CN106032479A - Lubricating grease composition and preparation method thereof - Google Patents
Lubricating grease composition and preparation method thereof Download PDFInfo
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- CN106032479A CN106032479A CN201510105597.0A CN201510105597A CN106032479A CN 106032479 A CN106032479 A CN 106032479A CN 201510105597 A CN201510105597 A CN 201510105597A CN 106032479 A CN106032479 A CN 106032479A
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Abstract
A lubricating grease composition and a preparation method thereof are disclosed. The invention relates to the field of lubricating grease, and discloses a lubricating grease composition. The lubricating grease composition comprises base oil (10-80 wt%) and a thickening agent, which comprises non-Newton fluid sulfurized calcium alkyl phenate-calcium sulfonate (10-70 wt%), and calcium salts of higher fatty acid (1-20 wt%), and also optionally comprises one or more of non-Newton fluid calcium naphthenate (0-70 wt%), non-Newton fluid calcium salicylate (0-70 wt%), non-Newton fluid calcium oleate (0-70 wt%), calcium salts of aromatic acid (0-15 wt%), and calcium salts of micro-molecular inorganic acid and/or lower fatty acid (0-15 wt%). The invention also discloses a preparation method of the lubricating grease composition. The provided lubricating grease composition has excellent performances.
Description
Technical field
The present invention relates to a kind of lubricant composition and preparation method thereof.
Background technology
SULFURIZED CALCIUM ALKYL PHENATE WITH HIGH BASE NUMBER has preferable detergent-dispersant performance, good acid neutralization capacity and excellence
Diffusibility, be used as the detersive of lubricating oil, be widely used in modulation medium and high classes I. C. engine oil,
It is particularly suited for pressurized diesel engine oil to reduce the carbon deposit of top land and the additive of marine cylinder oil, its
Technology development mainly makes its high alkalization, it is simply that the calcium carbonate calcium sulfenyl phenolate with surface activity
It is distributed in flux oil become a kind of colloidal dispersion system.SULFURIZED CALCIUM ALKYL PHENATE WITH HIGH BASE NUMBER is alkyl phenol warp
React with CaO, vulcanize, carbonating contour alkalization technology and obtain, the Patents about preparation has CN
200810011927 etc..
Utilize calcium sulfonate with high base number for raw material production grease, because of its have excellence antirust and anticorrosion
Property, since putting goods on the market, cause the extensive concern of domestic and international grease industry, but, although high-alkali
Value complex calcium sulfonate grease has the most excellent antirust and anticorrosive property, but easy in storage process
Harden, and the high price of its raw materials for production calcium sulfonate with high base number and complicated preparation technology itself cause it
Do not promoted rapidly, meanwhile, along with people are more and more higher to the requirement of environmental conservation, sulfonate with high base number
In calcium production process must through sulfonation process the pollution of environment is also increasingly subject to the concern of people.Find one
Plant antirust and anticorrosive property is similar with high base number composite calcium sulfonate base grease but can alleviate the problems referred to above
Grease become the big problem that people face at present.
Summary of the invention
It is an object of the invention to provide one have the most antirust and anticorrosive property, storage good security and
Grease that its feed preparation process is simple and environmentally-friendly and preparation method thereof.
The present inventor finds under study for action, and calcium sulfenyl phenolate is due to containing active sulfur, at high temperature
Under easily may separate out elemental sulfur and produce corrosion, therefore, when as detersive, calcium sulfenyl phenolate
Antirust and anticorrosive property far below sulfoacid calcium, but calcium sulfenyl phenolate is prepared grease as thickening agent
Time, but can obtain and anticorrosion the most antirust with high base number composite calcium sulfonate base grease
Property, and storage good security.
Therefore, to achieve these goals, on the one hand, the invention provides a kind of lubricant composition,
Described lubricant composition contains base oil and thickening agent, and described thickening agent contains non-newtonian fluid alkyl monosulfide
Phenol calcium sulfoacid calcium and the calcium salt of higher fatty acids, described thickening agent is also optionally with non-newtonian fluid cycloalkanes
Acid calcium, non-newtonian fluid calcium salicylate, non-newtonian fluid calcium oleate, the calcium salt of aromatic acid, little molecule mineral acid and
/ or the calcium salt of lower fatty acid in one or more, on the basis of the weight of described lubricant composition,
The content of base oil is 10 80 weight %, and the content of non-newtonian fluid calcium sulfenyl phenolate sulfoacid calcium is
10 70 weight %, the content of the calcium salt of higher fatty acids is 1 20 weight %, non-newtonian fluid calcium naphthenate
Content be 0-70 weight %, the content of non-newtonian fluid calcium salicylate is 0-70 weight %, non-newtonian fluid
The content of calcium oleate is 0-70 weight %, and the content of the calcium salt of aromatic acid is 0-15 weight %, little molecule without
The content of the calcium salt of machine acid and/or lower fatty acid is 0 15 weight %.
Preferably, on the basis of lubricant composition weight, the content of base oil is 20 70 weight %,
The content of non-newtonian fluid calcium sulfenyl phenolate sulfoacid calcium is 20 65 weight %, the calcium salt of higher fatty acids
Content be 2 15 weight %, the content of non-newtonian fluid calcium naphthenate is 0-50 weight %, non-newtonian fluid
The content of calcium salicylate is 0-50 weight %, and the content of non-newtonian fluid calcium oleate is 0-50 weight %, virtue
The content of the calcium salt of acid is 2-10 weight %, containing of the calcium salt of little molecule mineral acid and/or lower fatty acid
Amount is 2 10 weight %.
Second aspect, the invention provides the preparation method of lubricant composition as above, the method
Including: by thickening agent and part basis oil mix homogeneously, refine at 180 230 DEG C of constant temperature, add surplus
Base oil, adds necessary additive, obtains finished product, and described thickening agent contains non-newtonian fluid alkyl monosulfide
Phenol calcium sulfoacid calcium and the calcium salt of higher fatty acids, described thickening agent is also optionally with non-newtonian fluid cycloalkanes
Acid calcium, non-newtonian fluid calcium salicylate, non-newtonian fluid calcium oleate, the calcium salt of aromatic acid, little molecule mineral acid and
/ or the calcium salt of lower fatty acid in one or more.
The third aspect, the invention provides the preparation method of a kind of lubricant composition, and the method includes:
(1) containing newton body calcium sulfenyl phenolate, newton body and/or non-newtonian fluid sulfoacid calcium, or will contain
There are newton body and/or non-newtonian fluid calcium sulfenyl phenolate, the high base number material of newton body sulfoacid calcium, and part
Base oil mixes, and obtains mixture, and described high base number material is also optionally with newton body and/or non newtonian
Body calcium naphthenate, newton body and/or non-newtonian fluid calcium salicylate and newton body and/or non-newtonian fluid calcium oleate
In one or more；
(2) optionally carry out the reaction of at least part of composite calcium: add Calx or calcium hydroxide, add
Higher fatty acids, optional aromatic acid, optional little molecule mineral acid and/or lower fatty acid, react；
(3) add transforming agent, heat up and treat material retrogradation；
(4) carry out remaining the reaction of composite calcium；
(5) heat up dehydration；
(6) it is warmed up to 180 230 DEG C of constant temperature refinings, adds surplus base oil, add necessary additive,
Obtain finished product.
Preferably, in step (2), the reaction of at least part of composite calcium is carried out.
Fourth aspect, the invention provides the lubricant composition prepared by method as above.
The lubricant composition of the present invention, has the most excellent with complex calcium sulfonate grease
Antirust and anticorrosive property, and there is excellent storage stability, also have and be better than Composite calcium-sulfonate-batetrapolyurea lubrication
The viscous resistance of fat, mechanical stability, water-resistance, colloid stability, abrasion resistance and extreme pressure anti-wear,
And also there is the performances such as excellent heat-resisting quantity.The feed preparation process of the grease of the present invention is simple, ring
Protect, constant product quality.
Other features and advantages of the present invention will be described in detail in detailed description of the invention part subsequently.
Accompanying drawing explanation
Fig. 1 is the overbased calcium sulfenyl phenolate raw material of embodiment 2 and infrared point of grease prepared
Analysis spectrogram contrast.
Detailed description of the invention
Hereinafter the detailed description of the invention of the present invention is described in detail.It should be appreciated that this place is retouched
The detailed description of the invention stated is merely to illustrate and explains the present invention, is not limited to the present invention.
The invention provides a kind of lubricant composition, this lubricant composition have employed calcium mahogany sulfonate
And/or calcium alkylbenzenesulfonate, synthesis calcium sulfenyl phenolate, optional petroleum naphthenic acid calcium and/or synthesis cycloalkanes
Acid calcium, optional salicylate calcium, optional natural calcium oleate and/or synthesis calcium oleate are raw material, with
Shi Hanyou composite calcium thickening agent.
Present invention also offers the preparation method of foregoing grease composition.
On the one hand, the invention provides a kind of lubricant composition, lubricant composition contain base oil and
Thickening agent, thickening agent contains non-newtonian fluid calcium sulfenyl phenolate sulfoacid calcium and the calcium salt of higher fatty acids,
Thickening agent is also optionally with non-newtonian fluid calcium naphthenate, non-newtonian fluid calcium salicylate, non-newtonian fluid oleic acid
One or more in the calcium salt of calcium, the calcium salt of aromatic acid, little molecule mineral acid and/or lower fatty acid, with
On the basis of the weight of lubricant composition, the content of base oil is 10 80 weight %, and non-newtonian fluid vulcanizes
The content of alkyl phenol calcium sulfoacid calcium is 10 70 weight %, and the content of the calcium salt of higher fatty acids is 1 20
Weight %, the content of non-newtonian fluid calcium naphthenate is 0-70 weight %, the content of non-newtonian fluid calcium salicylate
For 0-70 weight %, the content of non-newtonian fluid calcium oleate is 0-70 weight %, the content of the calcium salt of aromatic acid
For 0-15 weight %, the content of the calcium salt of little molecule mineral acid and/or lower fatty acid is 0 15 weight %.
Preferably, on the basis of lubricant composition weight, the content of base oil is 20 70 weight %,
The content of non-newtonian fluid calcium sulfenyl phenolate sulfoacid calcium is 20 65 weight %, the calcium salt of higher fatty acids
Content be 2 15 weight %, the content of non-newtonian fluid calcium naphthenate is 0-50 weight %, non-newtonian fluid
The content of calcium salicylate is 0-50 weight %, and the content of non-newtonian fluid calcium oleate is 0-50 weight %, virtue
The content of the calcium salt of acid is 2-10 weight %, containing of the calcium salt of little molecule mineral acid and/or lower fatty acid
Amount is 2 10 weight %.
In the present invention, " optionally with " refer to can not contain this component containing this component,
That is, non-newtonian fluid calcium naphthenate, non-newtonian fluid calcium salicylate, non-newtonian fluid calcium oleate, the calcium salt of aromatic acid,
One or more in the calcium salt of little molecule mineral acid and/or lower fatty acid are optional components, the present invention's
Lubricant composition can include this component, it is also possible to do not include this component.
Non-newtonian fluid calcium sulfenyl phenolate sulfoacid calcium, non-newtonian fluid calcium naphthenate, non-newtonian fluid salicylic acid
Calcium, non-newtonian fluid calcium oleate or a combination thereof thing are at infrared spectrum 873cm–1–886cm–1There is crystal formation carbon in place
Acid calcium characteristic absorption peak.Non-newtonian fluid calcium sulfenyl phenolate sulfoacid calcium is by newton body sulfoacid calcium and newton
Body calcium sulfenyl phenolate is converted by transforming agent and obtains, non-newtonian fluid calcium sulfenyl phenolate sulfoacid calcium total
Base number is 250 450mgKOH/g, preferably 300 400mgKOH/g；Non-newtonian fluid calcium naphthenate is
Being obtained by the conversion of newton body calcium naphthenate, the total base number of non-newtonian fluid calcium naphthenate is
250-450mgKOH/g, preferably 300-400mgKOH/g；Non-newtonian fluid calcium salicylate is by newton
The conversion of body calcium salicylate obtains, and the total base number of non-newtonian fluid calcium salicylate is 250-450mgKOH/g,
It is preferably 300-400mgKOH/g；Non-newtonian fluid calcium oleate is converted by newton body calcium oleate and obtains,
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 calcium sulfenyl phenolate, newton body calcium naphthenate, newton body calcium salicylate,
Containing unformed calcium carbonate in newton body calcium oleate, at infrared spectrum 860cm–1–865cm–1There is nothing in place
Sizing calcium carbonate characteristic absorption peak.Newton body calcium sulfenyl phenolate is synthesis calcium sulfenyl phenolate, its total alkali
Value is 250-450mgKOH/g, preferably 300-400mgKOH/g；Newton body sulfoacid calcium is oil sulphur
Acid calcium and/or calcium alkylbenzenesulfonate, its total base number is 250-450mgKOH/g, is preferably
300-400mgKOH/g；Newton body calcium naphthenate is petroleum naphthenic acid calcium and/or synthesis calcium naphthenate, its
Total base number is 250-450mgKOH/g, preferably 300-400mgKOH/g；Newton body calcium salicylate is
Salicylate calcium, its total base number is 250-450mgKOH/g, preferably 300-400mgKOH/g；
Newton body calcium oleate is natural calcium oleate and/or synthesis calcium oleate, and its total base number is
250-450mgKOH/g, preferably 300-400mgKOH/g.Non-newtonian fluid calcium sulfenyl phenolate sulphur
Acid calcium, non-newtonian fluid calcium naphthenate, non-newtonian fluid calcium salicylate and the base number of non-newtonian fluid calcium oleate mixing
Weight meansigma methods for the base number of each component.
In the present invention, higher fatty acids be carbon number be fatty acid or the hydroxyl fat of 8-20, preferably 10-18
Fat acid, such as in lauric acid, Palmic acid, stearic acid, 12-hydroxy stearic acid, eicosyl carboxylic acid
At least one, preferably 12-hydroxy stearic acid.
In the present invention, aromatic acid is the carboxylic acid that at least 1 carboxyl is joined directly together with aromatic ring, and aromatic acid can be
Substituted or unsubstituted aromatic acid, its substituent group can be alkyl, thiazolinyl, alkynyl, aryl, halo or
At least one in the alkyl or aryl of perhalogeno etc., the molecular weight of aromatic acid is preferably smaller than equal to 550.Virtue
Acid is preferably binary aromatic acid, for example, it is possible to selected from the unsubstituted or substituted adjacent benzene two of C1-C5 alkyl
At least one in formic acid, M-phthalic acid, p-phthalic acid, biphenyl dicarboxylic acid, polyphenyls dioctyl phthalate.
It is preferably phthalic acid, M-phthalic acid, p-phthalic acid, biphenyl dicarboxylic acid, and methyl replaces
Biphenyl dicarboxylic acid, at least one in polyphenyls dioctyl phthalate etc..
In the present invention, the molecular weight of little molecule mineral acid and lower fatty acid is less than or equal to 250.Wherein,
Little molecule mineral acid can be selected from least one in boric acid, phosphoric acid, sulphuric acid etc., preferably boric acid and/
Or phosphoric acid；Lower fatty acid can be selected from acetic acid, ethanedioic acid, propanoic acid, malonic acid, butanoic acid, succinic acid
At least one in Deng, preferably acetic acid.
In the present invention, base oil can be mineral oil, artificial oil, vegetable oil or their mixture, 100 DEG C
Dynamic viscosity is 4 60mm2/ s, preferably 10 30mm2/s.Artificial oil can be poly-a-olefin oil (PAO),
Esters oil, alkyl-silicone oil, Fischer-Tropsch synthesis oil etc..
The lubricant composition of the present invention can also contain various additives, such as antioxidant, extreme-pressure anti-wear
Agent, antirust agent etc..Wherein, antioxidant preferred arylamine kind antioxidant, account for grease gross weight
0.01-5%, preferably 0.1-2.5%, can be diphenylamines, phenyl-a-naphthylamine and di-iso-octyldiphenylamine
In at least one, preferably di-iso-octyldiphenylamine.Extreme pressure anti-wear additives accounts for grease gross weight
0.5-12%, preferably 0.8-8%, can be dithio Acidic phosphates zinc, dithio dialkyl amido first
Acid molybdenum, dithio dialkyl amido lead formate, triphenylphosphorothionate, organic molybdenum complex compound, sulfuration
Alkene, molybdenum bisuphide, politef, D2EHDTPA molybdenum, chlorinated paraffin, dibutyl dithio amino
At least one in formic acid antimony, tungsten disulfide, selenium sulfide, fluorographite, calcium carbonate and zinc oxide；
Antirust agent accounts for the 0.01-4.5% of grease gross weight, preferably 0.1-2%, can be barium mahogany sulfonate, stone
At least one in oil sodium sulfonate, benzothiazole, benzotriazole, zinc naphthenate and alkenyl succinic acid.
Second aspect, the invention provides the preparation method of lubricant composition as above, the method
Including: by thickening agent and part basis oil mix homogeneously, refine at 180 230 DEG C of constant temperature, add surplus
Base oil, adds necessary additive, obtains finished product, it is characterised in that described thickening agent contains non-cattle
Body calcium sulfenyl phenolate sulfoacid calcium and the calcium salt of higher fatty acids, described thickening agent also optionally with
Non-newtonian fluid calcium naphthenate, non-newtonian fluid calcium salicylate, non-newtonian fluid calcium oleate, the calcium salt of aromatic acid, little
One or more in the calcium salt of molecule mineral acid and/or lower fatty acid.
In the present invention, " optionally with " as it was previously stated, do not repeat them here.
In the present invention, non-newtonian fluid calcium sulfenyl phenolate sulfoacid calcium, the calcium salt of higher fatty acids, non-cattle
Pause body calcium naphthenate, non-newtonian fluid calcium salicylate, non-newtonian fluid calcium oleate, the calcium salt of aromatic acid, little molecule
Mineral acid and/or the calcium salt of lower fatty acid, base oil and additive be not as it was previously stated, repeat them here.
It will be understood by those skilled in the art that the amount of part basis oil and the amount sum of surplus base oil
Being the total amount of base oil used, in the present invention, part basis oil is excellent with the weight ratio of surplus base oil
Elect 1:0.1-5 as.
For non-newtonian fluid calcium sulfenyl phenolate sulfoacid calcium, non-newtonian fluid calcium naphthenate, non-newtonian fluid water
Poplar acid calcium, non-newtonian fluid calcium oleate or a combination thereof thing, can be by newton body calcium sulfenyl phenolate, Niu Dunti
Sulfoacid calcium, newton body calcium naphthenate, newton body calcium salicylate, newton body calcium oleate or a combination thereof thing are respectively
Converted by transforming agent and obtain, such as, by newton body calcium sulfenyl phenolate, newton body sulfoacid calcium, optionally
Newton body calcium naphthenate, optional newton body calcium salicylate, optional newton body calcium oleate and base oil
Hybrid Heating to 50-80 DEG C, the transforming agent needed for addition reacts, after all transforming agents add,
80-100 DEG C of constant temperature 60-90 minute, then heats to 110-130 DEG C of dehydration.
In the present invention, " optional " refer to have this raw material can also not this raw material, such as, " appoint
The newton body calcium naphthenate of choosing " i.e. refer to there is newton this raw material of body calcium naphthenate, it is also possible to do not have
This raw material of newton body calcium naphthenate.
The third aspect, the invention provides the preparation method of a kind of lubricant composition, it is characterised in that
The method includes:
(1) containing newton body calcium sulfenyl phenolate, newton body and/or non-newtonian fluid sulfoacid calcium, or will contain
There are newton body and/or non-newtonian fluid calcium sulfenyl phenolate, the high base number material of newton body sulfoacid calcium, and part
Base oil mixes, and obtains mixture, and described high base number material is also optionally with newton body and/or non newtonian
Body calcium naphthenate, newton body and/or non-newtonian fluid calcium salicylate and newton body and/or non-newtonian fluid calcium oleate
In one or more；
(2) optionally carry out the reaction of at least part of composite calcium: add Calx or calcium hydroxide, add
Higher fatty acids, optional aromatic acid, optional little molecule mineral acid and/or lower fatty acid, react；
(3) add transforming agent, heat up and treat material retrogradation；
(4) carry out remaining the reaction of composite calcium；
(5) heat up dehydration；
(6) it is warmed up to 180 230 DEG C of constant temperature refinings, adds surplus base oil, add necessary additive,
Obtain finished product.
" optionally with " as it was previously stated, do not repeat them here.
In the present invention, newton body calcium sulfenyl phenolate, non-newtonian fluid calcium sulfenyl phenolate, newton body sulfonic acid
Calcium, non-newtonian fluid sulfoacid calcium, newton body calcium naphthenate, non-newtonian fluid calcium naphthenate, newton body salicylic acid
Calcium, non-newtonian fluid calcium salicylate, newton body calcium oleate, non-newtonian fluid calcium oleate, higher fatty acids, virtue
Molecule mineral acid sour, little, lower fatty acid and base oil be not as it was previously stated, repeat them here.
In step of the present invention (1), " containing newton body calcium sulfenyl phenolate, newton body and/or non newtonian
Body sulfoacid calcium, or containing newton body and/or non-newtonian fluid calcium sulfenyl phenolate, newton body sulfoacid calcium high-alkali
Value material " i.e. refer to the calcium sulfenyl phenolate in high base number material and sulfoacid calcium at least one be newton body
Type.
In step of the present invention (1), for the weight ratio of sulfoacid calcium and calcium sulfenyl phenolate without particular/special requirement,
It is preferably 1:0.25 4.For the amount of other optional high base number materials without particular/special requirement, can basis
Being actually needed the amount commonly used in the art that uses, high base number material gross weight is excellent with the weight ratio of part basis oil
Elect 1:0.1 3 as.
In step of the present invention (2), " optionally carrying out the reaction of at least part of composite calcium " i.e. includes three kinds
Situation: (i) does not carry out the reaction of composite calcium, i.e. do not have step (2), only carry out in step (4)
The reaction of whole composite calciums, is i.e. equivalent to the inventive method and is initially charged transforming agent and converts, after conversion
Carry out the reaction of composite calcium again；(ii) carry out the reaction of part composite calcium, i.e. carry out in step (2)
The reaction of part composite calcium, carries out remaining the reaction of composite calcium in step (4) again, is i.e. equivalent to this
Inventive method carries out the reaction of part composite calcium before conversion, carries out the anti-of part composite calcium the most again
Should；(iii) carry out the reaction of whole composite calcium, i.e. in step (2), carry out the anti-of whole composite calciums
Should, do not carry out step (4), be i.e. equivalent to the inventive method and first carry out the reaction of composite calcium, then carry out turning
Change.
This area, when preparing grease, is generally individually to be initially charged transforming agent to convert, then is combined
The reaction of calcium, during as prepared complex calcium sulfonate grease.But the present inventor finds under study for action,
The method carrying out the present invention according to above-mentioned situation (ii) or (iii), carries out this than according to situation (i)
Bright method, the most first carries out all or part of composite calcium reaction, then converts, it is possible to further
Improve the performance of the grease prepared.This reaction being likely due to first carry out composite calcium, it is possible to preferably
Newton body calcium sulfenyl phenolate by oily is converted into the non-newtonian fluid calcium sulfenyl phenolate of smectic.Therefore,
Preferably, in step (2), the reaction of at least part of composite calcium is carried out.
When carrying out step (2) and step (4), it is preferable that at 85-100 DEG C, add Calx
Or the suspension of calcium hydroxide, add higher fatty acids, stir 5-20 minute, add optional aromatic acid,
Optional little molecule mineral acid and/or lower fatty acid, stir 5-20 minute.Wherein, higher fatty acids
Can exchange with the addition sequence of aromatic acid, little molecule mineral acid and/or lower fatty acid.
In the present invention, higher fatty acids and optional aromatic acid and optional little molecule mineral acid and/or low
The H of level fatty acid+The amount of total material and Calx or the OH contained by suspension of calcium hydroxide-Total material
Measure equal, OH-Amount also can excess 1-10%.
In the present invention, in terms of calcium hydroxide, the addition of the suspension of Calx or calcium hydroxide is preferably height
The 1-15% of base number material gross weight；With H+The gauge of material, higher fatty acids and optional aromatic acid
It is preferably 1:1-10 with the mol ratio of optional little molecule mineral acid and/or lower fatty acid.
In the present invention, the suspension of Calx or calcium hydroxide i.e. refers to that Calx or calcium hydroxide are formed in water
Suspension, the solid content of suspension is preferably 10-60 weight %.
In step of the present invention (3), it is preferable that at 50 80 DEG C, preferably constant temperature 10 30 minutes, adds
Enter required transforming agent to react, preferably add and stir 8 12 minutes after every kind of transforming agent, all turns
After agent adds, 80 100 DEG C of constant temperature 60 90 minutes.
Described transforming agent be preferably selected from fatty alcohol, fatty acid, aliphatic ketone, fatty aldehyde, fatty amine, ether,
Calcium carbonate, boric acid, phosphonic acids, carbon dioxide, phenol, aromatic alcohol, aromatic amine, aphthenic acids, C8 C20
At least one in alkyl benzene sulphonate, C16-C24 alkyl phenol and water；It is more preferably selected from the fat of C1 C5
Fat alcohol, the fatty acid of C1 C5, the aliphatic ketone of C1 C5, the fatty aldehyde of C1 C5, the fat of C1 C5
Fat amine, the ether of C1 C5, boric acid, the alkyl phosphonic acid of C1 C10, the di alkyl phosphonic acid of C2 C16,
The arylphosphonic acid of C6 C20, the diaryl phosphonic acids of C12 C24, the aromatic alcohol of C7 C20, C7 C20
Aromatic amine, C8 C20 alkyl benzene sulphonate, aphthenic acids, C16-C22 alkyl phenol and water at least one
Kind；Further it is preferably selected from DBSA, aphthenic acids, octadecyl phenol, methanol, isopropyl
At least one in alcohol, butanol, boric acid, acetic acid and water.The addition of transforming agent is preferably high base number thing
The 2 30% of material gross weight, more preferably the 6 22% of high base number material gross weight.
In the present invention, fatty alcohol includes straight chain, side chain and ring-type fatty alcohol, fatty acid, aliphatic ketone,
Fatty aldehyde, fatty amine are in like manner.
In step of the present invention (5), it is preferable that be warming up to 110-130 DEG C, 30-60 is preferably kept to divide
Clock is to realize dehydration.
In step of the present invention (6), it is preferable that be warmed up to 180 230 DEG C of constant temperature 5 30 minutes；Add
Surplus base oil, treats that temperature is cooled to 100 120 DEG C, adds necessary additive, stirring, is circulated throughout
Filter, homogenizing, degassing.
In the present invention, base oil used by step (1) is the weight ratio of base oil used with step (6)
It is preferably 1:0.1-5.
Fourth aspect, the profit that the preparation method that present invention also offers is provided by third aspect present invention prepares
Grease composition.
Compared with the lubricant composition that the preparation method provided by second aspect prepares, the third aspect provides
Preparation method prepare lubricant composition have more preferable viscous resistance, mechanical stability, water-resistance,
Colloid stability, abrasion resistance and extreme pressure anti-wear.
Embodiment
The present invention is further illustrated for below example, but and is not so limited the present invention.
In the following Examples and Comparative Examples:
Non-newtonian fluid alkyl monosulfide calcium phenolsulfonate in the lubricant composition prepared, non-newtonian fluid cycloalkanes
The total content of acid calcium, non-newtonian fluid calcium salicylate and non-newtonian fluid calcium oleate all uses non-newtonian fluid alkyl monosulfide
Phenol calcium sulfoacid calcium % represents, i.e.
Non-newtonian fluid calcium sulfenyl phenolate sulfoacid calcium %=(overbased or calcium sulfonate with high base number raw material weight
Amount+overbased 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 gross weight)/grease gross weight × 100%.Transforming agent all counts non-newtonian fluid sulfur
Change in the content of alkyl phenol calcium sulfoacid calcium.
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.
It is limited that overbased and overbased calcium alkyl-salicylate raw material is purchased from Xinjiang Lander Speciality Petrochemicals share
Company.
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.
High base number calcium oleate is prepared according to document (NLGI Spokeman, 2009,73 (2): 1 17) method.
Embodiment 1
The present embodiment is for illustrating lubricant composition prepared by the present invention.
Raw material components: overbased sulfoacid calcium (total base number is 400mgKOH/g, 24kg)；Superelevation alkali
Value calcium sulfenyl phenolate (total base number is 400mgKOH/g, 6kg)；HVI150BS lubricating base oil (100
DEG C kinematic viscosity is 31mm2/ s, 30kg)；4-octadecylphenol (2.8kg)；Acetic acid (0.56kg)；
Calcium hydroxide (1.8kg)；12-hydroxy stearic acid (2kg)；P-phthalic acid (3.5kg)；HVI500SN
(100 DEG C of kinematic viscositys are 11mm to lubricating base oil2/ s, 17kg).
A volume be 160L and with the normal-pressure reaction kettle heating, stirring, circulate, cool down in add
Entering 24kg total base number is that the overbased sulfoacid calcium of 400mgKOH/g, 6kg total base number are
The overbased calcium sulfenyl phenolate of 400mgKOH/g and the HVI150BS lubricating base oil of 30kg,
Stirring, is warmed up to 95 DEG C, adds the calcium hydroxide suspension 9kg that solid content is 20 weight %, stirring
10 minutes；Add 2kg 12-hydroxy stearic acid, stir 10 minutes；Add 3.5kg p-phthalic acid,
Stir 10 minutes；Add the HVI500SN lubricating base oil of 10kg and make material be down to 50 DEG C, permanent
Temperature 30 minutes, adds 2.8kg 4-octadecylphenol, and temperature controls at 50 DEG C, stirs 10 minutes,
Add the aqueous acetic acid that 2.8kg concentration is 20 weight %, stir 10 minutes, be warmed up to 80 DEG C, permanent
Temperature 90 minutes, material retrogradation；It is warmed up to 120 DEG C under stirring, keeps 45 minutes, dehydration；It is warmed up to
200 DEG C of constant temperature 10 minutes.Then, it is cooled to 160 DEG C, adds remaining HVI500SN lubrication base
Oil；Treating that temperature is cooled to 110 DEG C, circulating filtration, homogenizing, degassing obtain finished product.Assay is shown in Table
1。
In the grease that the present embodiment obtains, on the basis of grease weight, consist of: non-newtonian fluid sulfur
Change alkyl phenol calcium sulfoacid calcium 38.4 weight %；Lubricating base oil 54.2 weight %；12-hydroxy stearic acid
Calcium 2.4 weight %；P-phthalic acid calcium 5.0 weight %.
Embodiment 2
The present embodiment is for illustrating lubricant composition prepared by the present invention.
Raw material components: overbased sulfoacid calcium (total base number is 420mgKOH/g, 6kg)；Overbased
Calcium sulfenyl phenolate (total base number is 420mgKOH/g, 24kg)；HVI150BS lubricating base oil (100
DEG C kinematic viscosity is 31mm2/ s, 30kg)；4-octadecylphenol (1.8kg)；Acetic acid (0.56kg)；
Boric acid (1kg)；Calcium hydroxide (1.8kg)；12-hydroxy stearic acid (2kg)；Phthalic acid (3.5kg)；
(100 DEG C of kinematic viscositys are 11mm to HVI500SN lubricating base oil2/ s, 17kg).
A volume be 160L and with the normal-pressure reaction kettle heating, stirring, circulate, cool down in add
Entering 6kg total base number is that the overbased sulfoacid calcium of 420mgKOH/g, 24kg total base number are
The overbased calcium sulfenyl phenolate of 420mgKOH/g and the HVI150BS lubricating base oil of 30kg,
Stirring, is warmed up to 85 DEG C, adds the calcium hydroxide suspension 0.9kg that solid content is 20 weight %, stirring
10 minutes；Add 0.2kg 12-hydroxy stearic acid, stir 10 minutes；Add 0.35kg phthalic acid,
Stir 10 minutes；At 80 DEG C, constant temperature 10 minutes, add 1.8kg 4-octadecylphenol, temperature control
System, at 80 DEG C, stirs 10 minutes, adds the aqueous acetic acid that 2.8kg concentration is 20 weight %, stirring
10 minutes, add the boric acid aqueous solution that 5kg concentration is 20 weight %, stir 10 minutes, be warmed up to
90 DEG C, constant temperature 60 minutes, material retrogradation；At 85 DEG C, add the hydrogen-oxygen that solid content is 20 weight %
Change calcium suspension 8.1kg, stir 10 minutes, add 1.8kg 12-hydroxy stearic acid, stir 10 minutes,
Add 3.15kg phthalic acid, stir 10 minutes；It is warmed up to 110 DEG C under stirring, keeps 60 minutes,
Dehydration；It is warmed up to 230 DEG C of constant temperature 5 minutes.Then, the HVI500SN lubrication base of 17kg is added
Oil；Treating that temperature is cooled to 120 DEG C, circulating filtration, homogenizing, degassing obtain finished product.Assay is shown in Table
1.Fig. 1 is shown in the infrared analysis spectrogram contrast of overbased calcium sulfenyl phenolate raw material and prepared grease.
In the grease that the present embodiment obtains, on the basis of grease weight, consist of: non-newtonian fluid sulfur
Change alkyl phenol calcium sulfoacid calcium 38.4 weight %；Lubricating base oil 54.2 weight %；12-hydroxy stearic acid
Calcium 2.4 weight %；Calcium phthalate 5.0 weight %.
Embodiment 3
The present embodiment is for illustrating lubricant composition prepared by the present invention.
Raw material components: overbased sulfoacid calcium (total base number is 400mgKOH/g, 24kg)；High base number
Calcium sulfenyl phenolate (total base number is 320mgKOH/g, 6kg)；HVI150BS lubricating base oil (100
DEG C kinematic viscosity is 31mm2/ s, 20kg)；4-octadecylphenol (1kg)；Butanol (0.8kg)；
Acetic acid (0.56kg)；Boric acid (1kg)；Calcium hydroxide (1.8kg)；Stearic acid (1.9kg)；Isophthalic two
Formic acid (3.5kg)；(100 DEG C of kinematic viscositys are 11mm to HVI500SN lubricating base oil2/ s, 28kg).
A volume be 160L and with the normal-pressure reaction kettle heating, stirring, circulate, cool down in add
Entering 24kg total base number is that the overbased sulfoacid calcium of 400mgKOH/g, 6kg total base number are
The SULFURIZED CALCIUM ALKYL PHENATE WITH HIGH BASE NUMBER of 320mgKOH/g and the HVI150BS lubricating base oil of 20kg, stir
Mix, be warmed up to 90 DEG C, add the calcium hydroxide suspension 9kg that solid content is 20 weight %, stir 10
Minute, add 1.9kg stearic acid, stir 10 minutes, add 3.5kg M-phthalic acid, stir 10
Minute；Add the HVI500SN lubricating base oil of 15kg and make material be down to 65 DEG C, constant temperature 10 points
Clock, adds 1kg 4-octadecylphenol and 0.8kg butanol, and temperature controls at about 65 DEG C, stirs 10
Minute, add the aqueous acetic acid that 2.8kg concentration is 20 weight %, stir 10 minutes, add 5kg
Concentration is the boric acid aqueous solution of 20 weight %, stirs 10 minutes, is warmed up to 100 DEG C, constant temperature 70 minutes,
Material retrogradation；It is warmed up to 130 DEG C under stirring, keeps 30 minutes, dehydration；It is warmed up to 180 DEG C of constant temperature 20
Minute.Then, remaining HVI500SN lubricating base oil is added；Treat that temperature is cooled to 100 DEG C, follow
Ring filtration, homogenizing, degassing obtain finished product.Assay is shown in Table 1.
In the grease that the present embodiment obtains, on the basis of grease weight, consist of: non-newtonian fluid sulfur
Change alkyl phenol calcium sulfoacid calcium 38.4 weight %；Lubricating base oil 54.3 weight %；Calcium stearate 2.3 weight
Amount %；M-phthalic acid calcium 5.0 weight %.
Embodiment 4
The present embodiment is for illustrating lubricant composition prepared by the present invention.
Raw material components: overbased sulfoacid calcium (total base number is 400mgKOH/g, 23kg)；High base number
Calcium sulfenyl phenolate (total base number is 320mgKOH/g, 6kg)；(total base number is overbased calcium alkyl-salicylate
360mgKOH/g, 10kg)；(100 DEG C of kinematic viscositys are 31mm to HVI150BS lubricating base oil2/ s,
20kg)；4-octadecylphenol (1.6kg)；DBSA (1.2kg)；Acetic acid (0.56kg)；
Calcium hydroxide (1.8kg)；12-hydroxy stearic acid (2kg)；P-phthalic acid (3.5kg)；HVI500SN
(100 DEG C of kinematic viscositys are 11mm to lubricating base oil2/ s, 28kg), right, right '-di-iso-octyldiphenylamine
(0.2kg)。
Preparing lubricant composition according to the method for embodiment 1, except for the difference that, calcium sulfenyl phenolate uses
Total base number is the SULFURIZED CALCIUM ALKYL PHENATE WITH HIGH BASE NUMBER of 320mgKOH/g, and adds overbased calcium alkyl-salicylate；
Transforming agent adds DBSA；And treat that temperature is cooled to 110 DEG C, add the right of 0.2kg,
Right '-di-iso-octyldiphenylamine, after stirring 10 minutes, then circulating filtration, homogenizing, degassing obtain finished product；
The consumption of each composition is as above.Assay is shown in Table 1.
In the grease that the present embodiment obtains, on the basis of grease weight, consist of: non-newtonian fluid sulfur
Change alkyl phenol calcium sulfoacid calcium 39.6 weight %；Lubricating base oil 54.2 weight %；12-hydroxy stearic acid
Calcium 2 weight %；P-phthalic acid calcium 4.0 weight %, right, right '-di-iso-octyldiphenylamine 0.2 weight %.
Embodiment 5
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 is 320mgKOH/g, 14kg)；High base number sulfur
Change alkyl phenol calcium (total base number is 320mgKOH/g, 6kg)；(total base number is overbased calcium salicylate
400mgKOH/g, 10kg)；(100 DEG C of kinematic viscositys are 31mm to HVI150BS lubricating base oil2/ s,
15kg)；4-octadecylphenol (1.8kg)；Aphthenic acids (total acid number is 180mgKOH/g, 1.0kg)；
Acetic acid (0.56kg)；Calcium hydroxide (1.8kg)；12-hydroxy stearic acid (2kg)；P-phthalic acid (3.5kg)；
(100 DEG C of kinematic viscositys are 11mm to HVI500SN lubricating base oil2/ s, 7kg).
Preparing lubricant composition according to the method for embodiment 1, except for the difference that, sulfoacid calcium uses total base number
For the calcium sulfonate with high base number of 320mgKOH/g, calcium sulfenyl phenolate uses total base number to be 320mgKOH/g
SULFURIZED CALCIUM ALKYL PHENATE WITH HIGH BASE NUMBER, and add overbased calcium salicylate；Transforming agent increases aphthenic acids；
The consumption of each composition is as above.Assay is shown in Table 1.
In the grease that the present embodiment obtains, on the basis of grease weight, consist of: non-newtonian fluid sulfur
Change alkyl phenol calcium sulfoacid calcium 54.0 weight %；Lubricating base oil 35.6 weight %；12-hydroxy stearic acid
Calcium 3.4 weight %；P-phthalic acid calcium 7.0 weight %.
Embodiment 6
The present embodiment is for illustrating lubricant composition prepared by the present invention.
Raw material components: overbased sulfoacid calcium (total base number is 400mgKOH/g, 6kg)；Overbased
Calcium sulfenyl phenolate (total base number is 400mgKOH/g, 20kg)；(total base number is high base number calcium oleate
320mgKOH/g, 4kg)；(100 DEG C of kinematic viscositys are 41 to full synthetic oil poly & Alpha ,-olefin oil PAO 40
mm2/ s, 30kg)；4-octadecylphenol (2kg)；DBSA (0.8kg)；Acetic acid
(0.56kg)；Calcium hydroxide (1.8kg)；12-hydroxy stearic acid (2kg)；P-phthalic acid (3.5kg)；
(100 DEG C of kinematic viscositys are 11mm to full synthetic oil poly & Alpha ,-olefin oil PAO 102/ s, 17kg).
Prepare lubricant composition according to the method for embodiment 1, except for the difference that, add high base number oleic acid
Calcium；Transforming agent increases DBSA；Use full synthetic oil poly & Alpha ,-olefin oil PAO 40 (100
DEG C kinematic viscosity is 41mm2/ s) and PAO 10 (100 DEG C of kinematic viscositys are 11mm2/ s) replace respectively
(100 DEG C of kinematic viscositys are 31mm to HVI150BS2/ s) and HVI500SN (100 DEG C of kinematic viscositys are
11mm2/s)；The consumption of each composition is as above.Assay is shown in Table 1.
In the grease that the present embodiment obtains, on the basis of grease weight, consist of: non-newtonian fluid sulfur
Change alkyl phenol calcium sulfoacid calcium 38.4 weight %；Lubricating base oil 54.2 weight %；12-hydroxy stearic acid
Calcium 2.4 weight %；P-phthalic acid calcium 5.0 weight %.
Embodiment 7
The present embodiment is for illustrating lubricant composition prepared by the present invention.
Raw material components: overbased sulfoacid calcium (total base number is 400mgKOH/g, 6kg)；High base number sulfur
Change alkyl phenol calcium (total base number is 320mgKOH/g, 10kg)；Naphthenate with superhigh base number calcium (total base number
For 400mgKOH/g, 6kg)；High base number calcium salicylate (total base number is 360mgKOH/g, 8kg)；
(100 DEG C of kinematic viscositys are 31mm to HVI150BS lubricating base oil2/ s, 30kg)；4-octadecyl benzene
Phenol (2.2kg)；Aphthenic acids (total acid number is 180mgKOH/g, 0.6kg)；Acetic acid (0.56kg)；Hydrogen
Calcium oxide (2.2kg)；12-hydroxy stearic acid (10kg)；2-methyl isophthalic acid, 4-phthalic acid (2.2kg)；
(100 DEG C of kinematic viscositys are 11mm to HVI500SN lubricating base oil2/ s, 20kg).
Preparing lubricant composition according to the method for embodiment 1, except for the difference that, calcium sulfenyl phenolate uses
Total base number is the SULFURIZED CALCIUM ALKYL PHENATE WITH HIGH BASE NUMBER of 320mgKOH/g, and adds naphthenate with superhigh base number calcium
With high base number calcium salicylate；Transforming agent increases aphthenic acids；Using 2-methyl isophthalic acid, it is right that 4-phthalic acid replaces
Phthalic acid；The consumption of each composition is as above.Assay is shown in Table 1.
In the grease that the present embodiment obtains, on the basis of grease weight, consist of: non-newtonian fluid sulfur
Change alkyl phenol calcium sulfoacid calcium 34.5 weight %；Lubricating base oil 51.7 weight %；12-hydroxy stearic acid
Calcium 11.0 weight %；2-methyl isophthalic acid, 4-phthalic acid calcium 2.8 weight %.
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 is 320mgKOH/g, 6kg)；Overbased sulfur
Change alkyl phenol calcium (total base number is 400mgKOH/g, 9kg)；(total base number is high base number calcium salicylate
360mgKOH/g, 10kg)；High base number calcium oleate (total base number is 360mgKOH/g, 5kg)；
(100 DEG C of kinematic viscositys are 31mm to HVI150BS lubricating base oil2/ s, 30kg)；4-octadecyl benzene
Phenol (2.8kg)；Acetic acid (0.56kg)；Calcium hydroxide (1.8kg)；12-hydroxy stearic acid (2kg)；4,4'-
Biphenyl dicarboxylic acid (5.1kg)；(100 DEG C of kinematic viscositys are 11mm to HVI500SN lubricating base oil2/ s,
20kg), right, right '-di-iso-octyldiphenylamine (0.2kg)；Dithio dibutylamino formic acid molybdenum (4kg)；
Selenium sulfide (4kg)；Benzotriazole (0.4kg).
Preparing lubricant composition according to the method for embodiment 1, except for the difference that, sulfoacid calcium uses total base number
For the calcium sulfonate with high base number of 320mgKOH/g, and add high base number calcium salicylate and high base number oleic acid
Calcium；4,4'-biphenyl dicarboxylic acid is used to replace p-phthalic acid；And treat that temperature is cooled to 110 DEG C, add
0.2kg's is right, right '-di-iso-octyldiphenylamine, stirs 10 minutes, adds the dithio dibutylamine of 4kg
Base formic acid molybdenum, stirs 10 minutes, adds the selenium sulfide of 4kg, stirs 10 minutes, adds 0.4kg
Benzotriazole, stir 10 minutes, then circulating filtration, homogenizing, degassing obtain finished product；Each one-tenth
The consumption divided is as above.Assay is shown in Table 1.
In the grease that the present embodiment obtains, on the basis of grease weight, consist of: non-newtonian fluid sulfur
Change alkyl phenol calcium sulfoacid calcium 33.4 weight %；Lubricating base oil 50.0 weight %；12-hydroxy stearic acid
Calcium 2.1 weight %；4,4'-biphenyl dicarboxylic acid calcium 5.9 weight %；Right, right '-di-iso-octyldiphenylamine 0.2 weight
Amount %；Dithio dibutylamino formic acid molybdenum 4.0 weight %；Selenium sulfide 4.0 weight %；Benzene a pair of horses going side by side three nitrogen
Azoles 0.4 weight %.
Embodiment 9
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 is 320mgKOH/g, 6kg)；High base number vulcanizes
Alkyl phenol calcium (total base number is 320mgKOH/g, 8kg)；(total base number is naphthenate with superhigh base number calcium
400mgKOH/g, 8kg)；Overbased calcium oleate (total base number is 400mgKOH/g, 8kg)；
(100 DEG C of kinematic viscositys are 31mm to HVI150BS lubricating base oil2/ s, 15kg)；4-octadecyl benzene
Phenol (2.8kg)；Acetic acid (0.56kg)；Calcium hydroxide (1.8kg)；12-hydroxy stearic acid (2kg)；Right
Phthalic acid (3.5kg)；(100 DEG C of kinematic viscositys are 11mm to HVI500SN lubricating base oil2/ s,
32kg)。
Preparing lubricant composition according to the method for embodiment 1, except for the difference that, sulfoacid calcium uses total base number
For the calcium sulfonate with high base number of 320mgKOH/g, calcium sulfenyl phenolate uses total base number to be 320mgKOH/g
SULFURIZED CALCIUM ALKYL PHENATE WITH HIGH BASE NUMBER, and add naphthenate with superhigh base number calcium and overbased calcium oleate；Respectively
The consumption of composition is as above.Assay is shown in Table 1.
In the grease that the present embodiment obtains, on the basis of grease weight, consist of: non-newtonian fluid sulfur
Change alkyl phenol calcium sulfoacid calcium 38.4 weight %；Lubricating base oil 54.2 weight %；12-hydroxy stearic acid
Calcium 2.4 weight %；P-phthalic acid calcium 5.0 weight %.
Embodiment 10
The present embodiment is for illustrating lubricant composition prepared by the present invention.
Raw material components: overbased sulfoacid calcium (total base number is 400mgKOH/g, 5kg)；Overbased
Calcium sulfenyl phenolate (total base number is 400mgKOH/g, 5kg)；(total base number is overbased calcium alkyl-salicylate
360mgKOH/g, 10kg)；High base number calcium salicylate (total base number is 320mgKOH/g, 5kg)；High
Base number calcium oleate (total base number is 360mgKOH/g, 5kg)；HVI150BS lubricating base oil (100
DEG C kinematic viscosity is 31mm2/ s, 30kg)；4-octadecylphenol (2.8kg)；Acetic acid (0.56kg)；
Calcium hydroxide (4.2kg)；12-hydroxy stearic acid (2kg)；Boric acid (2.32kg)；Ethanedioic acid (3.02kg)；
(100 DEG C of kinematic viscositys are 11mm to HVI500SN lubricating base oil2/ s, 15kg), right, right '-two different pungent
Base diphenylamines (0.2kg).
Prepare lubricant composition according to the method for embodiment 1, except for the difference that, add high base number cycloalkanes
Acid calcium, high base number calcium salicylate and high base number calcium oleate；Add 12-hydroxy stearic acid, stir 10
After minute, add boric acid, stir 10 minutes, then add ethanedioic acid, stir 10 minutes, be not added with
Enter p-phthalic acid；And treat that temperature is cooled to 110 DEG C, add the right of 0.2kg, right '-diisooctyl two
Aniline, stirs 10 minutes, and then circulating filtration, homogenizing, degassing obtain finished product；The consumption of each composition
As above.Assay is shown in Table 1.
In the grease that the present embodiment obtains, on the basis of grease weight, consist of: non-newtonian fluid sulfur
Change alkyl phenol calcium sulfoacid calcium 38.2 weight %；Lubricating base oil 51.5 weight %；12-hydroxy stearic acid
Calcium 2.5 weight %；Calcium pyroborate 2.7 weight %；Ethanedioic acid calcium 4.9 weight %；Right, right '-diisooctyl two
Aniline 0.2 weight %.
Embodiment 11
The present embodiment is for illustrating lubricant composition prepared by the present invention.
Raw material components: non-newtonian fluid calcium sulfonate with high base number (15kg)；SULFURIZED CALCIUM ALKYL PHENATE WITH HIGH BASE NUMBER is (total
Base number is 320mgKOH/g, 15kg)；(100 DEG C of kinematic viscositys are 31 to HVI150BS lubricating base oil
mm2/ s, 30kg)；4-octadecylphenol (2.8kg)；Acetic acid (0.56kg)；Calcium hydroxide (3kg)；
12-hydroxy stearic acid (2kg)；P-phthalic acid (3.5kg)；Acetic acid (2kg)；HVI500SN lubricates
(100 DEG C of kinematic viscositys are 11mm to base oil2/ s, 14kg), right, right '-di-iso-octyldiphenylamine (0.2kg).
The preparation of non-newtonian fluid calcium sulfonate with high base number: volume be 30L and with heating, stirring,
Adding 8kg total base number in circulation, the normal-pressure reaction kettle cooled down is the calcium sulfonate with high base number of 360mgKOH/g
It is 31mm with 100 DEG C of kinematic viscositys of 5kg2The HVI150BS lubricating base oil of/s, stirring, heating rises
Warm to 80 DEG C, constant temperature 10 minutes；Adding 1.7kg DBSA, temperature controls on 80 DEG C of left sides
The right side, stirs 10 minutes；Add acetic acid and the aqueous solution of acetic acid weight 4 times of 0.33kg, stir 10
Minute；Being warmed up to 85 DEG C, constant temperature 90 minutes, material retrogradation becomes smectic, obtains non-newtonian fluid sulfoacid calcium
Standby.
Preparing lubricant composition according to the method for embodiment 1, except for the difference that, sulfoacid calcium uses total base number
For the non-newtonian fluid sulfoacid calcium prepared of 360mgKOH/g, calcium sulfenyl phenolate use total base number is
The SULFURIZED CALCIUM ALKYL PHENATE WITH HIGH BASE NUMBER of 320mgKOH/g；And add p-phthalic acid, stir 10 points
Zhong Hou, adds acetic acid, stirs 10 minutes；And treat that temperature is cooled to 110 DEG C, add the right of 0.2kg,
Right '-di-iso-octyldiphenylamine, stirs 10 minutes, and then circulating filtration, homogenizing, degassing obtain finished product；
The consumption of each composition is as above.Assay is shown in Table 1.
In the grease that the present embodiment obtains, on the basis of grease weight, consist of: non-newtonian fluid sulfur
Change alkyl phenol calcium sulfoacid calcium 38.5 weight %；Lubricating base oil 50.8 weight %；12-hydroxy stearic acid
Calcium 2.4 weight %；P-phthalic acid calcium 5.0 weight %；Calcium acetate 3.1 weight %；Right, right '-two different pungent
Base diphenylamines 0.2 weight %.
Embodiment 12
The present embodiment is for illustrating lubricant composition prepared by the present invention.
Raw material components: overbased sulfoacid calcium (total base number is 400mgKOH/g, 24kg)；Superelevation alkali
Value calcium sulfenyl phenolate (total base number is 400mgKOH/g, 6kg)；HVI150BS lubricating base oil (100
DEG C kinematic viscosity is 31mm2/ s, 30kg)；4-octadecylphenol (2.8kg)；Acetic acid (0.56kg)；
Calcium hydroxide (1.8kg)；12-hydroxy stearic acid (2kg)；P-phthalic acid (3.5kg)；HVI500SN
(100 DEG C of kinematic viscositys are 11mm to lubricating base oil2/ s, 17kg).
A volume be 160L and with the normal-pressure reaction kettle heating, stirring, circulate, cool down in add
Entering 24kg total base number is that the overbased sulfoacid calcium of 400mgKOH/g, 6kg total base number are
The overbased calcium sulfenyl phenolate of 400mgKOH/g and the HVI150BS lubricating base oil of 30kg,
Stirring, heats to 50 DEG C, constant temperature 10 minutes；Add 2.8kg 4-octadecylphenol, temperature
Control at about 50 DEG C, stir 10 minutes；Add the aqueous acetic acid that 2.8kg concentration is 20 weight %,
Stir 10 minutes；It is warmed up to 80 DEG C, constant temperature 90 minutes, material retrogradation.
Another volume be 50L and with the normal-pressure reaction kettle heating, stirring, circulate, cool down in add
Enter 7kg HVI500SN lubricating base oil, at 100 DEG C, add the hydroxide that solid content is 20 weight %
Calcium suspension 9kg, stirs 10 minutes；Add 2kg 12-hydroxy stearic acid, stir 10 minutes；Add
3.5kg p-phthalic acid, stirs 10 minutes, obtains 12-hydroxy stearic acid calcium and p-phthalic acid calcium.
12-hydroxy stearic acid calcium and the p-phthalic acid calcium of gained are all squeezed in a upper still, stirring
Uniformly, under stirring, it is warmed up to 120 DEG C, keeps 45 minutes, dehydration, finally it is warmed up to 200 DEG C of constant temperature 10
Minute.Then, it is cooled to 160 DEG C, adds remaining HVI500SN lubricating base oil；Treat that temperature is cold
But to 110 DEG C, circulating filtration, homogenizing, degassing obtain finished product.Assay is shown in Table 1.
In the grease that the present embodiment obtains, on the basis of grease weight, consist of: non-newtonian fluid sulfur
Change alkyl phenol calcium sulfoacid calcium 38.4 weight %；Lubricating base oil 54.2 weight %；12-hydroxy stearic acid
Calcium 2.4 weight %；P-phthalic acid calcium 5.0 weight %.
Embodiment 13
The present embodiment is for illustrating lubricant composition prepared by the present invention.
Raw material components: overbased sulfoacid calcium (total base number is 400mgKOH/g, 24kg)；Superelevation alkali
Value calcium sulfenyl phenolate (total base number is 400mgKOH/g, 6kg)；HVI150BS lubricating base oil (100
DEG C kinematic viscosity is 31mm2/ s, 30kg)；4-octadecylphenol (2.8kg)；Acetic acid (0.56kg)；
Calcium hydroxide (1.8kg)；12-hydroxy stearic acid (2kg)；P-phthalic acid (3.5kg)；HVI500SN
(100 DEG C of kinematic viscositys are 11mm to lubricating base oil2/ s, 17kg).
A volume be 160L and with the normal-pressure reaction kettle heating, stirring, circulate, cool down in add
Entering 24kg total base number is that the overbased sulfoacid calcium of 400mgKOH/g, 6kg total base number are
The overbased calcium sulfenyl phenolate of 400mgKOH/g and the HVI150BS lubricating base oil of 30kg,
Stirring, is warmed up to 50 DEG C, constant temperature 30 minutes, adds 2.8kg 4-octadecylphenol, and temperature controls
At 50 DEG C, stir 10 minutes, add the aqueous acetic acid that 2.8kg concentration is 20 weight %, stir 10
Minute, it is warmed up to 80 DEG C, constant temperature 90 minutes, material retrogradation；It is warmed up to 100 DEG C, adds solid content
It is the calcium hydroxide suspension 9kg of 20 weight %, stirs 10 minutes；Add 2kg 12-hydroxy stearic acid,
Stir 10 minutes；Add 3.5kg p-phthalic acid, stir 10 minutes；120 DEG C it are warmed up under stirring,
Keep 45 minutes, dehydration；It is warmed up to 200 DEG C of constant temperature 10 minutes.Then, it is cooled to 160 DEG C, adds
Enter the HVI500SN lubricating base oil of 17kg；Treat that temperature is cooled to 110 DEG C, circulating filtration, homogenizing,
Degassing obtains finished product.Assay is shown in Table 1.
In the grease that the present embodiment obtains, on the basis of grease weight, consist of: non-newtonian fluid sulfur
Change alkyl phenol calcium sulfoacid calcium 38.4 weight %；Lubricating base oil 54.2 weight %；12-hydroxy stearic acid
Calcium 2.4 weight %；P-phthalic acid calcium 5.0 weight %.
Embodiment 14
The present embodiment is for illustrating lubricant composition prepared by the present invention.
Lubricant composition is prepared, except for the difference that, by 4-octadecyl benzene according to the method for embodiment 1
Phenol replaces with methyl propyl ketone, and acetic acid is replaced with butyl ether.Assay is shown in Table 1.
In the grease that the present embodiment obtains, on the basis of grease weight, consist of: non-newtonian fluid sulfur
Change alkyl phenol calcium sulfoacid calcium 38.4 weight %；Lubricating base oil 54.2 weight %；12-hydroxy stearic acid
Calcium 2.4 weight %；P-phthalic acid calcium 5.0 weight %.
Comparative example 1
Complex calcium sulfonate grease is prepared according to the method for embodiment 1, except for the difference that, overbased sulfur
Change the overbased sulfoacid calcium that alkyl phenol calcium total base number is 400mgKOH/g to replace, the grease obtained
The each performance data of finished product is shown in Table 1.
In the grease that this comparative example obtains, on the basis of grease weight, consist of: non-newtonian fluid sulphur
Acid calcium 38.4 weight %；Lubricating base oil 54.2 weight %；12-hydroxy stearic acid calcium 2.4 weight %；Right
Phthalic acid calcium 5.0 weight %.
It will be understood by those skilled in the art that Drawing cone in-degree is the least, grease thickening performance is more
Good；Extending Drawing cone in-degree the least with the difference of Drawing cone in-degree, the mechanical stability of grease can be the best；
Water pouring number of dropouts is the least, and the water-resistance of grease is the best；Salt spray test the highest grade, grease antirust
And anticorrosive property is the best；Water resistant spraying value is the least, and the adhesiveness of grease and water-resistance are the best；Steel mesh divides
Oil value is the least, and the colloid stability of grease is the best；The absolute value of Surface hardened layer value is the least, grease
Storage stability is the best；Coefficient of friction is the least, and the abrasion resistance of grease is the best；PB, PD value is the biggest,
The extreme pressure anti-wear of grease is the best.
Table 1 each grease properties of sample data
Each indication test method: dropping point: GB/T 3498；Drawing cone in-degree and prolongation Drawing cone in-degree: GB/T 269；Corrosion: GB/T 7326；
Anticorrosive property: GB/T 5018；Water drenches number of dropouts: SH/T 0109；Salt spray test: SH/T 0081；Water resistant is sprayed: SH/T0643；Steel
Net point oil: SH/T 0324；Surface hardened layer value: SH/T 0370 appendix A；Coefficient of friction: SH/T 0721；Tetra-ball machine test: SH/T 0202.
Table 1 (Continued) each grease properties of sample data
Each indication test method: dropping point: GB/T 3498；Drawing cone in-degree and prolongation Drawing cone in-degree: GB/T 269；Corrosion: GB/T 7326；
Anticorrosive property: GB/T 5018；Water drenches number of dropouts: SH/T 0109；Salt spray test: SH/T 0081；Water resistant is sprayed: SH/T0643；Steel
Net point oil: SH/T 0324；Surface hardened layer value: SH/T 0370 appendix A；Coefficient of friction: SH/T 0721；Tetra-ball machine test: SH/T 0202.
Embodiment 1 and comparative example 1 are compared it can be seen that lubricant composition anti-of the present invention
Rust and anticorrosive property, storage stability are substantially better than complex calcium sulfonate grease.And, the present invention's
Lubricant composition have be better than the viscous resistance of complex calcium sulfonate grease, mechanical stability, water-resistance,
Colloid stability, abrasion resistance and extreme pressure anti-wear.And, the lubricant composition of the present invention also has
Excellent heat-resisting quantity.
Embodiment 1 and embodiment 12 are compared it can be seen that the lubricant composition of preparation in situ,
There is more preferable viscous resistance, mechanical stability, water-resistance, colloid stability, abrasion resistance and extreme pressure anti-
Mill property；Embodiment 1 is compared it can be seen that be first combined with embodiment 12, embodiment 13
The reaction of calcium, then convert, the lubricant composition prepared has more preferable viscous resistance, machinery is stabilized
Property, water-resistance, colloid stability, abrasion resistance and extreme pressure anti-wear；By embodiment 1 and embodiment 14
Compare it can be seen that transforming agent is selected from DBSA, aphthenic acids, octadecyl phenol, first
At least one in alcohol, isopropanol, butanol, boric acid, acetic acid and water, the lubricant composition of preparation,
There is more preferable viscous resistance, mechanical stability, water-resistance, colloid stability, abrasion resistance and extreme pressure anti-
Mill property.
The lubricant composition of the present invention, has the most excellent with complex calcium sulfonate grease
Antirust and anticorrosive property, and there is excellent storage stability, also have and be better than Composite calcium-sulfonate-batetrapolyurea lubrication
The viscous resistance of fat, mechanical stability, water-resistance, colloid stability, abrasion resistance and extreme pressure anti-wear,
And also there is the performances such as excellent heat-resisting quantity.The feed preparation process of the grease of the present invention is simple, ring
Protect, constant product quality.
The preferred embodiment of the present invention is described in detail above in association with accompanying drawing, but, the present invention does not limit
Detail in above-mentioned embodiment, in the technology concept of the present invention, can be to the present invention
Technical scheme carry out multiple simple variant, these simple variant belong to protection scope of the present invention.
It is further to note that each the concrete technology described in above-mentioned detailed description of the invention is special
Levy, in the case of reconcilable, can be combined by any suitable means, in order to avoid need not
The repetition wanted, various possible compound modes are illustrated by the present invention the most separately.
Additionally, combination in any can also be carried out between the various different embodiment of the present invention, as long as its
Without prejudice to the thought of the present invention, it should be considered as content disclosed in this invention equally.
Claims (20)
1. a lubricant composition, described lubricant composition contains base oil and thickening agent, and it is special
Levying and be, described thickening agent contains non-newtonian fluid calcium sulfenyl phenolate sulfoacid calcium and the calcium of higher fatty acids
Salt, described thickening agent is also optionally with non-newtonian fluid calcium naphthenate, non-newtonian fluid calcium salicylate, non-cattle
One in the calcium salt of body calcium oleate, the calcium salt of aromatic acid, little molecule mineral acid and/or lower fatty acid or
Multiple, on the basis of the weight of described lubricant composition, the content of base oil is 10 80 weight %,
The content of non-newtonian fluid calcium sulfenyl phenolate sulfoacid calcium is 10 70 weight %, the calcium salt of higher fatty acids
Content be 1 20 weight %, the content of non-newtonian fluid calcium naphthenate is 0-70 weight %, non-newtonian fluid
The content of calcium salicylate is 0-70 weight %, and the content of non-newtonian fluid calcium oleate is 0-70 weight %, virtue
The content of the calcium salt of acid is 0-15 weight %, containing of the calcium salt of little molecule mineral acid and/or lower fatty acid
Amount is 0 15 weight %.
Lubricant composition the most according to claim 1, wherein, with lubricant composition weight
On the basis of, the content of base oil is 20 70 weight %, non-newtonian fluid calcium sulfenyl phenolate sulfoacid calcium
Content is 20 65 weight %, and the content of the calcium salt of higher fatty acids is 2 15 weight %, non-newtonian fluid ring
The content of alkanoic acid calcium is 0-50 weight %, and the content of non-newtonian fluid calcium salicylate is 0-50 weight %, non-
The content of newton body calcium oleate is 0-50 weight %, and the content of the calcium salt of aromatic acid is 2-10 weight %, little
The content of the calcium salt of molecule mineral acid and/or lower fatty acid is 2 10 weight %.
Lubricant composition the most according to claim 1 and 2, wherein, described non-newtonian fluid sulfur
Change alkyl phenol calcium sulfoacid calcium to be obtained by newton body sulfoacid calcium and the conversion of newton body calcium sulfenyl phenolate,
The total base number of described non-newtonian fluid calcium sulfenyl phenolate sulfoacid calcium is 250 450mgKOH/g；Described non-
Newton body calcium naphthenate is converted by newton body calcium naphthenate and obtains, described non-newtonian fluid calcium naphthenate
Total base number is 250-450mgKOH/g；Described non-newtonian fluid calcium salicylate is to be turned by newton body calcium salicylate
Change obtains, and the total base number of described non-newtonian fluid calcium salicylate is 250-450mgKOH/g；Described non-cattle
The body calcium oleate that pauses is converted by newton body calcium oleate and obtains, and the total base number of described non-newtonian fluid calcium oleate is
250-450mgKOH/g。
Lubricant composition the most according to claim 1 and 2, wherein, described higher fatty acids
For fatty acid that carbon number is 8-20 or hydroxy fatty acid.
Lubricant composition the most according to claim 4, wherein, described higher fatty acids is selected from
At least one in lauric acid, Palmic acid, stearic acid, 12-hydroxy stearic acid, eicosyl carboxylic acid.
Lubricant composition the most according to claim 1 and 2, wherein, described aromatic acid is for replacing
Or unsubstituted aromatic acid, substituent group is the alkane of alkyl, thiazolinyl, alkynyl, aryl, halo or perhalogeno
At least one in base or aryl, the molecular weight of described aromatic acid is less than or equal to 550.
7. according to the lubricant composition described in claim 6, wherein, described aromatic acid is selected from unsubstituted
Or the substituted phthalic acid of C1-C5 alkyl, M-phthalic acid, p-phthalic acid, biphenyl diformazan
At least one in acid, polyphenyls dioctyl phthalate.
Lubricant composition the most according to claim 1 and 2, wherein, described little molecule is inorganic
The molecular weight of sour and described lower fatty acid is less than or equal to 250.
Lubricant composition the most according to claim 8, wherein, described little molecule mineral acid selects
At least one in boric acid, phosphoric acid, sulphuric acid, described lower fatty acid selected from acetic acid, ethanedioic acid, third
At least one in acid, malonic acid, butanoic acid, succinic acid.
10. the preparation method of lubricant composition described in any one, the method in claim 1-9
Including: by thickening agent and part basis oil mix homogeneously, refine at 180 230 DEG C of constant temperature, add surplus
Base oil, adds necessary additive, obtains finished product, it is characterised in that described thickening agent contains non-cattle
Body calcium sulfenyl phenolate sulfoacid calcium and the calcium salt of higher fatty acids, described thickening agent also optionally with
Non-newtonian fluid calcium naphthenate, non-newtonian fluid calcium salicylate, non-newtonian fluid calcium oleate, the calcium salt of aromatic acid, little
One or more in the calcium salt of molecule mineral acid and/or lower fatty acid.
The preparation method of 11. 1 kinds of lubricant compositions, it is characterised in that the method includes:
(1) containing newton body calcium sulfenyl phenolate, newton body and/or non-newtonian fluid sulfoacid calcium, or will contain
There are newton body and/or non-newtonian fluid calcium sulfenyl phenolate, the high base number material of newton body sulfoacid calcium, and part
Base oil mixes, and obtains mixture, and described high base number material is also optionally with newton body and/or non newtonian
Body calcium naphthenate, newton body and/or non-newtonian fluid calcium salicylate and newton body and/or non-newtonian fluid calcium oleate
In one or more；
(2) optionally carry out the reaction of at least part of composite calcium: add Calx or calcium hydroxide, add
Higher fatty acids, optional aromatic acid, optional little molecule mineral acid and/or lower fatty acid, react；
(3) add transforming agent, heat up and treat material retrogradation；
(4) carry out remaining the reaction of composite calcium；
(5) heat up dehydration；
(6) it is warmed up to 180 230 DEG C of constant temperature refinings, adds surplus base oil, add necessary additive,
Obtain finished product.
12. preparation methoies according to claim 11, wherein, in step (2), are carried out at least
The reaction of part composite calcium.
13. according to the preparation method described in claim 11 or 12, wherein, and step (2) and step
(4) in, at 85-100 DEG C, add Calx or the suspension of calcium hydroxide, add higher fatty acids,
Stir 5-20 minute, add optional aromatic acid, optional little molecule mineral acid and/or lower fatty acid,
Stir 5-20 minute.
14. according to the preparation method described in claim 11 or 12, wherein, in step (3),
At 50-80 DEG C, the transforming agent needed for addition reacts, after all transforming agents add, at 80-100 DEG C
Constant temperature 60-90 minute.
15. according to the preparation method described in claim 11 or 12, wherein, in step (5), rises
Temperature is to 110-130 DEG C of dehydration.
16. according to the preparation method described in claim 11 or 12, wherein, in step (6), rises
Temperature to 180-230 DEG C constant temperature 5-30 minute, adds surplus base oil, treats that temperature is cooled to 100-120
DEG C, add necessary additive, stirring, circulating filtration, homogenizing, degassing.
17. according to the preparation method described in claim 11 or 12, wherein, and described newton body sulfuration alkane
Base phenol calcium is synthesis calcium sulfenyl phenolate, and the total base number of described newton body calcium sulfenyl phenolate is
250-450mgKOH/g；Described newton body sulfoacid calcium is calcium mahogany sulfonate and/or calcium alkylbenzenesulfonate, described
The total base number of newton body sulfoacid calcium is 250-450mgKOH/g；Described newton body calcium naphthenate is oil ring
Alkanoic acid calcium and/or synthesis calcium naphthenate, the total base number of described newton body calcium naphthenate is
250-450mgKOH/g；Described newton body calcium salicylate is salicylate calcium, described newton body bigcatkin willow
The total base number of acid calcium is 250-450mgKOH/g；Described newton body calcium oleate is natural calcium oleate and/or conjunction
Becoming calcium oleate, the total base number of described newton body calcium oleate is 250-450mgKOH/g.
18. according to the preparation method described in claim 11 or 12, and wherein, described transforming agent is selected from fat
Fat alcohol, fatty acid, aliphatic ketone, fatty aldehyde, fatty amine, ether, calcium carbonate, boric acid, phosphonic acids, dioxy
Change carbon, phenol, aromatic alcohol, aromatic amine, C8-C20 alkyl benzene sulphonate, aphthenic acids, C16-C24 alkane
At least one in base phenol and water, the addition of transforming agent is described high base number material gross weight
2-30%.
19. preparation methoies according to claim 18, wherein, described transforming agent is selected from dodecane
In base benzenesulfonic acid, aphthenic acids, octadecyl phenol, methanol, isopropanol, butanol, boric acid, acetic acid and water
At least one, the addition of transforming agent is the 6-22% of described high base number material gross weight.
20. lubricant compositions prepared by the method described in any one in claim 11-19.
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| CN103740435A (en) * | 2014-02-11 | 2014-04-23 | 上海禾泰特种润滑技术有限公司 | Composite calcium sulfonate lubricating grease composition and preparation method thereof |
| CN104212560A (en) * | 2014-08-26 | 2014-12-17 | 青岛康泰鑫环保科技有限公司 | Improved rail lubricating grease |
| CN104212554A (en) * | 2014-08-22 | 2014-12-17 | 青岛康泰鑫环保科技有限公司 | Lubricating grease for gears |
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|---|---|---|---|---|
| US2921904A (en) * | 1957-07-17 | 1960-01-19 | California Research Corp | Grease composition containing metal salt of reaction product of alkylphenol, fatty acid and aldehyde |
| US3376222A (en) * | 1963-09-16 | 1968-04-02 | Lubrizol Corp | Process for preparing lubricating grease |
| US5338467A (en) * | 1993-03-03 | 1994-08-16 | Witco Corporation | Sulfonate grease improvement |
| KR101132881B1 (en) * | 2004-07-29 | 2012-04-03 | 켐트라 캐나다 코./시 | Modified overbased calcium or calcium borate salicylate complex greases |
| US20130109602A1 (en) * | 2011-10-31 | 2013-05-02 | J. Andrew Waynick | Calcium Carbonate Based Sulfonate Grease Compositions and Method of Manufacture |
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