CN104449959B - A kind of high base number complex calcium lubricating grease and preparation method thereof - Google Patents
A kind of high base number complex calcium lubricating grease and preparation method thereof Download PDFInfo
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- CN104449959B CN104449959B CN201310419089.0A CN201310419089A CN104449959B CN 104449959 B CN104449959 B CN 104449959B CN 201310419089 A CN201310419089 A CN 201310419089A CN 104449959 B CN104449959 B CN 104449959B
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Abstract
The invention discloses a kind of high base number complex calcium lubricating grease, it is characterised in that on the basis of lubricating grease weight, including following components：10 70 weight % non-newtonian fluid sulfoacid calcium calcium naphthenate；The calcium salt of 1 20 weight % higher fatty acids；1 15 weight % small molecule inorganic acid and/or the calcium salt of lower fatty acid；10 80 weight % base oil.The invention also discloses the preparation method of high base number complex calcium lubricating grease and its high base number complex calcium lubricating grease of preparation.The high base number complex calcium lubricating grease of the present invention, there is excellent anticorrosive property and heat-resisting quantity, but also the performance such as mechanical stability, water-resistance and adhesiveness with better than complex calcium sulfonate grease, resistance to saltfog, colloid stability, extreme pressure anti-wear.The preparation of greases technique of the present invention is simple and environmentally-friendly, and cost is low, and product quality is stable.
Description
Technical field
The present invention relates to lubricating grease, in particular it relates to a kind of high base number complex calcium lubricating grease and preparation method thereof.
Background technology
Sulfoacid calcium is used as the detersive and the history of antirust agent existing decades of lubricating oil, is widely used in internal combustion engine lubrication
The additive of oil, the development of its technology mainly make its height alkalization, are exactly alkyl benzene sulphonate of the calcium carbonate with surface-active
Calcium or alkyl carboxylic acid calcium turn into a kind of colloidal dispersion system to be distributed in flux oil.Calcium sulfonate with high base number according to the mode of production not
It is same to be divided into calcium mahogany sulfonate and calcium alkylbenzenesulfonate.Calcium mahogany sulfonate is to use oleum or SO3Sulfonation mineral lubricating oil produces
Accessory substance mahogany acid during white oil, through with Ca (OH)2React, the contour alkalization technology that is carbonated and obtain；Calcium alkylbenzenesulfonate is to use
Oleum or SO3The alkylbenzene of sulfonation synthesis, the alkyl benzene sulphonate of generation pass through and Ca (OH)2React, be carbonated contour alkalization skill
Art and obtain.
Overbased calcium alkyl-salicylate has preferable detergent-dispersant performance, good acid neutralization capacity and excellent diffusivity, can
To be used as the detersive of lubricating oil, the additive of IC engine lubricating oil is widely used in, the development of its technology mainly makes its high-alkali
Change, calcium carbonate is exactly turned into a kind of colloidal dispersion system with the naphthenic acid calcium with surface-active to be distributed in flux oil.It is high
Base number calcium naphthenate mostly be the acidic components extracted in the distillate obtained from crude distillation, through with Ca (OH)2Reaction, carbonating
Contour alkalization technology and obtain, about prepare Patents have CN1465560 etc..
Using calcium sulfonate with high base number be raw material produce lubricating grease, because its have excellent high temperature performance, mechanical stability,
Colloid stability, oxidation stability, water-resistance, anticorrosive property and antirust wear resistence, since putting goods on the market, domestic and international profit is caused
The extensive concern of consistent lubricant industry, however, although high base number composite calcium sulfonate base grease has very excellent combination property, but
The high price of its raw materials for production calcium sulfonate with high base number and complicated preparation technology itself cause it not promoted rapidly, together
When, with requirement more and more higher of the people to environmental protection, in calcium sulfonate with high base number production process must through sulfonation process to ring
The pollution in border is also increasingly subject to the concern of people.Find a kind of performance it is similar with high base number composite calcium sulfonate base grease but can
Mitigating the lubricating grease of above mentioned problem turns into the big problem that people face at present.
The content of the invention
Similar with high base number composite calcium sulfonate base grease it is an object of the invention to provide a kind of performance, cost is low, prepares
Simple and environmentally-friendly lubricating grease of technique and preparation method thereof.
The present inventor has found under study for action, on the basis of lubricating grease weight, including following components：10-70 weight %
Non-newtonian fluid sulfoacid calcium-calcium naphthenate；The calcium salt of 1-20 weight % higher fatty acids；1-15 weight % small molecule inorganic acid
And/or the calcium salt of lower fatty acid；10-80 weight % base oil.The performance and high base number composite calcium sulfonate Ji Run of the lubricating grease
Consistent lubricant is similar, and cost is low, and preparation technology is simple and environmentally-friendly.
Therefore, to achieve these goals, on the one hand, the invention provides a kind of high base number complex calcium lubricating grease, with
On the basis of lubricating grease weight, including following components：10-70 weight % non-newtonian fluid sulfoacid calcium-calcium naphthenate；1-20 weight %'s
The calcium salt of higher fatty acids；1-15 weight % small molecule inorganic acid and/or the calcium salt of lower fatty acid；10-80 weight % base
Plinth oil.
Preferably, on the basis of lubricating grease weight, including following components：20-65 weight % non-newtonian fluid sulfoacid calcium-ring
Alkanoic acid calcium；The calcium salt of 2-15 weight % higher fatty acids；2-10 weight % small molecule inorganic acid and/or the calcium of lower fatty acid
Salt；20-70 weight % base oil.
Second aspect, the invention provides the preparation method of high base number complex calcium lubricating grease as described above, this method
Including：By non-newtonian fluid sulfoacid calcium-calcium naphthenate, the calcium salt of higher fatty acids, small molecule inorganic acid and/or lower fatty acid
Calcium salt and part basis oil are well mixed, are refined in 180-230 DEG C of constant temperature, add surplus base oil, add necessary addition
Agent, obtain finished product.
The third aspect, the invention provides a kind of preparation method of high base number complex calcium lubricating grease, this method includes：
（1）By newton body sulfoacid calcium, newton body calcium naphthenate and part basis oil Hybrid Heating, transforming agent, heating are added
Treat material retrogradation；
（2）In step（1）Lime or calcium hydroxide are added in products therefrom, adds higher fatty acids, small molecule inorganic acid
And/or lower fatty acid is reacted, heat up dehydration after reaction；
（3）By step（2）Reaction gained mixture is warming up to 180-230 DEG C of constant temperature refining, adds surplus base oil, adds
Necessary additive, obtains finished product.
Fourth aspect, the invention provides the high base number complex calcium lubricating grease as made from method as described above.
The high base number complex calcium lubricating grease of the present invention, not only as complex calcium sulfonate grease, have excellent
Anticorrosive property and heat-resisting quantity, but also mechanical stability, water-resistance and adhesion with better than complex calcium sulfonate grease
The performances such as property, resistance to saltfog, colloid stability, extreme pressure anti-wear.The preparation of greases technique of the present invention is simple and environmentally-friendly, into
This is low, and product quality is stable.
Other features and advantages of the present invention will be described in detail in subsequent specific embodiment part.
Brief description of the drawings
Fig. 1 is the infrared spectrum of lubricating grease prepared by embodiment 2.
Embodiment
The embodiment of the present invention is described in detail below.It is it should be appreciated that described herein specific
Embodiment is merely to illustrate and explain the present invention, and is not intended to limit the invention.
The invention provides a kind of high base number complex calcium lubricating grease, this lubricating grease employ calcium mahogany sulfonate and/or
Calcium alkylbenzenesulfonate, and petroleum naphthenic acid calcium and/or synthesis calcium naphthenate are raw material, simultaneously containing composite calcium thickening agent.
Present invention also offers above-mentioned preparation of greases method.
On the one hand, the invention provides a kind of high base number complex calcium lubricating grease, on the basis of lubricating grease weight, including with
Lower component：10-70 weight % non-newtonian fluid sulfoacid calcium-calcium naphthenate；The calcium salt of 1-20 weight % higher fatty acids；1-15 weights
Measure % small molecule inorganic acid and/or the calcium salt of lower fatty acid；10-80 weight % base oil.
Preferably, on the basis of lubricating grease weight, including following components：20-65 weight % non-newtonian fluid sulfoacid calcium-ring
Alkanoic acid calcium；The calcium salt of 2-15 weight % higher fatty acids；2-10 weight % small molecule inorganic acid and/or the calcium of lower fatty acid
Salt；20-70 weight % base oil.
Non-newtonian fluid sulfoacid calcium-the calcium naphthenate is in infrared spectrum 873cm-1-886cm-1There is crystal form calcium carbonate spy in place
Levy absworption peak, preferably total base number 250mgKOH/g-450mgKOH/g, 300mgKOH/g-400mgKOH/g.The non newtonian
Body sulfoacid calcium-calcium naphthenate is to convert to obtain by transforming agent by newton body sulfoacid calcium and newton body calcium naphthenate.And newton body
Contain unformed calcium carbonate in sulfoacid calcium, newton body calcium naphthenate, in infrared spectrum 860cm-1-865cm-1Place occurs unformed
Calcium carbonate characteristic absorption peak.The newton body sulfoacid calcium is calcium mahogany sulfonate and/or calcium alkylbenzenesulfonate, and its total base number is
250mgKOH/g-450mgKOH/g, preferably 300mgKOH/g-400mgKOH/g；The newton body calcium naphthenate is oil ring
Alkanoic acid calcium and/or synthesis calcium naphthenate, its total base number is 250mgKOH/g-450mgKOH/g, preferably 300mgKOH/g-
400mgKOH/g.The base number of non-newtonian fluid sulfoacid calcium-calcium naphthenate is the base number and newton body calcium naphthenate of newton body sulfoacid calcium
Base number weight average value.
In the present invention, higher fatty acids is that carbon number is 8-20, preferably 10-16 straight chain fatty acid or hydroxy fatty acid, example
Such as at least one of laurate, palmitic acid, stearic acid, 12- hydroxy stearic acids, eicosyl carboxylic acid, preferably 12- hydroxyls are hard
Resin acid.
In the present invention, the molecular weight of small molecule inorganic acid or lower fatty acid is less than or equal to 150.Wherein, small molecule is inorganic
Acid can be selected from least one of boric acid, phosphoric acid, sulfuric acid etc., preferably boric acid and/or phosphoric acid；Lower fatty acid can be selected from
At least one of acetic acid, ethanedioic acid, propionic acid, malonic acid, butyric acid, succinic acid etc., preferably acetic acid.
The lube base oil can be mineral oil, artificial oil, vegetable oil or their mixture, and 100 DEG C of motions are glutinous
Spend for 4-150mm2/ s, preferably 10-60mm2/s.Artificial oil can be poly-a-olefin oil（PAO）, Esters oil, alkyl-silicone oil, take
Hold in the palm artificial oil etc..
Various additives, such as antioxidant, extreme pressure anti-wear additives, antirust agent can also be contained in lubricating grease of the present invention.Its
In, the preferred arylamine kind antioxidant of antioxidant, account for 0.01-5%, the preferably 0.1-2.5% of lubricating grease gross weight, can be diphenylamines,
At least one of phenyl-α-naphthylamine and di-iso-octyldiphenylamine, preferably di-iso-octyldiphenylamine.Extreme pressure anti-wear additives account for lubricating grease
The 0.5-12% of gross weight, preferably 0.8-8%, can be two thio Acidic phosphates zinc, two thio dialkyl amido formic acid molybdenums, two
Thio dialkyl amido lead formate, triphenylphosphorothionate, organic molybdenum complex compound, olefine sulfide, molybdenum disulfide, polytetrafluoroethyl-ne
Alkene, D2EHDTPA molybdenum, chlorinated paraffin, dibutyl dithiocaarbamate antimony, tungsten disulfide, selenium disulfide, fluorographite, carbonic acid
At least one of calcium and zinc oxide；Antirust agent accounts for the 0.01-4.5% of lubricating grease gross weight, preferably 0.1-2%, can be oil
At least one of barium sulfonate, petroleum sodium sulfonate, benzothiazole, benzotriazole, zinc naphthenate and alkenyl succinic acid.
Second aspect, the invention provides the preparation method of high base number complex calcium lubricating grease as described above, this method
Including：By non-newtonian fluid sulfoacid calcium-calcium naphthenate, the calcium salt of higher fatty acids, small molecule inorganic acid and/or lower fatty acid
Calcium salt and part basis oil are well mixed, are refined in 180-230 DEG C of constant temperature, add surplus base oil, add necessary addition
Agent, obtain finished product.
In the present invention, for non-newtonian fluid sulfoacid calcium-calcium naphthenate, the calcium salt of higher fatty acids, small molecule inorganic acid and/
Or calcium salt, base oil and the additive of lower fatty acid are as described above, will not be repeated 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 are used
Base oil total amount, in the present invention, part basis oil and the weight ratio preferably 1 of surplus base oil：0.1-5.
For non-newtonian fluid sulfoacid calcium-calcium naphthenate, conversion can be passed through by newton body sulfoacid calcium, newton body calcium naphthenate
Agent converts to obtain, for example, by newton body ring sulfoacid calcium, newton body alkanoic acid calcium, base oil Hybrid Heating to 50-80 DEG C, adds institute
The transforming agent needed is reacted, and after all transforming agents add, in 80-100 DEG C of constant temperature 60-90 minute, then heats to 100-120
DEG C dehydration.
The third aspect, the invention provides a kind of preparation method of high base number complex calcium lubricating grease, including：
（1）By newton body sulfoacid calcium, newton body calcium naphthenate and part basis oil Hybrid Heating, transforming agent, heating are added
Treat material retrogradation；
（2）In step（1）Lime or calcium hydroxide are added in products therefrom, adds higher fatty acids, small molecule inorganic acid
And/or lower fatty acid is reacted, heat up dehydration after reaction；
（3）By step（2）Products therefrom is warming up to 180-230 DEG C of constant temperature refining, adds surplus base oil, adds necessary
Additive, obtain finished product.
Step（1）In, by newton body sulfoacid calcium, newton body calcium naphthenate, part basis oil Hybrid Heating to 50-80 DEG C,
Transforming agent needed for adding is reacted, after all transforming agents add, in 80-100 DEG C of constant temperature 60-90 minute.
In the present invention, for the weight ratio of newton body sulfoacid calcium and newton body calcium naphthenate without particular/special requirement, preferably 1：
0.25-4.Newton body sulfoacid calcium and the gross weight of newton body calcium naphthenate and the weight ratio of part basis oil are preferably 1：0.1-3.
The newton body sulfoacid calcium is calcium mahogany sulfonate and/or calcium alkylbenzenesulfonate, and its total base number is 250mgKOH/g-
450mgKOH/g, preferably 300mgKOH/g-400mgKOH/g；The newton body calcium naphthenate be petroleum naphthenic acid calcium and/or
Calcium naphthenate is synthesized, its total base number is 250mgKOH/g-450mgKOH/g, preferably 300mgKOH/g-400mgKOH/g.
The transforming agent be preferably selected from fatty alcohol, aliphatic acid, aliphatic ketone, fatty aldehyde, fatty amine, ether, calcium carbonate, boric acid,
At least one of phosphonic acids, carbon dioxide, phenol, aromatic alcohol, aromatic amine, aphthenic acids, C8-C20 alkyl benzene sulphonates and water；It is more excellent
Choosing selected from C1-C5 fatty alcohol, C1-C5 aliphatic acid, C1-C5 aliphatic ketone, C1-C5 fatty aldehyde, C1-C5 fatty amine,
C1-C5 ether, boric acid, C1-C10 alkyl phosphonic acid, C2-C16 di alkyl phosphonic acid, C6-C20 arylphosphonic acid, C12-C24
At least one of diaryl phosphonic acids, C7-C20 aromatic alcohol, C7-C20 aromatic amine, C8-C20 alkyl benzene sulphonates and water；More
At least one further preferably in DBSA, aphthenic acids, methanol, isopropanol, butanol, boric acid, acetic acid and water
Kind.The addition of transforming agent is preferably the 2-30% of newton body sulfoacid calcium and newton body calcium naphthenate gross weight, more preferably newton
The 6-22% of body sulfoacid calcium and newton body calcium naphthenate gross weight.
In the present invention, fatty alcohol includes the fatty alcohol of straight chain, side chain and ring-type, aliphatic acid, aliphatic ketone, fatty aldehyde, fat
Amine is similarly.
Step（2）In, at 85-100 DEG C, the suspension of lime or calcium hydroxide is added, adds higher fatty acids, stirring
5-20 minutes, small molecule inorganic acid and/or lower fatty acid are added, stir 5-20 minutes, be warming up to 100-120 DEG C, preferably protect
30-60 minutes are held to realize dehydration；Wherein, higher fatty acids and small molecule inorganic acid and/or the addition sequence of lower fatty acid
It can exchange.
In the present invention, higher fatty acids, small molecule inorganic acid, lower fatty acid are as it was previously stated, will not be repeated here.
In the present invention, higher fatty acids and small molecule inorganic acid and/or the H of lower fatty acid+The amount and lime of total material
Or the OH contained by the suspension of calcium hydroxide-The amount of total material is equal, OH-Amount also can excessive 1-10%.
In the present invention, in terms of calcium hydroxide, the addition of the suspension of lime or calcium hydroxide is preferably newton body sulfonic acid
The 1-15% of calcium and newton body calcium naphthenate gross weight；With H+Material gauge, higher fatty acids and small molecule inorganic acid and/
Or the mol ratio of lower fatty acid is preferably 1：1-10.
In the present invention, the suspension of lime or calcium hydroxide refers to lime or calcium hydroxide formed in water it is suspended
Liquid, the solid content of suspension is preferably 10-60 weight %.
Step（3）In, it is warming up to 180-230 DEG C of constant temperature 5-20 minute；Surplus base oil is added, treats that temperature is cooled to 100-
120 DEG C, necessary additive is added, is stirred, circulating filtration, homogenizing, degassing.
In the present invention, step（1）In base oil used and step（3）In base oil used weight ratio preferably 1：0.1-
5。
Fourth aspect, present invention also offers high base number made from the preparation method provided as third aspect present invention is compound
Calcium-base grease.
Compared with the high base number complex calcium lubricating grease as made from the preparation method that second aspect provides, the third aspect provides
Preparation method made from high base number complex calcium lubricating grease there is more preferable mechanical stability, water-resistance and adhesiveness, colloid
Stability.
Embodiment
The present invention is further illustrated for following embodiment, but and is not so limited the present invention.
In the following Examples and Comparative Examples：
Non-newtonian fluid sulfoacid calcium-calcium naphthenate %=（Overbased or calcium sulfonate with high base number raw material weight+overbased or high
Base number calcium naphthenate raw material weight+transforming agent gross weight）/ lubricating grease gross weight × 100%.Transforming agent is included in non-newtonian fluid sulphur
In the content of sour calcium-calcium naphthenate.
Overbased and overbased calcium alkyl-salicylate raw material is purchased from Xinjiang Land Fine Petrochemical Co., Ltd, also may be used
To be prepared according to method disclosed in CN101885677A.
Overbased and calcium sulfonate with high base number raw material is purchased from Jinzhou Huifa Tianhe Chemical Co., Ltd..
Aphthenic acids is purchased from Jinzhou Tie Chen petrochemical industries Co., Ltd.
Embodiment 1
The present embodiment is used for the high base number complex calcium lubricating grease for illustrating prepared by the present invention.
Raw material components：Overbased sulfoacid calcium（Total base number is 400mgKOH/g, 24kg）；Naphthenate with superhigh base number calcium（Always
Base number is 400mgKOH/g, 6kg）；HVI150BS lubricating base oils（100 DEG C of kinematic viscosity are 31mm2/ s, 30kg）；Aphthenic acids
（Total acid number is 180mgKOH/g, 2.8kg）；Acetic acid（0.56kg）；Calcium hydroxide（1.8kg）；12- hydroxy stearic acids（2kg）；Boron
Acid（2.32kg）；HVI500SN lubricating base oils（100 DEG C of kinematic viscosity are 11mm2/ s, 18kg）.
A volume be 160L and with heating, stirring, circulation, cooling normal-pressure reaction kettle in add 24kg total base numbers
The naphthenate with superhigh base number calcium and 30kg for being 400mgKOH/g for 400mgKOH/g overbased sulfoacid calcium, 6kg total base numbers
HVI150BS lubricating base oils, stirring, heat to 50 DEG C, constant temperature 10 minutes；2.8kg aphthenic acids is added, temperature control exists
50 DEG C or so, stir 10 minutes；The aqueous acetic acid that 2.8kg concentration is 20 weight % is added, is stirred 10 minutes；80 DEG C are warming up to,
Constant temperature 90 minutes, material retrogradation；100 DEG C are warming up to, adds the calcium hydroxide suspension 9kg that solid content is 20 weight %, stirring 10
Minute；2kg12- hydroxy stearic acids are added, are stirred 10 minutes；Add the boric acid aqueous solution that 9.28kg concentration is 25 weight %, stirring
10 minutes, 110 DEG C are warming up under stirring, is kept for 45 minutes, dehydration；It is warming up to 200 DEG C of constant temperature 10 minutes.Then, 160 are cooled to
DEG C, 18kg HVI500SN lubricating base oils are added, treat that temperature is cooled to 110 DEG C, circulating filtration, homogenizing, degassing obtain finished product.
Assay is shown in Table 1.
In the lubricating grease that the present embodiment obtains, on the basis of lubricating grease weight, form and be：Non-newtonian fluid sulfoacid calcium-cycloalkanes
The sour weight % of calcium 38.5；The weight % of lubricating base oil 55.4；The weight % of 12- hydroxy stearic acids calcium 2.4；The weight % of line borate 3.7.
Embodiment 2
The present embodiment is used for the high base number complex calcium lubricating grease for illustrating prepared by the present invention.
Raw material components：Overbased sulfoacid calcium（Total base number is 420mgKOH/g, 6kg）；Naphthenate with superhigh base number calcium（Total alkali
It is worth for 420mgKOH/g, 24kg）；HVI150BS lubricating base oils（100 DEG C of kinematic viscosity are 31mm2/ s, 30kg）；Aphthenic acids
（Total acid number is 180mgKOH/g, 2.8kg）；Acetic acid（0.56kg）；Calcium hydroxide（1.8kg）；12- hydroxy stearic acids（2kg）；Boron
Acid（2.32kg）；HVI500SN lubricating base oils（100 DEG C of kinematic viscosity are 11mm2/ s, 18kg）.
A volume be 160L and with heating, stirring, circulation, cooling normal-pressure reaction kettle in add 6kg total base numbers
The naphthenate with superhigh base number calcium and 30kg for being 420mgKOH/g for 420mgKOH/g overbased sulfoacid calcium, 24kg total base numbers
HVI150BS lubricating base oils, stirring, heat to 60 DEG C, constant temperature 10 minutes；2.8kg aphthenic acids is added, temperature control exists
60 DEG C or so, stir 10 minutes；The aqueous acetic acid that 2.8kg concentration is 20 weight % is added, is stirred 10 minutes；85 DEG C are warming up to,
Constant temperature 75 minutes, material retrogradation；100 DEG C are warming up to, adds the calcium hydroxide suspension 9kg that solid content is 20 weight %, stirring 10
Minute；2kg12- hydroxy stearic acids are added, are stirred 10 minutes；Add the boric acid aqueous solution that 9.28kg concentration is 25 weight %, stirring
10 minutes, 100 DEG C are warming up under stirring, is kept for 60 minutes, dehydration；It is warming up to 180 DEG C of constant temperature 20 minutes.Then, 18kg is added
HVI500SN lubricating base oils, treat that temperature is cooled to 100 DEG C, circulating filtration, homogenizing, degassing obtain finished product.Assay is shown in
Table 1.
In the lubricating grease that the present embodiment obtains, on the basis of lubricating grease weight, form and be：Non-newtonian fluid sulfoacid calcium-cycloalkanes
The sour weight % of calcium 38.5；The weight % of lubricating base oil 55.4；The weight % of 12- hydroxy stearic acids calcium 2.4；The weight % of line borate 3.7.
Embodiment 3
The present embodiment is used for the high base number complex calcium lubricating grease for illustrating prepared by the present invention.
Raw material components：Overbased sulfoacid calcium（Total base number is 400mgKOH/g, 24kg）；Overbased calcium alkyl-salicylate（Total alkali
It is worth for 320mgKOH/g, 6kg）；HVI150BS lubricating base oils（100 DEG C of kinematic viscosity are 31mm2/ s, 20kg）；Butanol
（2.8kg）；Acetic acid（0.56kg）；Calcium hydroxide（1.8kg）；12- hydroxy stearic acids（2kg）；Boric acid（2.32kg）；HVI500SN
Lubricating base oil（100 DEG C of kinematic viscosity are 11mm2/ s, 28kg）.
A volume be 160L and with heating, stirring, circulation, cooling normal-pressure reaction kettle in add 24kg total base numbers
The naphthenate with superhigh base number calcium and 20kg for being 320mgKOH/g for 400mgKOH/g overbased sulfoacid calcium, 6kg total base numbers
HVI150BS lubricating base oils, stirring, heat to 80 DEG C, constant temperature 10 minutes；2.8kg butanol is added, temperature control is 80
DEG C or so, stir 10 minutes；The aqueous acetic acid that 2.8kg concentration is 20 weight % is added, is stirred 10 minutes；90 DEG C are warming up to, perseverance
Temperature 60 minutes, material retrogradation；The calcium hydroxide suspension 9kg that solid content is 20 weight % is added, is stirred 10 minutes；Add
2kg12- hydroxy stearic acids, stir 10 minutes；The boric acid aqueous solution that 9.28kg concentration is 25 weight % is added, stirs 10 minutes, stirs
Mix down and be warming up to 120 DEG C, kept for 30 minutes, dehydration；It is warming up to 230 DEG C of constant temperature 5 minutes.Then, 28kg HVI500SN is added
Lubricating base oil, treat that temperature is cooled to 120 DEG C, circulating filtration, homogenizing, degassing obtain finished product.Assay is shown in Table 1.
In the lubricating grease that the present embodiment obtains, on the basis of lubricating grease weight, form and be：Non-newtonian fluid sulfoacid calcium-cycloalkanes
The sour weight % of calcium 38.5；The weight % of lubricating base oil 55.4；The weight % of 12- hydroxy stearic acids calcium 2.4；The weight % of line borate 3.7.
Embodiment 4
The present embodiment is used for the high base number complex calcium lubricating grease for illustrating prepared by the present invention.
Raw material components：Overbased sulfoacid calcium（Total base number is 400mgKOH/g, 33kg）；Overbased calcium alkyl-salicylate（Total alkali
It is worth for 320mgKOH/g, 6kg）；HVI150BS lubricating base oils（100 DEG C of kinematic viscosity are 31mm2/ s, 20kg）；Dodecyl
Benzene sulfonic acid（2.8kg）；Acetic acid（0.56kg）；Calcium hydroxide（1.8kg）；12- hydroxy stearic acids（2kg）；Boric acid（2.32kg）；
HVI500SN lubricating base oils（100 DEG C of kinematic viscosity are 11mm2/ s, 28kg）, right, right '-di-iso-octyldiphenylamine（0.2kg）.
Method according to embodiment 1 prepares high base number complex calcium lubricating grease, unlike, calcium naphthenate uses total base number
For 320mgKOH/g overbased calcium alkyl-salicylate；Aphthenic acids is replaced with DBSA simultaneously；And treat that temperature is cooled to
110 DEG C, 0.2kg pair is added, after right '-di-iso-octyldiphenylamine stirs 10 minutes, then circulating filtration, homogenizing, degassing obtains
Finished product；The dosage of each composition is as above.Assay is shown in Table 1.
In the lubricating grease that the present embodiment obtains, on the basis of lubricating grease weight, form and be：Non-newtonian fluid sulfoacid calcium-cycloalkanes
The sour weight % of calcium 44.2；The weight % of lubricating base oil 50.1；The weight % of 12- hydroxy stearic acids calcium 2.2；The weight % of line borate 3.3；It is right,
Right ' weight % of-di-iso-octyldiphenylamine 0.2.
Embodiment 5
The present embodiment is used for the high base number complex calcium lubricating grease for illustrating prepared by the present invention.
Raw material components：Calcium sulfonate with high base number（Total base number is 320mgKOH/g, 24kg）；Overbased calcium alkyl-salicylate（Total base number
For 320mgKOH/g, 6kg）；HVI150BS lubricating base oils（100 DEG C of kinematic viscosity are 31mm2/ s, 15kg）；Aphthenic acids（Total acid
It is worth for 180mgKOH/g, 1.8kg）；150BS（15kg）；Aphthenic acids（1.8kg）；Butanol（1.0kg）；Acetic acid（0.56kg）；Hydrogen-oxygen
Change calcium Ca (OH)2（1.8kg）；12- hydroxy stearic acids（2kg）；Boric acid（2.32kg）；HVI500SN lubricating base oils（100 DEG C of fortune
Kinetic viscosity is 11mm2/ s, 7kg）；500SN（7kg）；It is right, right ' to p- di-iso-octyldiphenylamine（0.4kg）.
Method according to embodiment 1 prepares high base number complex calcium lubricating grease, unlike, sulfoacid calcium is using total base number
320mgKOH/g calcium sulfonate with high base number, calcium naphthenate use the overbased calcium alkyl-salicylate that total base number is 320mgKOH/g；Conversion
Agent is aphthenic acids, butanol and acetic acid, adds butanol after adding aphthenic acids, then adds acetic acid；And treat that temperature is cooled to 110
DEG C, 0.2kg pair is added, after right '-di-iso-octyldiphenylamine stirs 10 minutes, then circulating filtration, homogenizing, degassing obtains into
Product；The dosage of each composition is as above.Assay is shown in Table 1.
In the lubricating grease that the present embodiment obtains, on the basis of lubricating grease weight, form and be：Non-newtonian fluid sulfoacid calcium-cycloalkanes
The sour weight % of calcium 54.7；The weight % of lubricating base oil 36.1；The weight % of 12- hydroxy stearic acids calcium 3.5；The weight % of line borate 5.0；It is right,
Right ' weight % of-di-iso-octyldiphenylamine 0.7.
Embodiment 6
The present embodiment is used for the high base number complex calcium lubricating grease for illustrating prepared by the present invention.
Raw material components：Overbased sulfoacid calcium（Total base number is 400mgKOH/g, 6kg）；Naphthenate with superhigh base number calcium（Total alkali
It is worth for 400mgKOH/g, 24kg）；Poly alpha olefine synthetic oil PAO40（100 DEG C of kinematic viscosity are 41mm2/ s, 30kg）；Dodecane
Base benzene sulfonic acid（2.8kg）；Acetic acid（0.56kg）；Calcium hydroxide（1.8kg）；12- hydroxy stearic acids（2kg）；Boric acid（2.32kg）；
Poly alpha olefine synthetic oil PAO10（100 DEG C of kinematic viscosity are 11mm2/ s, 18kg）.
Method according to embodiment 1 prepares high base number complex calcium lubricating grease, unlike, use DBSA
Instead of aphthenic acids；Use full synthetic oil poly ＆ Alpha ,-olefin oil PAO40（100 DEG C of kinematic viscosity are 41mm2/s）And PAO10（100 DEG C of fortune
Kinetic viscosity is 11mm2/s）Respectively instead of HVI150BS（100 DEG C of kinematic viscosity are 31mm2/s）And HVI500SN（100 DEG C of motions are viscous
Spend for 11mm2/s）；The dosage of each composition is as above.Assay is shown in Table 1.
In the lubricating grease that the present embodiment obtains, on the basis of lubricating grease weight, form and be：Non-newtonian fluid sulfoacid calcium-cycloalkanes
The sour weight % of calcium 38.5；The weight % of lubricating base oil 55.4；The weight % of 12- hydroxy stearic acids calcium 2.4；The weight % of line borate 3.7.
Embodiment 7
The present embodiment is used for the high base number complex calcium lubricating grease for illustrating prepared by the present invention.
Raw material components：Overbased sulfoacid calcium（Total base number is 400mgKOH/g, 6kg）；Overbased calcium alkyl-salicylate（Total base number
For 320mgKOH/g, 24kg）；HVI150BS lubricating base oils（100 DEG C of kinematic viscosity are 31mm2/ s, 30kg）；Aphthenic acids（Always
Acid number is 180mgKOH/g, 2.8kg）；Acetic acid（0.56kg）；Calcium hydroxide（1.8kg）；12- hydroxy stearic acids（2kg）；Boric acid
（2.32kg）；HVI500SN lubricating base oils（100 DEG C of kinematic viscosity are 11mm2/ s, 18kg）.
Method according to embodiment 1 prepares high base number complex calcium lubricating grease, unlike, calcium naphthenate uses total base number
For 320mgKOH/g overbased calcium alkyl-salicylate；The dosage of each composition is as above.Assay is shown in Table 1.
In the lubricating grease that the present embodiment obtains, on the basis of lubricating grease weight, form and be：Non-newtonian fluid sulfoacid calcium-cycloalkanes
The sour weight % of calcium 38.5；The weight % of lubricating base oil 55.4；The weight % of 12- hydroxy stearic acids calcium 2.4；The weight % of line borate 3.7.
Embodiment 8
The present embodiment is used for the high base number complex calcium lubricating grease for illustrating prepared by the present invention.
Raw material components：Calcium sulfonate with high base number（Total base number is 320mgKOH/g, 6kg）；Naphthenate with superhigh base number calcium（Total base number
For 400mgKOH/g, 24kg）；HVI150BS lubricating base oils（100 DEG C of kinematic viscosity are 31mm2/ s, 30kg）；Aphthenic acids（Always
Acid number is 180mgKOH/g, 2.8kg）；Acetic acid（0.56kg）；Calcium hydroxide（1.8kg）；12- hydroxy stearic acids（2kg）；Boric acid
（2.32kg）；HVI500SN lubricating base oils（100 DEG C of kinematic viscosity are 11mm2/ s, 18kg）.
Method according to embodiment 1 prepares high base number complex calcium lubricating grease, unlike, sulfoacid calcium is using total base number
320mgKOH/g calcium sulfonate with high base number；The dosage of each composition is as above.Assay is shown in Table 1.
In the lubricating grease that the present embodiment obtains, on the basis of lubricating grease weight, form and be：Non-newtonian fluid sulfoacid calcium-cycloalkanes
The sour weight % of calcium 38.5；The weight % of lubricating base oil 55.4；The weight % of 12- hydroxy stearic acids calcium 2.4；The weight % of line borate 3.7.
Embodiment 9
The present embodiment is used for the high base number complex calcium lubricating grease for illustrating prepared by the present invention.
Raw material components：Calcium sulfonate with high base number（Total base number is 320mgKOH/g, 6kg）；Overbased calcium alkyl-salicylate（Total base number is
320mgKOH/g, 24kg）；HVI150BS lubricating base oils（100 DEG C of kinematic viscosity are 31mm2/ s, 15kg）；Aphthenic acids（Total acid
It is worth for 180mgKOH/g, 1.8kg）；Methanol（1.0kg）；Acetic acid（0.56kg）；Calcium hydroxide（1.8kg）；12- hydroxy stearic acids
（2kg）；Boric acid（2.32kg）；HVI500SN lubricating base oils（100 DEG C of kinematic viscosity are 11mm2/ s, 33kg）.
Method according to embodiment 1 prepares high base number complex calcium lubricating grease, unlike, sulfoacid calcium is using total base number
320mgKOH/g calcium sulfonate with high base number, calcium naphthenate use the overbased calcium alkyl-salicylate that total base number is 320mgKOH/g；Conversion
Agent uses aphthenic acids, methanol and acetic acid, adds methanol after aphthenic acids is added, then adds acetic acid；The dosage of each composition is such as
On.Assay is shown in Table 1.
In the lubricating grease that the present embodiment obtains, on the basis of lubricating grease weight, form and be：Non-newtonian fluid sulfoacid calcium-cycloalkanes
The sour weight % of calcium 38.4；The weight % of lubricating base oil 55.4；The weight % of 12- hydroxy stearic acids calcium 2.5；The weight % of line borate 3.7.
Embodiment 10
The present embodiment is used for the high base number complex calcium lubricating grease for illustrating prepared by the present invention.
Raw material components：Overbased sulfoacid calcium（Total base number is 400mgKOH/g, 15kg）；Naphthenate with superhigh base number calcium（Always
Base number is 400mgKOH/g, 15kg）；HVI150BS lubricating base oils（100 DEG C of kinematic viscosity are 31mm2/ s, 15kg）；Dodecane
Base benzene sulfonic acid（2.8kg）；Acetic acid（0.56kg）；Calcium hydroxide（5.2kg）；12- hydroxy stearic acids（2kg）；Boric acid（2.32kg）；
Phosphoric acid（3kg）；HVI500SN lubricating base oils（100 DEG C of kinematic viscosity are 11mm2/ s, 33kg）；It is right, right '-diisooctyl hexichol
Amine（0.2kg）.
Method according to embodiment 1 prepares high base number complex calcium lubricating grease, unlike, with DBSA generation
For aphthenic acids；And after adding boric acid and stirring 10 minutes, phosphoric acid is added, stirs 10 minutes, is then warming up to 110 under agitation
DEG C, kept for 45 minutes, dehydration；And treat that temperature is cooled to 110 DEG C, add 0.2kg pair, right '-di-iso-octyldiphenylamine stirring
After 10 minutes, then circulating filtration, homogenizing, degassing obtains finished product；The dosage of each composition is as above.Assay is shown in Table 1.
In the lubricating grease that the present embodiment obtains, on the basis of lubricating grease weight, form and be：Non-newtonian fluid sulfoacid calcium-cycloalkanes
The sour weight % of calcium 36.5；The weight % of lubricating base oil 52.5；The weight % of 12- hydroxy stearic acids calcium 2.3；The weight % of line borate 3.3；Phosphoric acid
The weight % of calcium 5.2；To the p- weight % of di-iso-octyldiphenylamine 0.2.
Embodiment 11
The present embodiment is used for the high base number complex calcium lubricating grease for illustrating prepared by the present invention.
Raw material components：Calcium sulfonate with high base number（Total base number is 320mgKOH/g, 15kg）；Overbased calcium alkyl-salicylate（Total base number
For 320mgKOH/g, 15kg）；；HVI150BS lubricating base oils（100 DEG C of kinematic viscosity are 31mm2/ s, 30kg）；Aphthenic acids（Always
Acid number is 180mgKOH/g, 2.8kg）；Acetic acid（0.56kg）；Calcium hydroxide（3kg）；12- hydroxy stearic acids（2kg）；Boric acid
（2.32kg）；Acetic acid（2kg）；HVI500SN lubricating base oils（100 DEG C of kinematic viscosity are 11mm2/ s, 18kg）, it is right, right '-two
Di-iso-octyldiphenylamine（0.2kg）.
Method according to embodiment 1 prepares high base number complex calcium lubricating grease, unlike, sulfoacid calcium is using total base number
320mgKOH/g calcium sulfonate with high base number, calcium naphthenate use the overbased calcium alkyl-salicylate that total base number is 320mgKOH/g；And
Boric acid is being added, after stirring 10 minutes, acetic acid is being added, stirs 10 minutes, be then warming up to 110 DEG C under agitation；And treat temperature
Degree is cooled to 110 DEG C, adds 0.2kg pair, after right '-di-iso-octyldiphenylamine stirs 10 minutes, then circulating filtration, homogenizing,
Degassing obtains finished product；The dosage of each composition is as above.Assay is shown in Table 1.
In the lubricating grease that the present embodiment obtains, on the basis of lubricating grease weight, form and be：Non-newtonian fluid sulfoacid calcium-cycloalkanes
The sour weight % of calcium 37.3；The weight % of lubricating base oil 53.6；The weight % of 12- hydroxy stearic acids calcium 2.4；The weight % of line borate 3.5；Acetic acid
The weight % of calcium 3.0；To the p- weight % of di-iso-octyldiphenylamine 0.2.
Embodiment 12
The present embodiment is used for the high base number complex calcium lubricating grease for illustrating prepared by the present invention.
Raw material components：Overbased sulfoacid calcium（Total base number is 400mgKOH/g, 24kg）；Naphthenate with superhigh base number calcium（Always
Base number is 400mgKOH/g, 6kg）；HVI150BS lubricating base oils（100 DEG C of kinematic viscosity are 31mm2/ s, 30kg）；Aphthenic acids
（Total acid number is 180mgKOH/g, 2.8kg）；Acetic acid（0.56kg）；Calcium hydroxide（1.8kg）；12- hydroxy stearic acids（2kg）；Boron
Acid（2.32kg）；HVI500SN lubricating base oils（100 DEG C of kinematic viscosity are 11mm2/ s, 18kg）.
A volume be 160L and with heating, stirring, circulation, cooling normal-pressure reaction kettle in add 24kg total base numbers
The naphthenate with superhigh base number calcium and 30kg for being 400mgKOH/g for 400mgKOH/g overbased sulfoacid calcium, 6kg total base numbers
HVI150BS lubricating base oils, stirring, heat to 50 DEG C, constant temperature 10 minutes；2.8kg aphthenic acids is added, temperature control exists
50 DEG C or so, stir 10 minutes；The aqueous acetic acid that 2.8kg concentration is 20 weight % is added, is stirred 10 minutes；80 DEG C are warming up to,
Constant temperature 90 minutes, material retrogradation.
Another volume be 50L and with heating, stirring, circulation, cooling normal-pressure reaction kettle in add 7kg
HVI500SN lubricating base oils, the calcium hydroxide suspension 9kg that solid content is 20 weight % is added at 100 DEG C, stirs 10 points
Clock；2kg12- hydroxy stearic acids are added, are stirred 10 minutes；Add the boric acid aqueous solution that 9.28kg concentration is 25 weight %, stirring 10
Minute, obtain 12- hydroxy stearic acids calcium and line borate.
The 12- hydroxy stearic acids calcium and line borate of gained are all squeezed into a upper kettle, stirred, stirs lower heat up
To 110 DEG C, kept for 45 minutes, dehydration is finally warming up to 200 DEG C of constant temperature 10 minutes.Then, 160 DEG C are cooled to, is added remaining
HVI500SN lubricating base oils；Treat that temperature is cooled to 110 DEG C, circulating filtration, homogenizing, degassing obtain finished product.Assay is shown in Table
1。
In the lubricating grease that the present embodiment obtains, on the basis of lubricating grease weight, form and be：Non-newtonian fluid sulfoacid calcium-cycloalkanes
The sour weight % of calcium 38.5；The weight % of lubricating base oil 55.4；The weight % of 12- hydroxy stearic acids calcium 2.4；The weight % of line borate 3.7.
Embodiment 13
The present embodiment is used for the high base number complex calcium lubricating grease for illustrating prepared by the present invention.
Method according to embodiment 1 prepares high base number complex calcium lubricating grease, unlike, aphthenic acids is replaced with into benzene
Phenol, acetic acid is replaced with into butyric acid.Assay is shown in Table 1.
In the lubricating grease that the present embodiment obtains, on the basis of lubricating grease weight, form and be：Non-newtonian fluid sulfoacid calcium-cycloalkanes
The sour weight % of calcium 38.5；The weight % of lubricating base oil 55.4；The weight % of 12- hydroxy stearic acids calcium 2.4；The weight % of line borate 3.7.
Embodiment 14
The present embodiment is used for the high base number complex calcium lubricating grease for illustrating prepared by the present invention.
Method according to embodiment 1 prepares high base number complex calcium lubricating grease, unlike, aphthenic acids is replaced with into first
Ketone, aqueous acetic acid is replaced with into ether.Assay is shown in Table 1.
In the lubricating grease that the present embodiment obtains, on the basis of lubricating grease weight, form and be：Non-newtonian fluid sulfoacid calcium-cycloalkanes
The sour weight % of calcium 38.5；The weight % of lubricating base oil 55.4；The weight % of 12- hydroxy stearic acids calcium 2.4；The weight % of line borate 3.7.
Comparative example 1
Method according to embodiment 1 prepares complex calcium sulfonate grease, unlike, naphthenate with superhigh base number calcium is with always
The overbased sulfoacid calcium that base number is 400mgKOH/g replaces, 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, form and be：The weight of non-newtonian fluid sulfoacid calcium 38.5
Measure %；The weight % of lubricating base oil 55.4；The weight % of 12- hydroxy stearic acids calcium 2.4；The weight % of line borate 3.7.
By embodiment 1 as can be seen that the extension of the high base number complex calcium lubricating grease of the present invention compared with comparative example 1
The difference of work cone penetration and the cone penetration that works is less than complex calcium sulfonate grease, and water leaching number of dropouts is much smaller than complex calcium sulfonate
Base grease, salt spray test are better than complex calcium sulfonate grease, and water resistant spraying value is less than complex calcium sulfonate grease, steel mesh
Oil value is divided to be much smaller than complex calcium sulfonate grease, tetra-ball machine test value is more than complex calcium sulfonate grease, illustrates the present invention
Mechanical stability, water-resistance and the adhesiveness of high base number complex calcium lubricating grease, resistance to saltfog, colloid stability, extreme pressure resist
Mill property is superior to complex calcium sulfonate grease, and the high base number complex calcium lubricating grease of the present invention lubricates with Composite calcium-sulfonate-batetrapolyurea
Fat equally has the performances such as excellent anticorrosive property and heat-resisting quantity.
By embodiment 1 as can be seen that the high base number complex calcium lubricating grease in situ prepared, tool compared with embodiment 12
There are more preferable mechanical stability, water-resistance and adhesiveness, colloid stability；By embodiment 1 respectively with embodiment 13 and embodiment
14 are compared as can be seen that transforming agent is selected from DBSA, aphthenic acids, methanol, isopropanol, butanol, boric acid, acetic acid
At least one of with water, the high base number complex calcium lubricating grease of preparation, there is more preferable mechanical stability, water-resistance and adhesion
Property, colloid stability.
Each lubricating grease properties of sample data of table 1
Each indication test method：Dropping point：GB/T3498；Work cone penetration and extension work cone penetration：GB/T269；Corrosion：
GB/T7326；Anticorrosive property：GB/T5018；Water drenches number of dropouts：SH/T0109；Salt spray test：SH/T0081；Water resistant is sprayed：SH/
T0643；Stencil oil-dividing：SH/T0324；Tetra-ball machine test：SH/T0202.
Table 1（It is continuous）Each lubricating grease properties of sample data
Each indication test method：Dropping point：GB/T3498；Work cone penetration and extension work cone penetration：GB/T269；Corrosion：
GB/T7326；Anticorrosive property：GB/T5018；Water drenches number of dropouts：SH/T0109；Salt spray test：SH/T0081；Water resistant is sprayed：SH/
T0643；Stencil oil-dividing：SH/T0324；Tetra-ball machine test：SH/T0202.
It will be seen from figure 1 that lubricating grease prepared by embodiment 2 is in 873cm-1-886cm-1There is crystal form calcium carbonate feature in place
Absworption peak.
The high base number complex calcium lubricating grease of the present invention, not only as complex calcium sulfonate grease, have excellent
Anticorrosive property and heat-resisting quantity, but also mechanical stability, water-resistance and adhesion with better than complex calcium sulfonate grease
The performances such as property, resistance to saltfog, colloid stability, extreme pressure anti-wear.The preparation of greases technique of the present invention is simple and environmentally-friendly, into
This is low, and product quality is stable.
The preferred embodiment of the present invention is described in detail above in association with accompanying drawing, still, the present invention is not limited to above-mentioned reality
The detail in mode is applied, in the range of the technology design of the present invention, a variety of letters can be carried out to technical scheme
Monotropic type, these simple variants belong to protection scope of the present invention.
It is further to note that each particular technique feature described in above-mentioned embodiment, in not lance
In the case of shield, can be combined by any suitable means, in order to avoid unnecessary repetition, the present invention to it is various can
The combination of energy no longer separately illustrates.
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 equally be considered as content disclosed in this invention.
Claims (15)
- A kind of 1. high base number complex calcium lubricating grease, it is characterised in that on the basis of lubricating grease weight, including following components：10- 70 weight % non-newtonian fluid sulfoacid calcium-calcium naphthenate；The calcium salt of 1-20 weight % higher fatty acids；1-15 weight %'s is small The calcium salt of molecule inorganic acid and/or lower fatty acid；10-80 weight % base oil, the non-newtonian fluid sulfoacid calcium-aphthenic acids Calcium is in infrared spectrum 873cm-1-886cm-1There is crystal form calcium carbonate characteristic absorption peak in place.
- 2. lubricating grease according to claim 1, wherein, on the basis of lubricating grease weight, including following components：20-65 weights Measure % non-newtonian fluid sulfoacid calcium-calcium naphthenate；The calcium salt of 2-15 weight % higher fatty acids；2-10 weight % small molecule The calcium salt of inorganic acid and/or lower fatty acid；20-70 weight % base oil.
- 3. lubricating grease according to claim 1 or 2, wherein, the non-newtonian fluid sulfoacid calcium-calcium naphthenate is by newton body Sulfoacid calcium and newton body calcium naphthenate convert what is obtained, and the total base number of the non-newtonian fluid sulfoacid calcium-calcium naphthenate is 250- 450mgKOH/g。
- 4. lubricating grease according to claim 1 or 2, wherein, the higher fatty acids is the straight chain fatty that carbon number is 8-20 Acid or hydroxy fatty acid.
- 5. lubricating grease according to claim 4, wherein, the higher fatty acids be selected from laurate, palmitic acid, stearic acid, At least one of 12- hydroxy stearic acids, eicosyl carboxylic acid.
- 6. lubricating grease according to claim 1 or 2, wherein, the molecular weight of small molecule inorganic acid or lower fatty acid is less than Equal to 150.
- 7. lubricating grease according to claim 6, wherein, the small molecule inorganic acid in boric acid, phosphoric acid, sulfuric acid extremely Few one kind, the lower fatty acid are selected from least one of acetic acid, ethanedioic acid, propionic acid, malonic acid, butyric acid, succinic acid.
- 8. the preparation method of the high base number complex calcium lubricating grease in claim 1-7 described in any one, it is characterised in that should Method includes：By non-newtonian fluid sulfoacid calcium-calcium naphthenate, the calcium salt of higher fatty acids, small molecule inorganic acid and/or lower aliphatic Calcium salt and the part basis oil of acid are well mixed, are refined in 180-230 DEG C of constant temperature, add surplus base oil, add necessary add Add agent, obtain finished product.
- 9. the preparation method of the high base number complex calcium lubricating grease in claim 1-7 described in any one, it is characterised in that should Method includes：(1) by newton body sulfoacid calcium, newton body calcium naphthenate and part basis oil Hybrid Heating, transforming agent is added, thing is treated in heating Expect retrogradation；(2) lime or calcium hydroxide are added in step (1) products therefrom, add higher fatty acids, small molecule inorganic acid and/or Lower fatty acid is reacted, and heat up dehydration after reaction；(3) step (2) is reacted into gained mixture and is warming up to 180-230 DEG C of constant temperature refining, added surplus base oil, add necessary Additive, obtain finished product.
- 10. preparation method according to claim 9, wherein, in step (1), by newton body sulfoacid calcium, newton body aphthenic acids Calcium, part basis oil Hybrid Heating add required transforming agent and reacted to 50-80 DEG C, after all transforming agents add, 80-100 DEG C of constant temperature 60-90 minute.
- 11. preparation method according to claim 9, wherein, in step (2), at 85-100 DEG C, add lime or hydrogen-oxygen Change the suspension of calcium, add higher fatty acids, stir 5-20 minutes, add small molecule inorganic acid and/or lower fatty acid, stirring 5-20 minutes, it is warming up to 100-120 DEG C of dehydration.
- 12. preparation method according to claim 9, wherein, in step (3), it is warming up to 180-230 DEG C of 5-20 points of constant temperature Clock；Add surplus base oil, treat that temperature is cooled to 100-120 DEG C, add necessary additive, stir, circulating filtration, homogenizing, Degassing.
- 13. preparation method according to claim 9, wherein, the newton body sulfoacid calcium is calcium mahogany sulfonate and/or synthesis Sulfoacid calcium, the total base number of the newton body sulfoacid calcium is 250-450mgKOH/g；The newton body calcium naphthenate is oil cycloalkanes Sour calcium and/or synthesis calcium naphthenate, the total base number of the newton body calcium naphthenate is 250-450mgKOH/g.
- 14. preparation method according to claim 9, wherein, the transforming agent is selected from fatty alcohol, aliphatic acid, aliphatic ketone, fat Fat aldehyde, fatty amine, ether, calcium carbonate, boric acid, phosphonic acids, carbon dioxide, phenol, aromatic alcohol, aromatic amine, aphthenic acids, C8-C20 alkyl At least one of benzene sulfonic acid and water, the addition of transforming agent are the 2- of newton body sulfoacid calcium and newton body calcium naphthenate gross weight 30%.
- 15. preparation method according to claim 14, wherein, the transforming agent be selected from DBSA, aphthenic acids, At least one of methanol, isopropanol, butanol, boric acid, acetic acid and water, the addition of transforming agent is newton body sulfoacid calcium and newton The 6-22% of body calcium naphthenate gross weight.
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| CN111040855A (en) * | 2019-12-26 | 2020-04-21 | 辽宁海华科技股份有限公司 | Long-life calcium sulfonate-based lubricating grease and preparation method thereof |
| US11661563B2 (en) | 2020-02-11 | 2023-05-30 | Nch Corporation | Composition and method of manufacturing and using extremely rheopectic sulfonate-based greases |
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| CN103122266A (en) * | 2012-12-25 | 2013-05-29 | 乌鲁木齐市隆成实业有限公司 | Composite calcium-sulfonate-base lubricating grease and preparation method thereof |
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| CN101921647A (en) * | 2010-08-04 | 2010-12-22 | 中国海洋石油总公司 | Complex calcium sulfonate grease and preparation method thereof |
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