide, selenium disulfide, At least one of fluorographite, calcium carbonate and zinc oxide；Antirust agent accounts for the 0.01-4.5% of lubricating grease total weight, preferably 0.1- 2%, it can be in barium mahogany sulfonate, petroleum sodium sulfonate, benzothiazole, benzotriazole, zinc naphthenate and alkenyl succinic acid It is at least one.
Second aspect, the present invention provides the preparation methods of lubricant composition as described above, this method comprises: by thick Agent and part basis oil are uniformly mixed, and refine in 180-230 DEG C of constant temperature, surplus base oil is added, necessary additive is added, Finished product is obtained, the thickening agent contains non-newtonian fluid sulfurized alkylphenol calcium-sulfoacid calcium and polyurea compound, and the thickening agent is also Optionally contain one of non-newtonian fluid calcium naphthenate, non-newtonian fluid calcium salicylate and non-newtonian fluid calcium oleate or a variety of.
In the present invention, " optionally containing " is as previously mentioned, details are not described herein.
In the present invention, for non-newtonian fluid sulfurized alkylphenol calcium-sulfoacid calcium, non-newtonian fluid calcium naphthenate, non-newtonian fluid water Poplar acid calcium, non-newtonian fluid calcium oleate, polyurea compound, base oil and additive are as described above, details are not described herein.
It will be understood by those skilled in the art that the sum of the amount of part basis oil and the amount of surplus base oil are used Base oil total amount, in the present invention, the weight ratio of part basis oil and surplus base oil is preferably 1:0.1-5.
For non-newtonian fluid sulfurized alkylphenol calcium-sulfoacid calcium, non-newtonian fluid calcium naphthenate, non-newtonian fluid calcium salicylate, non- Newton body calcium oleate or combinations thereof object, can by newton body sulfoacid calcium, newton body sulfurized alkylphenol calcium, newton body calcium naphthenate, Non-newtonian fluid calcium salicylate, non-newtonian fluid calcium oleate or combinations thereof object pass through transforming agent respectively and convert to obtain, for example, by newton body Sulfoacid calcium, newton body sulfurized alkylphenol calcium, optional newton body calcium naphthenate, optional newton body calcium salicylate, optional ox Body calcium oleate and base oil Hybrid Heating are added required transforming agent and are reacted, all transforming agents add to 50-80 DEG C Afterwards, 80-100 DEG C constant temperature 60-90 minutes, then heat to 110-130 DEG C of dehydrations.
In the present invention, " optional " refer to can there is the raw material or no raw material, for example, " optional newton body Calcium naphthenate ", which refers to, can this raw material of newton body calcium naphthenate, can also not have this raw material of newton body calcium naphthenate.
The third aspect, the present invention provides a kind of preparation methods of lubricant composition, this method comprises:
(1) will contain newton body sulfurized alkylphenol calcium, newton body and/or non-newtonian fluid sulfoacid calcium, or containing newton body and/ Or non-newtonian fluid sulfurized alkylphenol calcium, the high base number material of newton body sulfoacid calcium and the mixing of part basis oil, mixture is obtained, The high base number material also optionally contains newton body and/or non-newtonian fluid calcium naphthenate, newton body and/or non-newtonian fluid bigcatkin willow Sour calcium and one of newton body and/or non-newtonian fluid calcium oleate or a variety of；
(2) it optionally carries out the reaction of at least partly polyurea compound: part basis oil and monoamine is added, or is additionally added two Amine is added diisocyanate and is reacted；
(3) transforming agent is added, heats up to material retrogradation, further heats up dehydration；
(4) reaction of remaining polyurea compound is carried out；
(5) 180-230 DEG C of constant temperature refinings are warming up to, surplus base oil is added, necessary additive is added, obtains finished product.
" optionally containing " is as previously mentioned, details are not described herein.
In the present invention, newton body sulfurized alkylphenol calcium, non-newtonian fluid sulfurized alkylphenol calcium, newton body sulfoacid calcium, non newtonian Body sulfoacid calcium, newton body calcium naphthenate, non-newtonian fluid calcium naphthenate, newton body calcium salicylate, non-newtonian fluid calcium salicylate, newton Body calcium oleate, non-newtonian fluid calcium oleate, base oil are as previously mentioned, details are not described herein.
In step (1) of the present invention, " containing newton body sulfurized alkylphenol calcium, newton body and/or non-newtonian fluid sulfoacid calcium, or High base number material containing newton body and/or non-newtonian fluid sulfurized alkylphenol calcium, newton body sulfoacid calcium " refers to high base number material In sulfurized alkylphenol calcium and at least one of sulfoacid calcium be newton figure.
In step (1) of the present invention, for sulfoacid calcium and sulfurized alkylphenol calcium weight ratio without particular/special requirement, preferably 1: 0.25–4.For other optional high base number materials amount without particular/special requirement, can be according to actual needs using commonly used in the art Amount, the total weight of high base number material and the weight ratio of part basis oil are preferably 1:0.1-3.
In step (2) of the present invention, " optionally carrying out the reaction of at least partly polyurea compound " includes three kinds of situations: (i) without the reaction of polyurea compound, that is, do not have step (2), whole polyurea compounds is only carried out in step (4) Reaction, is converted that is, transforming agent is first added in the method for the present invention, carries out the reaction of polyurea compound after conversion again；(ii) The reaction of part polyurea compound is carried out, i.e., carries out the reaction of part polyurea compound in step (2), in step (4) again The reaction of remaining polyurea compound is carried out, that is, the method for the present invention carries out the reaction of part polyurea compound before conversion, Carry out the reaction of part polyurea compound again in post-conversion；(iii) reaction for carrying out whole polyurea compounds, i.e., in step (2) The middle reaction for carrying out whole polyurea compounds, without step (4), that is, the method for the present invention first carries out polyurea compound Reaction, then converted.
This field is generally transforming agent to be first added to be converted, then carry out polyurea compound when preparing lubricating grease Reaction, when such as preparing sulfoacid calcium base polyurea grease.But the present inventor has found under study for action, according to above situation (ii) Or (iii) carries out method of the invention, than carrying out method of the invention according to situation (i), i.e., first carries out all or part of poly- Carbamide compound reaction, then converted, it can further improve the performance of lubricating grease obtained.This may be due to first carrying out The reaction of polyurea compound can preferably vulcanize the non-newtonian fluid that the newton body sulfurized alkylphenol calcium of oily is converted into smectic Alkyl phenol calcium.It is therefore preferred that carrying out the reaction of at least partly polyurea compound in step (2).
When carrying out step (2) and step (4), single polyureas can be prepared, mixing polyureas can also be prepared.Prepare polyureas The method of compound can use those skilled in the art's commonly various methods without particular/special requirement, such as can be using as above The method that described CN103060069A, CN103060070A, CN103060068A, CN103060067A, the US3243372 is recorded Preparation.Preferably, in step (2) and step (4), after part basis oil, monoamine, optional diamines, diisocyanate is added, 100-120 DEG C constant temperature 10-30 minutes, wherein monoamine, optional diamines, diisocyanate the amount of substance meet following relationship: Amount × 2 of amount+diamines substance of the amount of the substance of diisocyanate × 2=monoamine substance, or, diisocyanate is excessive, Excessive amount≤10%.
The structure of the diisocyanate is OCN-R3- NCO, R3Can be carbon number is 6-30, preferably 6-20 arlydene, Alkylidene or cycloalkylidene, preferably Deng. For example, the diisocyanate can be toluene di-isocyanate(TDI) (TDI), methyl diphenylene diisocyanate (MDI), six it is sub- oneself In group diisocyanate (HDI), dicyclohexyl methyl hydride diisocyanate (HMDI) and xylylene diisocyanate (XDI) etc. At least one.
The monoamine can be fatty amine, aliphatic cyclic amine or arylamine, structural formula R1–NH2、R4–NH2, R therein1、R4It can be with It is alkyl, naphthenic base or aryl, the carbon number of alkyl or cycloalkyl can be 8-24, preferably 10-18, and aryl can be phenyl or take The phenyl that the phenyl in generation, preferably phenyl or C1-C3 alkyl or halogen replace.Preferred monoamine can be selected from aniline, chlorobenzene The arylamine of amine, parachloroanilinum and/or para-totuidine, and/or selected from lauryl amine, tetradecy lamine, cetylamine, octadecylamine fatty amine.
The diamines can be fatty amine or arylamine, structural formula NH2–R2–NH2, wherein R2It can be alkylidene or Asia Aryl, the carbon number of alkylidene can be 2-12, preferably 2-8, and arlydene can be phenylene or biphenylene.Preferred diamines can Be selected from p-phenylenediamine, o-phenylenediamine, 4,4 '-benzidines aromatic amine and/or selected from ethylenediamine, propane diamine, 1,6-oneself The straight-chain fatty amine of diamines.
In step (3) of the present invention, it is preferable that at 50-80 DEG C, required transforming agent is added in preferred constant temperature 10-30 minutes It is reacted, is stirred 8-12 minutes after preferably adding every kind of transforming agent, after all transforming agents add, in 80-100 DEG C of constant temperature 60- 90 minutes, then heat to 110-130 DEG C of dehydrations.
Transforming agent be preferably selected from fatty alcohol, fatty acid, aliphatic ketone, fatty aldehyde, fatty amine, ether, calcium carbonate, boric acid, phosphonic acids, In carbon dioxide, phenol, aromatic alcohol, aromatic amine, aphthenic acids, C8-C20 alkyl benzene sulphonate, C16-C24 alkyl phenol and water at least It is a kind of；It is more preferably selected from the fatty alcohol of C1-C5, the fatty acid of C1-C5, the aliphatic ketone of C1-C5, the fatty aldehyde of C1-C5, C1-C5 Fatty amine, the ether of C1-C5, boric acid, the alkyl phosphonic acid of C1-C10, the di alkyl phosphonic acid of C2-C16, C6-C20 arylphosphonic acid, The diaryl phosphonic acids of C12-C24, the aromatic alcohol of C7-C20, the aromatic amine of C7-C20, C8-C20 alkyl benzene sulphonate, C16-C22 alkane At least one of base phenol and water；Still more preferably selected from dodecyl benzene sulfonic acid, aphthenic acids, octadecyl phenol, methanol, different At least one of propyl alcohol, butanol, boric acid, acetic acid and water.The additional amount of transforming agent is preferably the 2-of high base number material total weight 30%, more preferably the 6-22% of high base number material total weight.
In the present invention, fatty alcohol includes straight chain, branch and cricoid fatty alcohol, fatty acid, aliphatic ketone, fatty aldehyde, fat Amine is similarly.
In step (5) of the present invention, it is preferable that be warming up to 180-230 DEG C of constant temperature 5-30 minutes；Surplus base oil is added, to Temperature is cooled to 100-120 DEG C, and necessary additive is added, stirring, circulating filtration, homogenizing, degassing.
In the present invention, in step (1) in base oil used and step (2) and step (4) base oil used total amount and step Suddenly the weight ratio of base oil used is preferably 1:0.1-5:0.1-5 in (5).
Fourth aspect, the present invention also provides grease compositions made from the preparation method provided as third aspect present invention Object.
Compared with the lubricant composition made from the preparation method provided as second aspect, preparation side that the third aspect provides Lubricant composition made from method has better viscous resistance, mechanical stability, water-resistance, extreme pressure anti-wear and storage stable Property.
Embodiment
The present invention is further illustrated for embodiment below, but is not intended to limit the present invention.
In the following Examples and Comparative Examples:
Non-newtonian fluid sulfenyl phenolate-sulfoacid calcium in lubricant composition obtained, non-newtonian fluid calcium naphthenate, non-ox The total content of body calcium salicylate and non-newtonian fluid calcium oleate uses non-newtonian fluid sulfurized alkylphenol calcium-sulfoacid calcium % to indicate, That is,
Non-newtonian fluid sulfurized alkylphenol calcium-sulfoacid calcium %=(overbased or calcium sulfonate with high base number raw material weight+superelevation Base number or SULFURIZED CALCIUM ALKYL PHENATE WITH HIGH BASE NUMBER raw material weight+overbased or overbased calcium alkyl-salicylate raw material weight+overbased or High base number calcium salicylate raw material weight+overbased or high base number calcium oleate raw material weight+transforming agent total weight)/lubricating grease is total Weight × 100%.Transforming agent is included in non-newtonian fluid sulfurized alkylphenol calcium-sulfoacid calcium content.
Overbased and SULFURIZED CALCIUM ALKYL PHENATE WITH HIGH BASE NUMBER is prepared according to patent CN101423483.
Overbased and calcium sulfonate with high base number is prepared according to the method for patent CN101928239A.
Overbased and overbased calcium alkyl-salicylate raw material is purchased from Xinjiang Land Fine Petrochemical Co., Ltd.
Aphthenic acids is purchased from Jinzhou Tie Chen petrochemical industry Co., Ltd.
High base number calcium salicylate is prepared according to the method for patent CN1345921.
(NLGI Spokeman, 2009,73 (2): 1-17) prepared by method according to document for high base number calcium oleate.
Embodiment 1
The present embodiment is for illustrating lubricant composition prepared by the present invention.
Raw material components: overbased sulfoacid calcium (total base number 400mgKOH/g, 24kg)；Overbased sulfurized alkylphenol calcium (total base number 400mgKOH/g, 6kg)；(100 DEG C of kinematic viscosity are 31mm to HVI150BS lubricating base oil2/ s, 30kg)；4-ten Eight alkylphenols (2.8kg)；Acetic acid (0.56kg)；Boric acid (2.32kg)；Octadecylamine (1.5kg)；MDI(0.7kg)；HVI500SN (100 DEG C of kinematic viscosity are 11mm to lubricating base oil2/ s, 18kg).
It in a volume is 160L and with 24kg total base number is added in heating, stirring, circulation, cooling normal-pressure reaction kettle For the overbased sulfoacid calcium of 400mgKOH/g, 6kg total base number be 400mgKOH/g overbased sulfurized alkylphenol calcium and The HVI150BS lubricating base oil of 30kg, stirring, is warming up to 120 DEG C, the HVI500SN lubricating base oil and 1.5kg of 2kg is added Octadecylamine stirs 4 minutes, is added with stirring the 0.7kg MDI dissolved with 2kg HVI500SN lubricating base oil, stirs 4 minutes, The molar ratio of added MDI and octadecylamine be 1:2,120 DEG C constant temperature 20 minutes；50 DEG C are cooled to, constant temperature 10 minutes, is added 4-octadecylphenol of 2.8kg, temperature are controlled at 50 DEG C, are stirred 10 minutes；The acetic acid that 2.8kg concentration is 20 weight % is added Aqueous solution stirs 10 minutes；The boric acid aqueous solution that 16.24kg concentration is 14.3 weight % is added, stirs 10 minutes, is warming up to 80 DEG C, constant temperature 90 minutes, material retrogradation；It is warming up to 130 DEG C under stirring, is kept for 30 minutes, dehydration；Finally it is warming up to 200 DEG C of constant temperature 10 minutes.Then, 160 DEG C are cooled to, remaining HVI500SN lubricating base oil is added；110 DEG C are cooled to temperature, is circulated throughout Filter, homogenizing, degassing obtain finished product.Inspection result is shown in Table 1.
In the lubricating grease that the present embodiment obtains, on the basis of lubricating grease weight, composition are as follows: non-newtonian fluid sulfenyl phenolate 41.5 weight % of calcium-sulfoacid calcium；2.6 weight % of polyureas；55.9 weight % of lubricating base oil.
Embodiment 2
The present embodiment is for illustrating lubricant composition prepared by the present invention.
Raw material components: overbased sulfoacid calcium (total base number 400mgKOH/g, 24kg)；SULFURIZED CALCIUM ALKYL PHENATE WITH HIGH BASE NUMBER (total base number 320mgKOH/g, 6kg)；(100 DEG C of kinematic viscosity are 31mm to HVI150BS lubricating base oil2/ s, 10kg)；4-ten Eight alkylphenols (2.2kg)；N-butanol (0.6kg)；Acetic acid (0.56kg)；Boric acid (2.32kg)；Lauryl amine (1.31kg)；MDI (0.89kg)；(100 DEG C of kinematic viscosity are 11mm to HVI500SN lubricating base oil2/ s, 38kg).
It in a volume is 160L and with 24kg total base number is added in heating, stirring, circulation, cooling normal-pressure reaction kettle For the overbased sulfoacid calcium of 400mgKOH/g, 6kg total base number be 320mgKOH/g overbased sulfurized alkylphenol calcium and The HVI150BS lubricating base oil of 10kg, stirring, be warming up to 100 DEG C, be added 1kg HVI500SN lubricating base oil and 0.131kg lauryl amine stirs 8 minutes, is added with stirring the 0.0895kg MDI dissolved with 1kg HVI500SN lubricating base oil, Stirring 8 minutes, the molar ratio of added MDI and lauryl amine are 1:2,100 DEG C constant temperature 10 minutes；80 DEG C are cooled to, constant temperature 10 divides Clock, is added 4-octadecylphenol of 2.8kg and 0.6kg n-butanol, and temperature is controlled at 80 DEG C or so, stirred 10 minutes；It is added 2.8kg concentration is the aqueous acetic acid of 20 weight %, is stirred 10 minutes；The boric acid that 16.24kg concentration is 14.3 weight % is added Aqueous solution stirs 10 minutes, is warming up to 90 DEG C, and constant temperature 60 minutes, material retrogradation；It is warming up to 110 DEG C under stirring, is kept for 60 points Clock, dehydration；The HVI500SN lubricating base oil and 1.179kg lauryl amine of 1kg is added, stirs 8 minutes, is added with stirring with 1kg The 0.801kg MDI of HVI500SN lubricating base oil dissolution, is stirred 8 minutes, and the molar ratio of added MDI and lauryl amine is 1:2, 110 DEG C constant temperature 10 minutes；Finally being warming up to 230 DEG C, constant temperature for 5 minutes.Then, remaining HVI500SN lubricating base oil is added；To Temperature is cooled to 120 DEG C, and circulating filtration, homogenizing, degassing obtain finished product.Inspection result is shown in Table 1.
In the lubricating grease that the present embodiment obtains, on the basis of lubricating grease weight, composition are as follows: non-newtonian fluid sulfenyl phenolate 41.5 weight % of calcium-sulfoacid calcium；2.6 weight % of polyureas；55.9 weight % of lubricating base oil.
Embodiment 3
The present embodiment is for illustrating lubricant composition prepared by the present invention.
Raw material components: calcium sulfonate with high base number (total base number 320mgKOH/g, 6kg)；Overbased sulfurized alkylphenol calcium is (total Base number is 400mgKOH/g, 24kg)；(100 DEG C of kinematic viscosity are 31mm to HVI150BS lubricating base oil2/ s, 25kg)；4-ten eight Alkylphenol (2.8kg)；Acetic acid (0.56kg)；Boric acid (2.32kg)；Octadecylamine (1.66kg)；TDI(0.54kg)；HVI500SN (100 DEG C of kinematic viscosity are 11mm to lubricating base oil2/ s, 23kg).
It in a volume is 160L and with 6kg total base number is added in heating, stirring, circulation, cooling normal-pressure reaction kettle The overbased sulfurized alkylphenol calcium and 25kg that calcium sulfonate with high base number, 24kg total base number for 320mgKOH/g are 400mgKOH/g HVI150BS lubricating base oil, stirring, be warming up to 110 DEG C, the HVI500SN lubricating base oil and 1.66kg 18 of 2kg be added Amine stirs 6 minutes, is added with stirring the 0.54kg TDI dissolved with 2kg HVI500SN lubricating base oil, stirs 6 minutes, institute The molar ratio of the TDI and octadecylamine that add be 1:2,110 DEG C constant temperature 15 minutes；65 DEG C are cooled to, constant temperature 10 minutes, 2.8kg is added 4-octadecylphenols, temperature are controlled at 65 DEG C, are stirred 10 minutes；The aqueous acetic acid that 2.8kg concentration is 20 weight % is added, Stirring 10 minutes；The boric acid aqueous solution that 16.24kg concentration is 14.3 weight % is added, stirs 10 minutes, is warming up to 100 DEG C, perseverance Temperature 70 minutes, material retrogradation；It is warming up to 120 DEG C under stirring, is kept for 45 minutes, dehydration；180 DEG C of constant temperature 20 are finally warming up to divide Clock.Then, 160 DEG C are cooled to, remaining HVI500SN lubricating base oil is added；100 DEG C are cooled to temperature, circulating filtration, Homogenizing, degassing obtain finished product.Inspection result is shown in Table 1.
In the lubricating grease that the present embodiment obtains, on the basis of lubricating grease weight, composition are as follows: non-newtonian fluid sulfenyl phenolate 39.6 weight % of calcium-sulfoacid calcium；2.6 weight % of polyureas；57.8 weight % of lubricating base oil.
Embodiment 4
The present embodiment is for illustrating lubricant composition prepared by the present invention.
Raw material components: calcium sulfonate with high base number (total base number 320mgKOH/g, 14kg)；SULFURIZED CALCIUM ALKYL PHENATE WITH HIGH BASE NUMBER is (total Base number is 320mgKOH/g, 6kg)；Naphthenate with superhigh base number calcium (total base number 400mgKOH/g, 10kg)；HVI150BS lubrication (100 DEG C of kinematic viscosity are 31mm to base oil2/ s, 15kg)；4-octadecylphenols (2.8kg)；Acetic acid (0.56kg)；Boric acid (2.32kg)；Octadecylamine (1.5kg)；MDI(0.7kg)；(100 DEG C of kinematic viscosity are 11mm to HVI500SN lubricating base oil2/ s, 7kg)；It is right, right '-di-iso-octyldiphenylamine (0.4kg).
Lubricant composition is prepared according to the method for embodiment 1, unlike, sulfoacid calcium is using total base number The calcium sulfonate with high base number of 320mgKOH/g, the high base number sulfenyl phenolate that sulfurized alkylphenol calcium is 320mgKOH/g using total base number Calcium, and increase the naphthenate with superhigh base number calcium that total base number is 400kgKOH/g；And 110 DEG C are cooled to temperature, is added Pair of 0.4kg, right '-di-iso-octyldiphenylamine stir 10 minutes, and then circulating filtration, homogenizing, degassing obtain finished product；Each ingredient Dosage it is as above.Inspection result is shown in Table 1.
In the lubricating grease that the present embodiment obtains, on the basis of lubricating grease weight, composition are as follows: non-newtonian fluid sulfenyl phenolate 59.2 weight % of calcium-sulfoacid calcium；3.6 weight % of polyureas；36.5 weight % of lubricating base oil；It is right, right '-di-iso-octyldiphenylamine 0.7 weight %.
Embodiment 5
The present embodiment is for illustrating lubricant composition prepared by the present invention.
Raw material components: overbased sulfoacid calcium (total base number 400mgKOH/g, 10kg)；Overbased sulfurized alkylphenol calcium (total base number 400mgKOH/g, 10kg)；Overbased calcium salicylate (total base number 400mgKOH/g, 10kg)；HVI150BS (100 DEG C of kinematic viscosity are 31mm to lubricating base oil2/ s, 25kg)；4-octadecylphenols (2.8kg)；Acetic acid (0.56kg)；Boron Sour (2.32kg)；Octadecylamine (4.5kg)；MDI(2.1kg)；(100 DEG C of kinematic viscosity are 11mm to HVI500SN lubricating base oil2/ S, 18kg).
Lubricant composition is prepared according to the method for embodiment 1, unlike, high base number material increases overbased water Poplar acid calcium, the dosage of each ingredient are as above.Inspection result is shown in Table 1.
In the lubricating grease that the present embodiment obtains, on the basis of lubricating grease weight, composition are as follows: non-newtonian fluid sulfenyl phenolate 41.8 weight % of calcium-sulfoacid calcium；7.8 weight % of polyureas；50.4 weight % of lubricating base oil.
Embodiment 6
The present embodiment is for illustrating lubricant composition prepared by the present invention.
Raw material components: overbased sulfoacid calcium (total base number 400mgKOH/g, 6kg)；SULFURIZED CALCIUM ALKYL PHENATE WITH HIGH BASE NUMBER is (total Base number is 320mgKOH/g, 20kg)；Overbased calcium oleate (total base number 400mgKOH/g, 4kg)；Poly- α-the alkene of full synthetic oil (100 DEG C of kinematic viscosity are 41mm to hydrocarbon ils PAO 402/ s, 25kg)；4-octadecylphenols (2.8kg)；Acetic acid (0.56kg)；Boron Sour (2.32kg)；Octadecylamine (1.5kg)；MDI(0.7kg)；(100 DEG C of kinematic viscosity are the poly- α of full synthetic oil-alkene oil PAO 10 11mm2/ s, 23kg)；Two thio dibutylphosphoric acid zinc (2kg), dibutyl dithiocaarbamate molybdenum (1kg), tungsten disulfide (2kg), two tungsten selenides (2kg) are right, right '-di-iso-octyldiphenylamine (0.2kg).
Lubricant composition is prepared according to the method for embodiment 1, unlike, sulfurized alkylphenol calcium is using total base number The SULFURIZED CALCIUM ALKYL PHENATE WITH HIGH BASE NUMBER of 320mgKOH/g, and increase the overbased calcium oleate that total base number is 400kgKOH/g；Make HVI150BS and HVI500SN are replaced respectively with the poly- α of full synthetic oil-alkene oil PAO 40 and PAO10；And it is cooled to temperature 110 DEG C, the two thio dibutylphosphoric acid zinc of 2kg are added, stirs 10 minutes, the dibutyl dithiocaarbamate molybdenum of 1kg is added, The tungsten disulfide of 2kg is added in stirring 10 minutes, stirs 10 minutes, and two tungsten selenides of 2kg are added, and stirs 10 minutes, is added Pair of 0.2kg, right '-di-iso-octyldiphenylamine stir 10 minutes, and then circulating filtration, homogenizing, degassing obtain finished product；Each ingredient Dosage it is as above.Inspection result is shown in Table 1.
In the lubricating grease that the present embodiment obtains, on the basis of lubricating grease weight, composition are as follows: non-newtonian fluid sulfenyl phenolate 38.3 weight % of calcium-sulfoacid calcium；2.4 weight % of polyureas；51.6 weight % of lubricating base oil；Two thio dibutylphosphoric acid zinc 2.2 Weight %；1.1 weight % of dibutyl dithiocaarbamate molybdenum；2.1 weight % of tungsten disulfide；Two tungsten selenides, 2.1 weight %； It is right, right ' 0.2 weight % of-di-iso-octyldiphenylamine.
Embodiment 7
The present embodiment is for illustrating lubricant composition prepared by the present invention.
Raw material components: calcium sulfonate with high base number (total base number 320mgKOH/g, 6kg)；Overbased sulfurized alkylphenol calcium is (total Base number is 400mgKOH/g, 12kg)；Overbased calcium alkyl-salicylate (total base number 300mgKOH/g, 6kg)；High base number calcium salicylate (total base number 300mgKOH/g, 6kg)；(100 DEG C of kinematic viscosity are 31mm to HVI150BS lubricating base oil2/ s, 25kg)；4-ten Eight alkylphenols (2.8kg)；Acetic acid (0.56kg)；Boric acid (2.32kg)；Octadecylamine (1.5kg)；MDI(0.7kg)；HVI500SN (100 DEG C of kinematic viscosity are 11mm to lubricating base oil2/ s, 23kg).
Lubricant composition is prepared according to the method for embodiment 1, unlike, sulfoacid calcium is using total base number The calcium sulfonate with high base number of 320mgKOH/g, while increasing overbased calcium alkyl-salicylate and high base number calcium salicylate；The use of each ingredient Amount is as above.Inspection result is shown in Table 1.
In the lubricating grease that the present embodiment obtains, on the basis of lubricating grease weight, composition are as follows: non-newtonian fluid sulfenyl phenolate 41.5 weight % of calcium-sulfoacid calcium；2.6 weight % of polyureas；55.9 weight % of lubricating base oil.
Embodiment 8
The present embodiment is for illustrating lubricant composition prepared by the present invention.
Raw material components: calcium sulfonate with high base number (total base number 320mgKOH/g, 6kg)；SULFURIZED CALCIUM ALKYL PHENATE WITH HIGH BASE NUMBER (total alkali Value is 320mgKOH/g, 12kg)；High base number calcium salicylate (total base number 360mgKOH/g, 6kg)；High base number calcium oleate (total alkali Value is 400mgKOH/g, 6kg)；(100 DEG C of kinematic viscosity are 31mm to HVI150BS lubricating base oil2/ s, 25kg)；4-octadecanes Base phenol (2.8kg)；Acetic acid (0.56kg)；Boric acid (2.32kg)；Octadecylamine (1.5kg)；MDI(0.7kg)；HVI500SN lubrication (100 DEG C of kinematic viscosity are 11mm to base oil2/ s, 23kg).
Lubricant composition is prepared according to the method for embodiment 1, unlike, sulfoacid calcium is using total base number The calcium sulfonate with high base number of 320mgKOH/g, the high base number sulfenyl phenolate that sulfurized alkylphenol calcium is 320mgKOH/g using total base number Calcium, while increasing high base number calcium salicylate and high base number calcium oleate；The dosage of each ingredient is as above.Inspection result is shown in Table 1.
In the lubricating grease that the present embodiment obtains, on the basis of lubricating grease weight, composition are as follows: non-newtonian fluid sulfenyl phenolate 41.5 weight % of calcium-sulfoacid calcium；2.6 weight % of polyureas；55.9 weight % of lubricating base oil.
Embodiment 9
The present embodiment is for illustrating lubricant composition prepared by the present invention.
Raw material components: overbased sulfoacid calcium (total base number 400mgKOH/g, 10kg)；Overbased sulfurized alkylphenol calcium (total base number 400mgKOH/g, 10kg)；Overbased calcium alkyl-salicylate (total base number 360mgKOH/g, 5kg)；High base number calcium oleate (total base number 320mgKOH/g, 5kg)；(100 DEG C of kinematic viscosity are 31mm to HVI150BS lubricating base oil2/ s, 25kg)；4-ten Eight alkylphenols (2.8kg)；Acetic acid (0.56kg)；Boric acid (2.32kg)；Octadecylamine (0.94kg)；Para-totuidine (0.38kg)； MDI(0.88kg)；(100 DEG C of kinematic viscosity are 11mm to HVI500SN lubricating base oil2/ s, 23kg).
Lubricant composition is prepared according to the method for embodiment 1, unlike, increase overbased calcium alkyl-salicylate and high-alkali It is worth calcium oleate, meanwhile, after octadecylamine is added, it is additionally added para-totuidine, then adds MDI；The dosage of each ingredient is as above.It examines It the results are shown in Table 1.
In the lubricating grease that the present embodiment obtains, on the basis of lubricating grease weight, composition are as follows: non-newtonian fluid sulfenyl phenolate 41.5 weight % of calcium-sulfoacid calcium；2.6 weight % of polyureas；55.9 weight % of lubricating base oil.
Embodiment 10
The present embodiment is for illustrating lubricant composition prepared by the present invention.
Raw material components: calcium sulfonate with high base number (total base number 320mgKOH/g, 5kg)；SULFURIZED CALCIUM ALKYL PHENATE WITH HIGH BASE NUMBER (total alkali Value is 320mgKOH/g, 12kg)；Naphthenate with superhigh base number calcium (total base number 400mgKOH/g, 3kg)；Overbased salicylic acid Calcium (total base number 400mgKOH/g, 5kg)；Overbased calcium oleate (total base number 400mgKOH/g, 5kg)；HVI150BS profit (100 DEG C of kinematic viscosity are 31mm to sliding base oil2/ s, 25kg)；4-octadecylphenols (1.6kg)；(total acid number is aphthenic acids 180mgKOH/g, 1.2kg)；Acetic acid (0.56kg)；Boric acid (2.32kg)；Octadecylamine (0.84kg)；Lauryl amine (0.58kg)；MDI (0.78kg)；(100 DEG C of kinematic viscosity are 11mm to HVI500SN lubricating base oil2/ s, 23kg).
Lubricant composition is prepared according to the method for embodiment 1, unlike, sulfoacid calcium is using total base number The calcium sulfonate with high base number of 320mgKOH/g, the high base number sulfenyl phenolate that sulfurized alkylphenol calcium is 320mgKOH/g using total base number Calcium, and increase naphthenate with superhigh base number calcium, calcium salicylate and calcium oleate；After 4-octadecylphenols are added, it is additionally added cycloalkanes Then acid adds acetic acid and boric acid；After octadecylamine is added, it is additionally added lauryl amine, then adds MDI；The dosage of each ingredient As above.Inspection result is shown in Table 1.
In the lubricating grease that the present embodiment obtains, on the basis of lubricating grease weight, composition are as follows: non-newtonian fluid sulfenyl phenolate 41.5 weight % of calcium-sulfoacid calcium；2.6 weight % of polyureas；55.9 weight % of lubricating base oil.
Embodiment 11
The present embodiment is for illustrating lubricant composition prepared by the present invention.
Raw material components: calcium sulfonate with high base number (total base number 360mgKOH/g, 5kg)；SULFURIZED CALCIUM ALKYL PHENATE WITH HIGH BASE NUMBER (total alkali Value is 360mgKOH/g, 12kg)；Overbased calcium alkyl-salicylate (total base number 300mgKOH/g, 3kg)；High base number calcium salicylate is (total Base number is 300mgKOH/g, 5kg)；High base number calcium oleate (total base number 300mgKOH/g, 5kg)；HVI150BS lubricating base oil (100 DEG C of kinematic viscosity are 31mm2/ s, 25kg)；4-octadecylphenols (2.8kg)；N-butanol (1kg)；Acetic acid (0.56kg)； Boric acid (2.32kg)；Octadecylamine (1.5kg)；MDI(0.7kg)；(100 DEG C of kinematic viscosity are HVI500SN lubricating base oil 11mm2/ s, 23kg).
Lubricant composition is prepared according to the method for embodiment 1, unlike, sulfoacid calcium is using total base number The calcium sulfonate with high base number of 360mgKOH/g, the high base number sulfenyl phenolate that sulfurized alkylphenol calcium is 360mgKOH/g using total base number Calcium, while increasing overbased calcium alkyl-salicylate, calcium salicylate and calcium oleate；Transforming agent increases n-butanol, is being added 4-ten eight It is added after alkylphenol；The dosage of each ingredient is as above.Inspection result is shown in Table 1.
In the lubricating grease that the present embodiment obtains, on the basis of lubricating grease weight, composition are as follows: non-newtonian fluid sulfenyl phenolate 41.5 weight % of calcium-sulfoacid calcium；2.6 weight % of polyureas；55.9 weight % of lubricating base oil.
Embodiment 12
The present embodiment is for illustrating lubricant composition prepared by the present invention.
The preparation of non-newtonian fluid calcium sulfonate with high base number: in a volume being 30L and with heating, stirring, circulation, cooling 100 DEG C of kinematic viscosity of calcium sulfonate with high base number and 5kg that 15kg total base number is 350mgKOH/g are added in normal-pressure reaction kettle is 31mm2The HVI150BS lubricating base oil of/s, stirring, heats to 80 DEG C, constant temperature 10 minutes；2.5kg dodecyl is added Benzene sulfonic acid, temperature are controlled at 80 DEG C or so, are stirred 10 minutes；The acetic acid and 4 times of acetic acid weight of aqueous solution of 0.5kg is added, stirs It mixes 10 minutes；85 DEG C are warming up to, constant temperature 90 minutes, it is spare to obtain non-newtonian fluid sulfoacid calcium at smectic for material retrogradation.
It in volume is 160L and with above-mentioned prepare is added in heating, stirring, circulation, cooling normal-pressure reaction kettle A The overbased sulfurized alkylphenol calcium and 25kg that non-newtonian fluid calcium sulfonate with high base number, 7kg total base number are 400mgKOH/g (100 DEG C of kinematic viscosity are 31mm to HVI150BS lubricating base oil2/ s, similarly hereinafter), it stirs evenly.
In volume for 10L and with heating, the HVI500SN for stirring, recycling, 5kg being added in the normal-pressure reaction kettle B of cooling (100 DEG C of kinematic viscosity are 11mm to lubricating base oil2/ s, similarly hereinafter) and 1kg MDI rapidly pre-warming is to 90 DEG C, is quickly added with stirring 0.12kg ethylenediamine stirs 4 minutes, 1.08kg octadecylamine is added and stirs 4 minutes, and added MDI, ethylenediamine and octadecylamine rub You than be 2:1:2,120 DEG C constant temperature 20 minutes, obtain polyureas I.
It in volume is 20L and with 10kg100 DEG C of movement is added in heating, stirring, circulation, cooling normal-pressure reaction kettle C Viscosity is 11mm2The HVI500SN lubricating base oil and 1.29kg MDI of/s is preheating to 90 DEG C, is quickly added with stirring 0.84kg Octadecylamine and 0.19kg ethylenediamine, added MDI, octadecylamine, ethylenediamine molar ratio be 3.3:2:2,120 DEG C of constant temperature 20 divide Clock obtains polyureas II.
Gained polyureas I and polyureas II are all squeezed into reaction kettle A, stirred evenly, at 60 DEG C, constant temperature 10 minutes, is added Enter 4-octadecylphenol of 3kg, temperature is controlled at 60 DEG C, stirred 10 minutes；It is water-soluble that the 12.5kg butanol that concentration is 20% is added Liquid stirs 10 minutes；87 DEG C constant temperature 70 minutes, material retrogradation；It is warming up to 130 DEG C under stirring, is kept for 30 minutes, dehydration.Most After be warming up to 200 DEG C constant temperature for 5 minutes.Then, 150 DEG C are cooled to, the HVI500SN lubricating base oil of 8kg is added；To temperature 110 DEG C are cooled to, circulating filtration, homogenizing, degassing obtain finished product.Inspection result is shown in Table 1.
In the lubricating grease that the present embodiment obtains, on the basis of lubricating grease weight, composition are as follows: non-newtonian fluid sulfenyl phenolate 40.4 weight % of calcium-sulfoacid calcium；5.0 weight % of polyureas；54.6 weight % of lubricating base oil.
Embodiment 13
The present embodiment is for illustrating lubricant composition prepared by the present invention.
It in a volume is 160L and with 6kg total base number is added in heating, stirring, circulation, cooling normal-pressure reaction kettle Overbased sulfurized alkylphenol calcium, the 6kg for being 420mgKOH/g for the overbased sulfoacid calcium of 400mgKOH/g, 6kg total base number High base number calcium salicylate that overbased calcium alkyl-salicylate that total base number is 320mgKOH/g, 6kg total base number are 360mgKOH/g, 6kg Total base number is the overbased calcium oleate of 400mgKOH/g and the HVI150BS lubricating base oil of 10kg, is stirred evenly.
In volume for 20L and with heating, the HVI500SN for stirring, recycling, 10kg being added in the normal-pressure reaction kettle of cooling Lubricating base oil and 1.17kg MDI are preheating to 80 DEG C, be quickly added with stirring 0.84kg octadecylamine, 0.19kg ethylenediamine it is mixed Close object, added MDI, monoamine, diamines molar ratio be 3:2:2,120 DEG C constant temperature 20 minutes, obtain polyureas.
Gained polyureas is all squeezed into a upper kettle, is stirred evenly, at 50 DEG C, constant temperature 10 minutes；1kg 12 is added 4-octadecylphenol of alkyl benzene sulphonate and 1kg, temperature are controlled at 50 DEG C, are stirred 10 minutes；1kg methanol is added, stirs 10 points Clock；The aqueous acetic acid that 2kg concentration is 20 weight % is added, stirs 10 minutes；83 DEG C constant temperature 80 minutes, material retrogradation；It stirs It mixes down and is warming up to 120 DEG C, kept for 45 minutes, dehydration.Finally being warming up to 200 DEG C, constant temperature for 5 minutes.Then, it is added 8kg's HVI500SN lubricating base oil；110 DEG C are cooled to temperature, circulating filtration, homogenizing, degassing obtain finished product.Inspection result is shown in Table 1。
In the lubricating grease that the present embodiment obtains, on the basis of lubricating grease weight, composition are as follows: non-newtonian fluid sulfenyl phenolate 52.5 weight % of calcium-sulfoacid calcium；3.5 weight % of polyureas；44.0 weight % of lubricating base oil.
Embodiment 14
The present embodiment is for illustrating lubricant composition prepared by the present invention.
Raw material components: overbased sulfoacid calcium (total base number 400mgKOH/g, 24kg)；Overbased sulfurized alkylphenol calcium (total base number 400mgKOH/g, 6kg)；(100 DEG C of kinematic viscosity are 31mm to HVI150BS lubricating base oil2/ s, 30kg)；4-ten Eight alkylphenols (2.8kg)；Acetic acid (0.56kg)；Boric acid (2.32kg)；Octadecylamine (1.5kg)；MDI(0.7kg)；HVI500SN (100 DEG C of kinematic viscosity are 11mm to lubricating base oil2/ s, 18kg).
It in a volume is 160L and with 24kg total base number is added in heating, stirring, circulation, cooling normal-pressure reaction kettle For the overbased sulfoacid calcium of 400mgKOH/g, 6kg total base number be 400mgKOH/g overbased sulfurized alkylphenol calcium and The HVI150BS lubricating base oil of 30kg, stirring, heats to 50 DEG C, constant temperature 10 minutes；4-octadecyl of 2.8kg is added Phenol, temperature are controlled at 50 DEG C, are stirred 10 minutes；The aqueous acetic acid that 2.8kg concentration is 20 weight % is added, stirs 10 points Clock；The boric acid aqueous solution that 16.24kg concentration is 14.3 weight % is added, stirs 10 minutes, is warming up to 80 DEG C, constant temperature 90 minutes, Material retrogradation；It is warming up to 130 DEG C under stirring, is kept for 30 minutes, dehydration.
It in another volume is 10L and with being added 2kg's in heating, stirring, circulation, cooling normal-pressure reaction kettle HVI500SN lubricating base oil and 1.5kg octadecylamine are warming up to 120 DEG C, stir 4 minutes, are added with stirring with 2kg The 0.7kg MDI of HVI500SN lubricating base oil dissolution, is stirred 4 minutes, and the molar ratio of added MDI and octadecylamine is 1:2, 120 DEG C constant temperature 20 minutes, obtain polyureas.
Gained polyureas is all squeezed into a upper kettle, is stirred evenly, is finally warming up to 200 DEG C of constant temperature 10 minutes.Then, 160 DEG C are cooled to, remaining HVI500SN lubricating base oil is added；110 DEG C are cooled to temperature, circulating filtration, homogenizing, degassing Obtain finished product.Inspection result is shown in Table 1.
In the lubricating grease that the present embodiment obtains, on the basis of lubricating grease weight, composition are as follows: non-newtonian fluid sulfenyl phenolate 41.5 weight % of calcium-sulfoacid calcium；2.6 weight % of polyureas；55.9 weight % of lubricating base oil.
The two polyureas molecular structural formulas contained in component are as follows:
Embodiment 15
The present embodiment is for illustrating lubricant composition prepared by the present invention.
Raw material components: overbased sulfoacid calcium (total base number 400mgKOH/g, 24kg)；Overbased sulfurized alkylphenol calcium (total base number 400mgKOH/g, 6kg)；(100 DEG C of kinematic viscosity are 31mm to HVI150BS lubricating base oil2/ s, 30kg)；4-ten Eight alkylphenols (2.8kg)；Acetic acid (0.56kg)；Boric acid (2.32kg)；Octadecylamine (1.5kg)；MDI(0.7kg)；HVI500SN (100 DEG C of kinematic viscosity are 11mm to lubricating base oil2/ s, 18kg).
It in a volume is 160L and with 24kg total base number is added in heating, stirring, circulation, cooling normal-pressure reaction kettle For the overbased sulfoacid calcium of 400mgKOH/g, 6kg total base number be 400mgKOH/g overbased sulfurized alkylphenol calcium and The HVI150BS lubricating base oil of 30kg, stirring are warming up to 50 DEG C, constant temperature 10 minutes, 4-octadecylphenol of 2.8kg are added, Temperature is controlled at 50 DEG C, is stirred 10 minutes；The aqueous acetic acid that 2.8kg concentration is 20 weight % is added, stirs 10 minutes；It is added 16.24kg concentration is the boric acid aqueous solution of 14.3 weight %, is stirred 10 minutes, is warming up to 80 DEG C, constant temperature 90 minutes, material became It is thick；It is warming up to 130 DEG C under stirring, is kept for 30 minutes, dehydration；The HVI500SN lubricating base oil and 1.5kg 18 of 2kg is added Amine stirs 4 minutes, is added with stirring the 0.7kg MDI dissolved with 2kg HVI500SN lubricating base oil, stirs 4 minutes, added MDI and octadecylamine molar ratio be 1:2,120 DEG C constant temperature 20 minutes.Finally it is warming up to 200 DEG C of constant temperature 10 minutes.Then, cold But to 160 DEG C, remaining HVI500SN lubricating base oil is added；110 DEG C are cooled to temperature, circulating filtration, deaerates at homogenizing To finished product.Inspection result is shown in Table 1.
In the lubricating grease that the present embodiment obtains, on the basis of lubricating grease weight, composition are as follows: non-newtonian fluid sulfenyl phenolate 41.5 weight % of calcium-sulfoacid calcium；2.6 weight % of polyureas；55.9 weight % of lubricating base oil.
Embodiment 16
The present embodiment is for illustrating lubricant composition prepared by the present invention.
Lubricant composition is prepared according to the method for embodiment 1, unlike, 4-octadecylphenols are replaced with into fourth Ketone, replaces with ethylene glycol monobutyl ether for aqueous acetic acid, and boric acid aqueous solution is replaced with octadecylamine.Inspection result is shown in Table 1.
In the lubricating grease that the present embodiment obtains, on the basis of lubricating grease weight, composition are as follows: non-newtonian fluid sulfenyl phenolate 41.5 weight % of calcium-sulfoacid calcium；2.6 weight % of polyureas；55.9 weight % of lubricating base oil.
Comparative example 1
Lubricant composition is prepared according to the method for embodiment 1, unlike, overbased sulfurized alkylphenol calcium total alkali Value is replaced by the overbased sulfoacid calcium of 400mgKOH/g, and obtained each performance data of lubricating grease finished product is shown in Table 1.
In the lubricating grease that this comparative example obtains, on the basis of lubricating grease weight, composition are as follows: 41.5 weight of non-newtonian fluid sulfoacid calcium Measure %；2.6 weight % of polyureas；55.9 weight % of lubricating base oil.
Each lubricating grease properties of sample data of table 1
Each indication test method: dropping point: GB/T 3498；Work cone penetration and extension work cone penetration: GB/T 269；It is rotten Erosion: GB/T 7326；Anticorrosive property: GB/T 5018；Water drenches number of dropouts: SH/T 0109；Salt spray test: SH/T 0081；Water resistant It is spraying: SH/T0643；Stencil oil-dividing: SH/T 0324；Surface hardened layer value: 0370 appendix A of SH/T；Coefficient of friction: SH/T 0721；Tetra-ball machine test: SH/T 0202；The bearing lubrication service life: ASTM D 3336.
Each lubricating grease properties of sample data of 1 (Continued) of table
Each indication test method: dropping point: GB/T 3498；Work cone penetration and extension work cone penetration: GB/T 269；It is rotten Erosion: GB/T 7326；Anticorrosive property: GB/T 5018；Water drenches number of dropouts: SH/T 0109；Salt spray test: SH/T 0081；Water resistant It is spraying: SH/T0643；Stencil oil-dividing: SH/T 0324；Surface hardened layer value: 0370 appendix A of SH/T；Coefficient of friction: SH/T 0721；Tetra-ball machine test: SH/T 0202；The bearing lubrication service life: ASTM D 3336.
It will be understood by those skilled in the art that work cone penetration is smaller, grease thickening performance is better；Extend work The difference for making cone penetration and the cone penetration that works is smaller, and the mechanical stability of lubricating grease can be better；Water leaching number of dropouts is smaller, lubricating grease Water-resistance it is better；Salt spray test higher grade, and the antirust and anticorrosive property of lubricating grease are better；Water resistant is worth smaller, lubrication by spraying The adhesiveness and water-resistance of rouge are better；Stencil oil-dividing value is smaller, and the colloid stability of lubricating grease is better；Surface hardened layer value it is absolute It is worth smaller, the storage stability of lubricating grease is better；Coefficient of friction is smaller, and the abrasion resistance of lubricating grease is better；PB, PD value are bigger, The extreme pressure anti-wear of lubricating grease is better.
Embodiment 1 and comparative example 1 are compared to antirust and anticorrosion as can be seen that lubricant composition of the invention Property, storage stability be substantially better than sulfoacid calcium base polyurea grease.Moreover, lubricant composition of the invention, which has, is better than sulfonic acid Viscous resistance, mechanical stability, water-resistance, colloid stability, abrasion resistance, extreme pressure anti-wear and the bearing of calcium base polyurea grease Lubricating life.Moreover, lubricant composition of the invention also has excellent heat-resisting quantity.
Embodiment 1 and embodiment 14 are compared the lubricant composition as can be seen that being prepared in situ, had better Viscous resistance, mechanical stability, water-resistance, extreme pressure anti-wear and storage stability；By embodiment 1 and embodiment 14, embodiment 15 It is compared as can be seen that first carrying out the reaction of polyurea compound, then converted, lubricant composition obtained has more preferable Viscous resistance, mechanical stability, water-resistance, colloid stability, storage stability, abrasion resistance, extreme pressure anti-wear and bearing profit The sliding service life；Embodiment 1 and embodiment 16 are compared as can be seen that transforming agent is selected from dodecyl benzene sulfonic acid, aphthenic acids, ten At least one of eight alkyl phenols, methanol, isopropanol, butanol, boric acid, acetic acid and water, lubricant composition obtained have more Good viscous resistance, mechanical stability, water-resistance, colloid stability, storage stability, abrasion resistance, extreme pressure anti-wear and bearing Lubricating life.
Lubricant composition of the invention with the antirust quite even more excellent with sulfoacid calcium base polyurea grease and is prevented Corrosivity, and there is excellent storage stability, also have the viscous resistance better than sulfoacid calcium base polyurea grease, machinery stable Property, water-resistance, colloid stability, abrasion resistance, extreme pressure anti-wear and bearing lubrication service life, and also there is excellent heat-resisting quantity Etc. performances.The feed preparation process of lubricating grease of the invention is simple and environmentally-friendly, stable product quality.
The preferred embodiment of the present invention has been described above in detail, still, during present invention is not limited to the embodiments described above Detail within the scope of the technical concept of the present invention can be with various simple variants of the technical solution of the present invention are made, this A little simple variants all belong to the scope of protection of the present invention.
It is further to note that specific technical features described in the above specific embodiments, in not lance In the case where shield, can be combined in any appropriate way, in order to avoid unnecessary repetition, the present invention to it is various can No further explanation will be given for the combination of energy.
In addition, various embodiments of the present invention can be combined randomly, as long as it is without prejudice to originally The thought of invention, it should also be regarded as the disclosure of the present invention.

Claims (23)

1. a kind of lubricant composition, the lubricant composition contains base oil and thickening agent, which is characterized in that the thickening Agent contains non-newtonian fluid sulfurized alkylphenol calcium-sulfoacid calcium and polyurea compound, and the thickening agent also optionally contains non-newtonian fluid One of calcium naphthenate, non-newtonian fluid calcium salicylate and non-newtonian fluid calcium oleate are a variety of, with the weight of lubricant composition On the basis of, non-newtonian fluid sulfurized alkylphenol calcium-sulfoacid calcium content is 10-70 weight %；The content of non-newtonian fluid calcium naphthenate For 0-70 weight %；The content of non-newtonian fluid calcium salicylate is 0-70 weight %；The content of non-newtonian fluid calcium oleate is 0-70 weight Measure %；The content of polyurea compound is 0.5-30 weight %；The content of base oil is 10-80 weight %.
2. lubricant composition according to claim 1, wherein on the basis of the weight of lubricant composition, non newtonian Body sulfurized alkylphenol calcium-sulfoacid calcium content is 20-65 weight %；The content of non-newtonian fluid calcium naphthenate is 0-50 weight %； The content of non-newtonian fluid calcium salicylate is 0-50 weight %；The content of non-newtonian fluid calcium oleate is 0-50 weight %；Polyureas chemical combination The content of object is 1-20 weight %；The content of base oil is 20-70 weight %.
3. lubricant composition according to claim 1 or 2, wherein the non-newtonian fluid sulfurized alkylphenol calcium-sulfonic acid Calcium is converted by newton body sulfoacid calcium and newton body sulfurized alkylphenol calcium, the non-newtonian fluid sulfurized alkylphenol calcium-sulphur The total base number of sour calcium is 250-450mgKOH/g；The non-newtonian fluid calcium naphthenate is to convert to obtain by newton body calcium naphthenate , the total base number of the non-newtonian fluid calcium naphthenate is 250-450mgKOH/g；The non-newtonian fluid calcium salicylate is by newton Body calcium salicylate converts, and the total base number of the non-newtonian fluid calcium salicylate is 250-450mgKOH/g；The non newtonian Body calcium oleate is converted by newton body calcium oleate, and the total base number of the non-newtonian fluid calcium oleate is 250-450mgKOH/ g。
4. lubricant composition according to claim 1 or 2, wherein the structural formula of the polyurea compound is
Wherein, n is 0-3 integer, R1、R4It is alkyl, naphthenic base or aryl, R2It is alkylidene or arlydene, R3It is arlydene, Asia Alkyl or cycloalkylidene.
5. lubricant composition according to claim 4, wherein polyurea compound is two polyurea compounds, four polyureas Close at least one of object, six polyurea compounds and eight polyurea compounds.
6. lubricant composition according to claim 4, wherein R1、R4It is phenyl or substituted phenyl or carbon number is 8- 24 alkyl or cycloalkyl；R2It is the alkylidene that phenylene or biphenylene or carbon number are 2-12；R3It is the Asia that carbon number is 6-30 Aryl, alkylidene or cycloalkylidene.
7. lubricant composition according to claim 6, wherein R1、R4It is phenyl or C1–C3Alkyl or halogen replace Phenyl or carbon number be 10-18 alkyl or cycloalkyl；R2It is the alkylidene that phenylene or biphenylene or carbon number are 2-8；R3 It is With- (CH2)6At least one of.
8. the preparation method of lubricant composition described in any one of claim 1-7, this method comprises: by thickening agent and Part basis oil is uniformly mixed, and refines in 180-230 DEG C of constant temperature, surplus base oil is added, necessary additive is added, obtains into Product, which is characterized in that the thickening agent contains non-newtonian fluid sulfurized alkylphenol calcium-sulfoacid calcium and polyurea compound, the thickening Agent also optionally contains one of non-newtonian fluid calcium naphthenate, non-newtonian fluid calcium salicylate and non-newtonian fluid calcium oleate or more Kind.
9. a kind of preparation method of lubricant composition, which is characterized in that this method comprises:
(1) newton body sulfurized alkylphenol calcium, newton body and/or non-newtonian fluid sulfoacid calcium will be contained, or contain newton body and/or non- Newton body sulfurized alkylphenol calcium, the high base number material of newton body sulfoacid calcium and the mixing of part basis oil, obtain mixture, described High base number material also optionally contains newton body and/or non-newtonian fluid calcium naphthenate, newton body and/or non-newtonian fluid calcium salicylate With one of newton body and/or non-newtonian fluid calcium oleate or a variety of；
(2) it optionally carries out the reaction of at least partly polyurea compound: part basis oil and monoamine is added, or is additionally added diamines, Diisocyanate is added to be reacted；
(3) transforming agent is added, heats up to material retrogradation, further heats up dehydration；
(4) reaction of remaining polyurea compound is carried out；
(5) 180-230 DEG C of constant temperature refinings are warming up to, surplus base oil is added, necessary additive is added, obtains finished product, with institute On the basis of the weight for obtaining finished product, non-newtonian fluid sulfurized alkylphenol calcium-sulfoacid calcium content is 10-70 weight %；Non-newtonian fluid ring The content of alkanoic acid calcium is 0-70 weight %；The content of non-newtonian fluid calcium salicylate is 0-70 weight %；Non-newtonian fluid calcium oleate Content is 0-70 weight %；The content of polyurea compound is 0.5-30 weight %；The content of base oil is 10-80 weight %.
10. preparation method according to claim 9, wherein in step (2), carry out the anti-of at least partly polyurea compound It answers.
11. preparation method according to claim 9 or 10, wherein in step (2) and step (4), part basis is added After oil, monoamine, optional diamines, diisocyanate, 100-120 DEG C constant temperature 10-30 minutes, wherein monoamine, optional two Amine, diisocyanate the amount of substance meet following relationship: the amount of the amount of the substance of diisocyanate × 2=monoamine substance+ Amount × 2 of the substance of diamines, or, diisocyanate is excessive, excessive amount≤10%.
12. preparation method according to claim 9 or 10, wherein in step (3), at 50-80 DEG C, required turn is added Agent is reacted, after all transforming agents add, 80-100 DEG C constant temperature 60-90 minutes, then heat to 110-130 DEG C it is de- Water.
13. preparation method according to claim 9 or 10, wherein in step (5), be warming up to 180-230 DEG C of constant temperature 5-30 Minute, be added surplus base oil, be cooled to 100-120 DEG C to temperature, necessary additive be added, stir, circulating filtration, Change, degassing.
14. preparation method according to claim 9 or 10, wherein the newton body sulfurized alkylphenol calcium is synthesis vulcanization Alkyl phenol calcium, the total base number of the newton body sulfurized alkylphenol calcium are 250-450mgKOH/g；The newton body sulfoacid calcium is stone Oily sulfoacid calcium and/or calcium alkylbenzenesulfonate, the total base number of the newton body sulfoacid calcium are 250-450mgKOH/g；The newton body ring Alkanoic acid calcium is petroleum naphthenic acid calcium and/or synthesis calcium naphthenate, and the total base number of the newton body calcium naphthenate is 250- 450mgKOH/g；The newton body calcium salicylate is salicylate calcium, and the total base number of the newton body calcium salicylate is 250- 450mgKOH/g；The newton body calcium oleate is natural calcium oleate and/or synthesis calcium oleate, the total alkali of the newton body calcium oleate Value is 250-450mgKOH/g.
15. preparation method according to claim 9 or 10, wherein the transforming agent is selected from fatty alcohol, fatty acid, fat Ketone, fatty aldehyde, fatty amine, ether, calcium carbonate, boric acid, phosphonic acids, carbon dioxide, phenol, aromatic alcohol, aromatic amine, aphthenic acids, C8- At least one of C20 alkyl benzene sulphonate, C16-C24 alkyl phenol and water, the additional amount of transforming agent are that the high base number material is total The 2-30% of weight.
16. preparation method according to claim 15, wherein the transforming agent be selected from dodecyl benzene sulfonic acid, aphthenic acids, At least one of octadecyl phenol, methanol, isopropanol, butanol, boric acid, acetic acid and water, the additional amount of transforming agent are the height The 6-22% of base number material total weight.
17. preparation method according to claim 9 or 10, wherein the structural formula of the monoamine is R1–NH2、R4–NH2, In, R1、R4It is phenyl or C1–C3The alkyl or cycloalkyl that the phenyl or carbon number that alkyl or halogen replace are 10-18.
18. preparation method according to claim 17, wherein the monoamine is selected from aniline, m-chloroaniline, parachloroanilinum And/or para-totuidine aromatic amine and/or fatty amine selected from lauryl amine, tetradecy lamine, cetylamine and/or octadecylamine.
19. preparation method according to claim 9 or 10, wherein the structural formula of the diamines is NH2–R2–NH2, wherein R2It is the alkylidene or phenylene or biphenylene that carbon number is 2-8.
20. preparation method according to claim 19, wherein the diamines is to be selected from p-phenylenediamine, o-phenylenediamine, 4, The aromatic amine of 4 '-benzidines and/or selected from ethylenediamine, propane diamine, 1,6-hexamethylene diamines straight-chain fatty amine.
21. preparation method according to claim 9 or 10, wherein the structure of the diisocyanate is OCN-R3- NCO, R3It is arlydene, alkylidene or the cycloalkylidene that carbon number is 6-30.
22. preparation method according to claim 21, wherein the diisocyanate is selected from toluene di-isocyanate(TDI), two Methylenebis phenyl isocyanate, six hexylidene diisocyanates, dicyclohexyl methyl hydride diisocyanate and xyxylene two are different At least one of cyanate.
23. lubricant composition made from the method as described in any one of claim 9-22.
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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4181619A (en) * 1978-10-30 1980-01-01 Mobil Oil Corporation Antiwear composition
WO2002012418A3 (en) * 2000-08-10 2002-04-25 Shell Int Research Grease composition with improved rust prevention and abrasion resistance properties
CN101117604A (en) * 2006-07-31 2008-02-06 中国石油化工股份有限公司 Lubricating grease composition
CN101550095A (en) * 2009-05-26 2009-10-07 辽宁渤大化工有限公司 Method for preparing overbased synthesized heavy alkyl benzene calcium sulfonate

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4181619A (en) * 1978-10-30 1980-01-01 Mobil Oil Corporation Antiwear composition
WO2002012418A3 (en) * 2000-08-10 2002-04-25 Shell Int Research Grease composition with improved rust prevention and abrasion resistance properties
CN101117604A (en) * 2006-07-31 2008-02-06 中国石油化工股份有限公司 Lubricating grease composition
CN101550095A (en) * 2009-05-26 2009-10-07 辽宁渤大化工有限公司 Method for preparing overbased synthesized heavy alkyl benzene calcium sulfonate

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