CN105586129B - Excellent sodium base grease composition of a kind of Wear vesistance and preparation method thereof - Google Patents
Excellent sodium base grease composition of a kind of Wear vesistance and preparation method thereof Download PDFInfo
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Abstract
The invention discloses the sodium base grease compositions that a kind of Wear vesistance is excellent, and on the basis of the weight of lubricant composition, the lubricant composition includes following components：The additive of the lubricating base oil of 65 95 weight %, the sodium base thickening agent of 5 35 weight % and 0.1 15 weight %, the additive contain the compound of structure shown in formula (I).The present invention also provides the preparation methods of the excellent sodium base grease composition of Wear vesistance.The sodium base grease composition of the present invention, due to containing multipurpose additive, drastically increase the anti-attrition ability and oxidation resistance of lubricating grease, the other performance of sodium base grease is influenced simultaneously little, still there is splendid colloid stability so that the lubricant composition can be competent in the harsh working condition such as high temperature, high speed, high load capacity, more water.
Description
Technical field
The present invention relates to lubricating grease fields, and in particular, to a kind of excellent sodium of Wear vesistance containing special additive
Base grease composition and preparation method thereof.
Background technology
Sodium base grease is usually to be made by natural animal-plant grease soda soap or fatty acid sodium soap thickening mineral oil, is had
Higher dropping point, good colloid stability, shear stability.In process of production by changing raw materials for production and preparation process
The product of different appearances and different performance can be made in condition.
CN102021546A reports a kind of aqueous rust preventive for firm product antirust；CN101153236 divides different-grain diameter
The solid powder of cloth is added in lubricating grease, not only increases the water repelling property of lubricating grease, also improves extreme pressure anti-wear；
CN1557922 is prepared for the aqueous sodium base grease containing 8-30% clean waters by adding clean water into sodium base grease,
The fat is a kind of substantially pollution-free to environment, high lubricating effect, has thermal balance to act on and of low cost can be suitable for heavy burden
The lubriation material of lotus sliding bearing；CN102021068A is prepared for a kind of sodium aluminate soap grease for ship, suitable for Ship Propeling
Device and Floating Crane and dredger, 75 DEG C of dropping point or more have good water-resistance, protective and rust-preventing characteristic, existing appropriate
Trace is lubricated, and has corrosion-resisting function, and has the function of to lower mechanicalness noise；US2468098 is containing 5-35% aliphatic acid
0.1-5% acrylic acid sodium salts are added in the lubricating grease of soda soap, reduce the solubility of soda soap in water；Morway in US2591586
Et al. find that methacrylaldehyde and its derivative also can prepare sodium base grease with polymer acid.
Recently as the development of modern industry, the industrial departments such as bearing, automobile, printing and dyeing, mine, metallurgy, aerospace are to profit
The quality of consistent lubricant proposes increasingly harsher requirement, and many lubricant housings are all disposably to fill fat, in the process of running no longer
Supplement is replaced, so higher to the abrasion resistance requirement of fat.
The content of the invention
The purpose of the invention is to meet the high request to the abrasion resistance of lubricating grease, it is excellent to provide a kind of Wear vesistance
Sodium base grease composition and preparation method thereof.
The present inventor has found that the additive in lubricant composition contains structure shown in formula (I) under study for action
Multipurpose additive：
It can make lubricant composition that there are the performances such as excellent anti-attrition is anti-oxidant.
Therefore, to achieve these goals, on the one hand, the present invention provides the sodium base greases that a kind of Wear vesistance is excellent
Composition, on the basis of the weight of lubricant composition, the lubricant composition includes following components：65-95 weight %'s
The additive of lubricating base oil, the sodium base thickening agent of 5-35 weight % and 0.1-15 weight %, the additive contain formula (I) institute
Show the compound of structure：
Preferably, on the basis of the weight of lubricant composition, the lubricant composition includes following components：70-90
The additive of the lubricating base oil of weight %, the sodium base thickening agent of 8-30 weight % and 0.5-10 weight %.
Preferably, on the basis of the weight of lubricant composition, the content of the compound of structure shown in formula (I) is 0.1-10
Weight %, more preferably 1-5 weight %.
On the other hand, the present invention provides a kind of preparation method of the excellent sodium base grease composition of Wear vesistance, institutes
The method of stating includes：
(1) by partial lubrication base oil and higher fatty acids Hybrid Heating, 80-105 DEG C is warming up to, adds in sodium hydroxide,
Saponification is carried out, then optionally, small molecule acid is added in and carries out recombination reaction；
(2) 180-220 DEG C is warming up to be refined；
(3) remaining lubricating base oil is added in, 90-130 DEG C is cooled to, then adds in additive；
(4) ground 2-4 times by three-roller；
Wherein, on the basis of the weight of lubricant composition, the dosage of lubricating base oil is 65-95 weight %, by advanced
The dosage of sodium base thickening agent prepared by aliphatic acid, optional small molecule acid and sodium hydroxide is 5-35 weight %, the use of additive
It measures as 0.1-15 weight %, the additive contains the compound of structure shown in formula (I)：
Preferably, on the basis of the weight of lubricant composition, the dosage of lubricating base oil is 70-90 weight %, by height
The dosage of sodium base thickening agent prepared by grade aliphatic acid, optional small molecule acid and sodium hydroxide is 8-30 weight %, additive
Dosage is 0.5-10 weight %.
Preferably, on the basis of the weight of lubricant composition, the dosage of the compound of structure shown in formula (I) is 0.1-10
Weight %, more preferably 1-5 weight %.
The sodium base grease composition of the present invention, due to containing multipurpose additive, drastically increases the anti-attrition of lubricating grease
Ability and oxidation resistance, while the other performance of sodium base grease is influenced less, still with splendid colloid stability, to make
The harsh working condition such as high temperature, high speed, high load capacity, more water can be competent in by obtaining the lubricant composition.
Other features and advantages of the present invention will be described in detail in subsequent specific embodiment part.
Description of the drawings
Fig. 1 is the reaction equation of (a) the step of preparing multipurpose additive.
Fig. 2 is the reaction equation of (b) the step of preparing multipurpose additive.
Fig. 3 is the hydrogen spectrum spectrogram of multipurpose additive prepared by preparation example.
Fig. 4 is the carbon spectrum spectrogram of multipurpose additive prepared by preparation example.
Fig. 5 is the mass spectrogram of multipurpose additive prepared by preparation example.
Specific embodiment
The specific 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 present invention provides the sodium base grease composition that a kind of Wear vesistance is excellent, using the weight of lubricant composition as
Benchmark, lubricant composition include following components：The lubricating base oil of 65-95 weight %, the sodium base thickening agent of 5-35 weight %
With the additive of 0.1-15 weight %, additive contains the compound of structure shown in formula (I)：
In the present invention, what multipurpose additive referred to is the compound of structure shown in formula (I).
In the present invention, it is preferable that on the basis of the weight of lubricant composition, the lubricant composition is included with the following group
Point：The additive of the lubricating base oil of 70-90 weight %, the sodium base thickening agent of 8-30 weight % and 0.5-10 weight %.
In the present invention, on the basis of the weight of lubricant composition, the content of the compound of structure is preferably shown in formula (I)
0.1-10 weight %, more preferably 1-5 weight %.
It is contemplated that the compound of structure shown in formula (I) is contained and reality by the additive in sodium base grease composition
Existing goal of the invention, even if sodium base grease composition has the performances such as excellent anti-attrition is anti-oxidant.Therefore, for sodium base grease
In each conventional constituents selection, do not limit specifically.
In the present invention, lubricating base oil can be lubricating base oil commonly used in the art, such as can be mineral oil,
At least one of vegetable oil and synthetic oil.100 DEG C of kinematic viscosity of lubricating base oil are preferably 4-60mm2/ s, more preferably 6-
32mm2/s.For the specific species of mineral oil, vegetable oil and synthetic oil, also there is no particular limitation, and it is normal that this field may be employed
Mineral oil, vegetable oil and synthetic oil, for example, mineral oil can select paraffinic base, cycloalkyl series, vegetable oil can be castor
At least one of sesame oil, rapeseed oil, peanut oil and soybean oil etc., synthetic oil can be poly-a-olefin oil (PAO), Esters oil, fluorine
At least one of oil and silicone oil etc..
In the present invention, sodium base thickening agent can be sodium base thickening agent commonly used in the art, for example, can be acid and hydroxide
Sodium reaction generation, acid include higher fatty acids and optional small molecule acid.
In the present invention, " optional ", which refers to have, not to be had." optional small molecule acid " refers to that small molecule acid is
A kind of optional component can include the component, can not also include the component, i.e. sodium base thickening agent of the invention can be by
Higher fatty acids is generated with sodium hydroxide reaction, can also be generated by higher fatty acids and small molecule acid with sodium hydroxide reaction.
Wherein, higher fatty acids can be the aliphatic acid of C12-C25, be preferably lauric acid, palmitic acid, stearic acid and 12-
At least one of hydroxy stearic acid, more preferably stearic acid and/or 12- hydroxy stearic acids.
Wherein, small molecule acid is preferably the carboxylic acid of C4-C12, more preferably benzoic acid, terephthalic acid (TPA), adipic acid, nonyl two
At least one of acid and decanedioic acid.
It will be understood by those skilled in the art that in actual use, sodium hydrate aqueous solution is generally added in, for hydrogen
The concentration of aqueous solution of sodium oxide is without particular/special requirement, such as can be 1-30 weight %.
Above-mentioned sodium base thickening agent may be employed the thinkable various methods of those skilled in the art institute and obtain.
In the present invention, since the multipurpose additive of structure shown in formula (I) and other additives have preferable compatibility, because
This, according to the use needs of lubricating grease, additive of the invention can also contain other antioxidant, extreme pressure anti-wear additives and antirust
At least one of agent.
In the present invention, for other antioxidant, extreme pressure anti-wear additives, antirust agent species and content without particular/special requirement, can
With using the species and content of this field routine.For example, antioxidant can be arylamine kind antioxidant, be preferably diphenylamines, phenyl-
At least one of alpha-naphthylamine and di-iso-octyldiphenylamine, more preferably di-iso-octyldiphenylamine, the content of antioxidant can account for
The 0.01-5 weight % of lubricant composition total weight, preferably 0.1-2.5 weight %；Extreme pressure anti-wear additives can be two thio dioxanes
Base trbasic zinc phosphate, two thio dialkyl amido formic acid molybdenums, two thio dialkyl amido lead formates, molybdenum disulfide, polytetrafluoroethylene (PTFE), two
At least one of butyl antimony dithiocarbamate, tungsten disulfide, selenium disulfide, fluorographite, calcium carbonate and zinc oxide, pole
The content of pressure antiwear additive can account for the 0.5-12 weight % of lubricant composition total weight, be preferably 0.5-5 weight %；Antirust agent
Can be barium mahogany sulfonate, petroleum sodium sulfonate, benzothiazole, benzotriazole, zinc naphthenate and alkenyl succinic acid at least
One kind, the content of antirust agent can account for the 0.01-4.5 weight % of lubricant composition total weight, be preferably 0.1-2 weight %.
In the present invention, the preparation method of the compound of structure preferably includes shown in formula (I)：
(a) aniline, sulfur chloride and 4- chloroanilines are reacted, generate the intermediate M shown in formula (II),
(b) the intermediate M and dimercapto -1,3,4- thiadiazoles that step (a) obtains is carried out nucleophilic in alkaline conditions to take
Generation reaction, generates the multipurpose additive shown in formula (I),
In step (a) of the present invention, the concrete mode that aniline, sulfur chloride and 4- chloroanilines react is preferably included：
(i) under an inert atmosphere, in the first solvent, aniline is fully reacted with sulfur chloride at -20-0 DEG C；
(ii) 4- chloroanilines are added in the reaction system of step (i), reacts 1-3h at 15-30 DEG C.
In the present invention, inert atmosphere can be the inert atmosphere of this field routine, such as can be by gases such as nitrogen, argon gas
It provides.
In step (i) of the present invention, the first solvent is preferably selected from dichloromethane, tetrahydrofuran, toluene, dimethylbenzene and dioxy six
At least one of ring, more preferably dichloromethane and/or tetrahydrofuran, are still more preferably dichloromethane.
In the present invention in step (i), fully reacted and refer to that the reaction was complete, i.e., reaction raw materials are reacted completely.
Method commonly used in the art may be employed to be monitored reaction, to confirm that the reaction was complete, such as thin layer chromatography may be employed
(TLC) or the methods of gas-chromatography, is monitored.
In step (ii) of the present invention, 1-3h is reacted at 15-30 DEG C, preferably after step (i) fully reaction, by reactant
The temperature of system is gradually increased to 15-30 DEG C, adds 4- chloroanilines and carries out reaction 1-3h.It, can be further under the preferable case
Improve reaction yield.
In step (ii) of the present invention, the feed postition of 4- chloroanilines is preferably to add in by several times, such as can divide 3-4 times and add
Enter.Under the preferable case, reaction yield can be further improved.When being added in for gradation, each addition can be identical,
Can not also be same, in order to easy to operate, preferably each addition is identical.
In step (ii) of the present invention, react 1-3h, stop reaction mode can be those skilled in the art it is contemplated that
Various modes, be quenched for example, quencher can be added in, quencher can be quencher commonly used in the art, such as can
Think saturated salt solution.
In the present invention, the dosage of aniline, sulfur chloride and 4- chloroanilines is substantially equimolar amounts, but aniline and sulfur chloride can
With appropriate excessive.The molar ratio of aniline, sulfur chloride and 4- chloroanilines is preferably 0.9-1.5：0.9-1.5：0.8-1.2.
It will be understood by those skilled in the art that in step (a) of the present invention, purer intermediate M, goes back in order to obtain
It needing to post-process the system after reaction, the mode of post processing can include washing, drying, solvent is removed under reduced pressure, for example,
By the reaction system after being quenched respectively with distilled water and saturated common salt water washing, then anhydrous calcium chloride is added at 15-30 DEG C
Or the drier such as anhydrous sodium sulfate, keep 10-60min.After being filtered to remove drier, at 0.01-0.05MPa, 40-60 DEG C
Solvent is removed, to obtain intermediate M.
In step (a) of the present invention, the reaction equation that aniline, sulfur chloride and 4- chloroanilines are reacted is as shown in Figure 1, figure
In 1, the first solvent is not construed as limiting the scope of the present invention using dichloromethane, purpose by way of example only.
In step (b) of the present invention, the condition of nucleophilic substitution preferably includes：Under an inert atmosphere, in the second solvent,
Dimercapto-1,3,4-thiadiazole, alkaline reagent and catalyst are mixed into 10-30min at 15-30 DEG C, then add in intermediate
M is fully reacted.I.e. alkaline condition is provided by alkaline reagent.
" inert atmosphere ", " fully being reacted " are as previously mentioned, details are not described herein.
In the present invention, intermediate M is preferably slowly added to, such as can be added in by several times, can generally divide 3-4 addition.
Under the preferable case, reaction yield can be further improved.When being added in for gradation, each addition can be identical, also may be used
With difference, in order to easy to operate, preferably each addition is identical.
In the present invention, the second solvent is preferably selected from dichloromethane, tetrahydrofuran, toluene, dimethylbenzene, N, N- dimethyl formyls
At least one of amine, more preferably dichloromethane and/or n,N-Dimethylformamide, are still more preferably N, N- dimethyl
Formamide.
In the present invention, alkaline reagent is preferably selected from least one of inorganic bases such as potassium carbonate, sodium carbonate, sodium methoxide.
In the present invention, catalyst is preferably potassium sulfate.
In step (b) of the present invention, the dosage of dimercapto-1,3,4-thiadiazole, alkaline reagent and intermediate M is substantially etc.
Mole, but dimercapto-1,3,4-thiadiazole and alkaline reagent can be suitably excessive.Dimercapto -1,3,4- thiadiazoles, alkalescence examination
The molar ratio of agent and intermediate M are preferably 0.9-3.0：0.9-5.0：0.8-1.5.
In step (b) of the present invention, the dosage of catalyst can be catalytic amount, with mole of dimercapto-1,3,4-thiadiazole
On the basis of number, the dosage of catalyst is preferably 5-100 moles of %, more preferably 10-50 moles of %.
In step (b) of the present invention, reaction equation such as Fig. 2 that dimercapto-1,3,4-thiadiazole and intermediate M are reacted
Shown, in Fig. 2, alkaline reagent does not form the scope of the present invention and limits using potassium carbonate, purpose by way of example only
System.
It will be understood by those skilled in the art that purer final product, i.e. multiple-effect of the invention add in order to obtain
Add agent, the method for the invention for preparing multipurpose additive, which preferably further includes, post-processes the system after reaction, the side of post processing
Formula can include washing, drying, solvent is removed under reduced pressure, for example, the system after abundant reaction to be poured into the acetic acid of 1-10 times of volume
In ethyl ester (or dichloromethane), respectively with distilled water and saturated common salt water washing, then anhydrous calcium chloride is added at 15-30 DEG C
Or the drier such as anhydrous sodium sulfate, keep 10-60min.After being filtered to remove drier, at 0.01-0.05MPa, 40-60 DEG C
Solvent is removed, to obtain final product.
Each step that the method for the compound of structure shown in formula (I) is prepared in the present invention preferably carries out under stiring, for
Mixing speed can be the mixing speed of this field routine, for example, mixing speed can be 100-800rpm without particular/special requirement.
In the present invention, for the first solvent and the second solvent amount without particular/special requirement, can be the solvent of this field routine
Dosage, this is known to those skilled in the art, and details are not described herein.
As described above, it is contemplated that structure shown in formula (I) is contained by the additive in sodium base grease composition
Compound and realize goal of the invention, even if lubricant composition has the performances such as excellent anti-attrition is anti-oxidant.Therefore, for sodium base
Without particular/special requirement method commonly used in the art may be employed, for example, second aspect, the present invention in preparation of greases method
A kind of preparation method of the excellent sodium base grease composition of Wear vesistance is additionally provided, this method includes：
(1) by partial lubrication base oil and higher fatty acids Hybrid Heating, 80-105 DEG C is warming up to, adds in sodium hydroxide,
Saponification is carried out, then optionally, small molecule acid is added in and carries out recombination reaction；
(2) 180-220 DEG C is warming up to be refined；
(3) remaining lubricating base oil is added in, 90-130 DEG C is cooled to, then adds in additive；
(4) ground 2-4 times by three-roller；
Wherein, on the basis of the weight of lubricant composition, the dosage of lubricating base oil is 65-95 weight %, by advanced
The dosage of sodium base thickening agent prepared by aliphatic acid, optional small molecule acid and sodium hydroxide is 5-35 weight %, the use of additive
It measures as 0.1-15 weight %, additive contains the compound of structure shown in formula (I)：
In the method for the present invention, it is preferable that on the basis of the weight of lubricant composition, the dosage of lubricating base oil is 70-
90 weight %, the dosage of the sodium base thickening agent prepared by higher fatty acids, optional small molecule acid and sodium hydroxide is 8-30 weights
% is measured, the dosage of additive is 0.5-10 weight %.
In the method for the present invention, the molar ratio of the total amount and sodium hydroxide of higher fatty acids and optional small molecule acid is preferably
Stoichiometric ratio, sodium hydroxide can also excess 1-10 weight %.The molar ratio of higher fatty acids and optional small molecule acid is excellent
Elect 1 as:0.1-2.It will be understood by those skilled in the art that according to by higher fatty acids, optional small molecule acid and hydrogen-oxygen
Change the dosage of sodium base thickening agent prepared by sodium, counter can release the dosage of higher fatty acids, small molecule acid and sodium hydroxide, this is
Known to one of skill in the art, details are not described herein.
In the present invention, can also not have as previously mentioned, " optional " refers to have.In step (1), " and then optionally, add
Enter small molecule acid and carry out recombination reaction " refer to that " add in small molecule acid progress recombination reaction " is an optional step, it can be with
Including the step, the step can not also be included；It is a kind of optional component that " optional small molecule acid ", which refers to small molecule acid,
It can include the component, the component can not also be included；" molar ratio of higher fatty acids and optional small molecule acid is 1:0.1-
2 " refer to when containing small molecule acid, and the molar ratio of higher fatty acids and small molecule acid is preferably 1:0.1-2.In short, ability
Field technique personnel should be understood that the sodium base thickening agent of the present invention can be generated by higher fatty acids and sodium hydroxide reaction,
It can also be generated by higher fatty acids and small molecule acid with sodium hydroxide reaction.
In the method for the present invention, on the basis of the weight of lubricant composition, the dosage of the compound of structure is excellent shown in formula (I)
Elect 0.1-10 weight % as, more preferably 1-5 weight %.
It will be understood by those skilled in the art that in the method for the present invention, the dosage of lubricating base oil is partial lubrication base
The sum of the dosage of plinth oil and the dosage of remaining lubricating base oil.Partial lubrication base oil and the weight ratio of remaining lubricating base oil are excellent
Elect 50-75 as:25-50.
In the method for the present invention step (1), 80-95 DEG C is preferably warming up to, the saponification time is preferably 0.1-1.5h, saponification
Reaction time can according to whether carried out including recombination reaction step it is further preferred, when not including recombination reaction step, saponification
Reaction time is more preferably 0.2-1.5h, further preferably 0.5-1h；When including recombination reaction step, the saponification time
More preferably 0.1-1h, further preferably 0.2-0.8h, complex reaction time is preferably 0.1-1h, more preferably 0.2-
0.8h." optional complex reaction time is 0.1-1h " refers to that complex reaction time is preferred when including recombination reaction step
For 0.1-1h.
In the method for the present invention step (2), 190-210 DEG C is preferably warming up to, the time of refining is preferably 5-15min.
Each step of the method for the present invention preferably carries out under stiring, can be this field for mixing speed without particular/special requirement
Conventional mixing speed, for example, mixing speed can be 20-400rpm.
Lubricating base oil, higher fatty acids, small molecule acid, additive are as previously mentioned, details are not described herein.
Embodiment
The present invention is further illustrated for following embodiment, but is not intended to limit the present invention.
In the following Examples and Comparative Examples：
The monitoring method that the reaction was complete：Thin-layer chromatography chromatography (TLC) fluorescence developing method.
Gross production rate=final product mole/aniline moles × 100%
The physico-chemical analysis method of product：Constituent content is measured by inductively coupled plasma ion emission spectroscopy method.
Structure characterization methods：Nuclear magnetic resonance method (1H hydrogen is composed,13C carbon is composed), high resolution mass spectrum.
Preparation example
Nitrogen protection is filled in the 500ml flasks with electromagnetic agitation sub (mixing speed 300rpm), adds in 150ml
Dichloromethane, then add in 0.2mol sulfur chloride, after being fully cooled in ice-water bath, add in the aniline of 0.2mol.Monitoring
Ice-water bath is removed to after the reaction was complete, 25 DEG C is placed at room temperature, after reaction system is gradually increased to 25 DEG C, is added three times 4- chlorine
Aniline is reacted, and each addition is identical, adds in 4- chloroanilines 0.15mol altogether.30ml saturations are added in after when sustained response 2 is small
Reaction is quenched in saline solution, and then reaction system is transferred in separatory funnel, respectively with 50ml distilled water and 50ml saturated salt solutions
Washing, and add in 10g anhydrous sodium sulfates dry 20min at 25 DEG C.Filtrate after filtering is evaporated off molten under 40 DEG C, 0.05MPa
Agent obtains intermediate M1.
Nitrogen protection is filled in the 500ml flasks with electromagnetic agitation sub (mixing speed 400rpm), adds in 150ml
DMF (n,N-Dimethylformamide), then add in 0.2mol dimercapto-1,3,4-thiadiazoles and 0.2mol potassium carbonate,
The potassium sulfate of 0.05mol stirs 20 minutes at 25 DEG C, is added three times above-mentioned intermediate M1, and each addition is identical, adds in altogether
Intermediate M1 0.12mol.Then reaction system is added in 250ml ethyl acetate by monitoring to the reaction was complete, and be transferred to liquid separation leakage
In bucket, respectively with 100ml distilled water (twice) and 50ml saturated common salt water washings, and 15g anhydrous sodium sulfates are added at 25 DEG C
Dry 20min.Solvent is evaporated off under 40 DEG C, 0.03MPa in filtrate after filtering, obtains final product S1.Calculating gross production rate is
76%.
The physico-chemical analysis data of product are as follows：Sulfur content, 41.3%；Nitrogen content, 13.9%.
S1 is subjected to structural characterization, respectively obtain hydrogen spectrum, carbon spectrum and high resolution mass spec spectrogram, see respectively Fig. 3, Fig. 4 and
Fig. 5.
Physico-chemical analysis data, Fig. 3, Fig. 4 and Fig. 5 from above-mentioned preparation example can be seen that S1 with the knot shown in formula (I)
Structure.
Embodiment 1
The present embodiment is used to illustrate sodium base grease composition of the present invention and preparation method thereof.
(1) by 675 grams of 150BS base oils, (100 DEG C of viscosity are 31mm2/ s, similarly hereinafter) add with 74.5 grams of 12- hydroxy stearic acids
Enter in fat kettle processed, the agitating and heating under 180rpm, be warming up to 95 DEG C, add in the aqueous solution (concentration 5 containing 10.5 grams of sodium hydroxides
Weight %), carry out saponification 0.5h；
(2) 190 DEG C are warming up to, refines 8min；
(3) 225 grams of 150BS base oils are added in, stirring is cooled to 120 DEG C, adds in 16 grams of S1, is stirred under 180rpm equal
It is even；
(4) 2 times are ground into fat by three-roller.Properties of product are as shown in table 1.
In the lubricating grease that the present embodiment obtains, on the basis of lubricating grease weight, form and be：8 weight of 12- hydroxyl sodium stearates
Measure %；90 weight % of lubricating base oil；2 weight % of S1.
Embodiment 2
The present embodiment is used to illustrate sodium base grease composition of the present invention and preparation method thereof.
(1) by 350 grams of 500SN base oils, (100 DEG C of viscosity are 10mm2/ s, similarly hereinafter) and 270.2 grams of 12- hydroxy stearic acids
In addition fat kettle, agitating and heating, is warming up to 85 DEG C at 200 rpm, adds in the aqueous solution (concentration containing 37.8 grams of sodium hydroxides
For 15 weight %), carry out saponification 1h；
(2) 210 DEG C are warming up to, refines 5min；
(3) 350 grams of 500SN base oils are added in, stirring is cooled to 105 DEG C, adds in 10 grams of S1, and stirring is equal at 200 rpm
It is even；
(4) 3 times are ground into fat by three-roller.Properties of product are as shown in table 1.
In the lubricating grease that the present embodiment obtains, on the basis of lubricating grease weight, form and be：29 weight of 12- hydroxyl sodium stearates
Measure %；70 weight % of lubricating base oil；1 weight % of S1.
Embodiment 3
The present embodiment is used to illustrate sodium base grease composition of the present invention and preparation method thereof.
(1) by 500 grams of PAO6 synthetic hydrocarbon oils, (100 DEG C of viscosity are 5.8mm2/ s, similarly hereinafter) and 185.6 grams of stearic acid addition systems
In fat kettle, agitating and heating, is warming up to 80 DEG C at 300 rpm, and adding in the aqueous solution containing 27.3 grams of sodium hydroxides, (concentration is 20 weights
Measure %), carry out saponification 0.8h；
(2) 195 DEG C are warming up to, refines 15min；
(3) 250 grams of PAO6 synthetic hydrocarbon oils are added in, stirring is cooled to 100 DEG C, adds in 50 grams of S1, and stirring is equal at 300 rpm
It is even；
(4) 3 times are ground into fat by three-roller.Properties of product are as shown in table 1.
In the lubricating grease that the present embodiment obtains, on the basis of lubricating grease weight, form and be：20 weight % of odium stearate；Profit
75 weight % of sliding base oil；5 weight % of S1.
Embodiment 4
The present embodiment is used to illustrate sodium base grease composition of the present invention and preparation method thereof.
(1) by the miscella of 600 grams of 500SN and 150BS, (100 DEG C of viscosity are 13mm2/ s, similarly hereinafter) and 139.3 grams of tristearin
Acid is added in fat kettle processed, the agitating and heating under 230rpm, is warming up to 90 DEG C, and it is (dense to add in the aqueous solution containing 20.3 grams of sodium hydroxides
Spend for 25 weight %), carry out saponification 0.6h；
(2) 200 DEG C are warming up to, refines 10min；
(3) miscella of 220 grams of 500SN and 150BS is added in, stirring is cooled to 120 DEG C, 30 grams of S1 is added in, in 230rpm
Under stir evenly；
(4) 2 times are ground into fat by three-roller.Properties of product are as shown in table 1.
In the lubricating grease that the present embodiment obtains, on the basis of lubricating grease weight, form and be：15 weight % of odium stearate；Profit
82 weight % of sliding base oil；3 weight % of S1.
Comparative example 1
Method according to embodiment 4 prepares sodium base grease, unlike, it is added without S1.Properties of product are as shown in table 1.
In the lubricating grease that this comparative example obtains, on the basis of lubricating grease weight, form and be：15.5 weight % of odium stearate,
84.5 weight % of lubricating base oil.
Embodiment 5
The present embodiment is used to illustrate sodium base grease composition of the present invention and preparation method thereof.
(1) by 540 grams of 500SN base oils, (100 DEG C of viscosity are 10mm2/ s, similarly hereinafter) and 41.14 grams of 12- hydroxy stearic acids
In addition fat kettle, the agitating and heating under 180rpm is warming up to 80 DEG C, adds in the aqueous solution (concentration containing 11.28 grams of sodium hydroxides
For 5 weight %), saponification 0.2h is carried out, then 16.84 grams of benzoic acid are added in into system, carry out recombination reaction 0.5h；
(2) 190 DEG C are warming up to, refines 15min；
(3) 180 grams of 500SN base oils are added in, stirring is cooled to 90 DEG C, adds in 16 grams of S1, is stirred evenly under 180rpm；
(4) 2 times are ground into fat by three-roller.Properties of product are as shown in table 2.
In the lubricating grease that the present embodiment obtains, on the basis of lubricating grease weight, form and be：5.5 weight of 12- hydroxyl sodium stearates
Measure %；2.5 weight % of sodium benzoate；90 weight % of lubricating base oil；2 weight % of S1.
Embodiment 6
The present embodiment is used to illustrate sodium base grease composition of the present invention and preparation method thereof.
(1) by 178 grams of 150BS base oils, (100 DEG C of viscosity are 31mm2/ s, similarly hereinafter) and 121.18 grams of 12- hydroxy stearic acids
In addition fat kettle, agitating and heating, is warming up to 85 DEG C at 200 rpm, adds in the aqueous solution (concentration containing 23.26 grams of sodium hydroxides
For 8 weight %), saponification 0.8h is carried out, then 13.4 grams of terephthalic acid (TPA)s are added in into system, carry out recombination reaction 0.2h；
(2) 210 DEG C are warming up to, refines 5min；
(3) 175 grams of 150BS base oils are added in, stirring is cooled to 100 DEG C, adds in 5.1 grams of S1, and stirring is equal at 200 rpm
It is even；
(4) 3 times are ground into fat by three-roller.Properties of product are as shown in table 2.
In the lubricating grease that the present embodiment obtains, on the basis of lubricating grease weight, form and be：12- hydroxyl sodium stearates 25.65
Weight %；3.35 weight % of para-phthalic sodium；70 weight % of lubricating base oil；S11 weight %.
Embodiment 7
The present embodiment is used to illustrate sodium base grease composition of the present invention and preparation method thereof.
(1) by 200 grams of PAO6 synthetic hydrocarbon oils, (100 DEG C of viscosity are 5.8mm2/ s, similarly hereinafter) and 59.6 grams of stearic acid addition systems
In fat kettle, agitating and heating, is warming up to 90 DEG C at 300 rpm, and adding in the aqueous solution containing 17.26 grams of sodium hydroxides, (concentration is 15 weights
Measure %), saponification 0.8h is carried out, then 21.19 grams of decanedioic acid are added in into system, carry out recombination reaction 0.6h；
(2) 200 DEG C are warming up to, refines 8min；
(3) 137.5 grams of PAO6 synthetic hydrocarbon oils are added in, stirring is cooled to 110 DEG C, adds in 22.5 grams of S1, stirs at 300 rpm
It mixes uniformly；
(4) 3 times are ground into fat by three-roller.Properties of product are as shown in table 2.
In the lubricating grease that the present embodiment obtains, on the basis of lubricating grease weight, form and be：14.27 weight % of odium stearate；
5.73 weight % of decanedioic acid sodium；75 weight % of lubricating base oil；5 weight % of S1.
Embodiment 8
The present embodiment is used to illustrate sodium base grease composition of the present invention and preparation method thereof.
(1) by the miscella of 350 grams of 500SN and 150BS, (100 DEG C of viscosity are 14mm2/ s, similarly hereinafter) and 45.79 grams of tristearin
Acid is added in fat kettle processed, the agitating and heating under 230rpm, is warming up to 95 DEG C, and it is (dense to add in the aqueous solution containing 19.89 grams of sodium hydroxides
Spend for 18 weight %), saponification 0.5h is carried out, then 39.59 grams of decanedioic acid are added in into system, carry out recombination reaction 0.4h；
(2) 205 DEG C are warming up to, refines 12min；
(3) miscella of 175 grams of 500SN and 150BS is added in, stirring is cooled to 130 DEG C, adds in 19.2 grams of S1,
It is stirred evenly under 230rpm；
(4) 2 times are ground into fat by three-roller.Properties of product are as shown in table 2.
In the lubricating grease that the present embodiment obtains, on the basis of lubricating grease weight, form and be：7.7 weight % of odium stearate；The last of the ten Heavenly stems
7.3 weight % of diacid sodium；82 weight % of lubricating base oil；3 weight % of S1.
Comparative example 2
Method according to embodiment 8 prepares sodium base grease, unlike, it is added without S1.Properties of product are as shown in table 2.
In the lubricating grease that this comparative example obtains, on the basis of lubricating grease weight, form and be：8 weight % of odium stearate；The last of the ten Heavenly stems two
Sour 7.5 weight % of sodium；84.5 weight % of lubricating base oil.
Table 1
Each indication test method：Dropping point：GB/T 3498；Work cone penetration：GB/T 269；Oxidation onset temperature：ASTM
D5483；Mechanical admixture：Acid decomposition；Copper corrosion：GB/T 7326；Anticorrosive property：GB/T 5018；Coefficient of friction：SH/T
0847。
Table 2
Each indication test method：Dropping point：GB/T 3498；Work cone penetration：GB/T 269；Oxidation stability：SH/T
0325；Stencil oil-dividing：SH/T 0324；Copper corrosion：GB/T 7326；Anticorrosive property：GB/T 5018；Coefficient of friction：SH/T
0847。
It will be understood by those skilled in the art that work cone penetration is smaller, the thickening performance of grease thickener is better；
Oxidation onset temperature is higher, and the oxidation resistance of lubricating grease is better；Oxidation stability is smaller, and the antioxygenic property of lubricating grease is got over
It is good；Stencil oil-dividing value is smaller, and the colloid stability of lubricating grease is better；Coefficient of friction is smaller, and the antifriction performance of lubricating grease is better.
By embodiment 4 compared with comparative example 1, by embodiment 8 compared with comparative example 2, it can be seen that the present invention
Lubricating grease have better inoxidizability, colloid stability and antifriction performance.
The sodium base grease composition of the present invention, due to containing multipurpose additive, drastically increases the anti-attrition of lubricating grease
Ability and oxidation resistance, while the other performance of sodium base grease is influenced less, still with splendid colloid stability, to make
The harsh working condition such as high temperature, high speed, high load capacity, more water can be competent in by obtaining the lubricant composition.
The preferred embodiment of the present invention is described in detail above in association with attached drawing, still, the present invention is not limited to above-mentioned realities
The detail in mode is applied, within the scope of the technical concept of the present invention, a variety of letters can be carried out to technical scheme
Monotropic type, these simple variants all belong to the scope of protection of the present invention.
It is further to note that the specific technical features described in the above specific embodiments, 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 also be regarded as the disclosure of the present invention.
Claims (21)
1. a kind of excellent sodium base grease composition of Wear vesistance, on the basis of the weight of lubricant composition, the lubrication
Oil/fat composition includes following components：The lubricating base oil of 65-95 weight %, the sodium base thickening agent of 5-35 weight % and 0.1-15 weights
Measure the additive of %, which is characterized in that the additive contains the compound of structure shown in formula (I)：
2. lubricant composition according to claim 1, wherein, on the basis of the weight of lubricant composition, the profit
Grease composition includes following components：The lubricating base oil of 70-90 weight %, the sodium base thickening agent and 0.5-10 of 8-30 weight %
The additive of weight %.
3. lubricant composition according to claim 1 or 2, wherein, on the basis of the weight of lubricant composition, formula
(I) content of the compound of structure shown in is 0.1-10 weight %.
4. lubricant composition according to claim 3, wherein, on the basis of the weight of lubricant composition, formula (I) institute
The content for showing the compound of structure is 1-5 weight %.
5. lubricant composition according to claim 1 or 2, wherein, the lubricating base oil is mineral oil, vegetable oil and
At least one of synthetic oil.
6. lubricant composition according to claim 1 or 2, wherein, the sodium base thickening agent is anti-with sodium hydroxide for acid
It should generate, the acid includes higher fatty acids and optional small molecule acid.
7. lubricant composition according to claim 6, wherein, the higher fatty acids is the aliphatic acid of C12-C25, institute
State the carboxylic acid that small molecule acid is C4-C12.
8. lubricant composition according to claim 7, wherein, the higher fatty acids is lauric acid, palmitic acid, tristearin
Acid and at least one of 12- hydroxy stearic acids, the small molecule acid is benzoic acid, terephthalic acid (TPA), adipic acid, azelaic acid and
At least one of decanedioic acid.
9. lubricant composition according to claim 1 or 2, wherein, the additive is also containing other antioxidant, pole
Press at least one of antiwear additive and antirust agent.
10. lubricant composition according to claim 9, wherein, the antioxidant is arylamine kind antioxidant.
11. lubricant composition according to claim 10, wherein, the antioxidant is diphenylamines, phenyl-α-naphthylamine and
At least one of di-iso-octyldiphenylamine.
12. lubricant composition according to claim 9, wherein, the extreme pressure anti-wear additives are two thio Acidic phosphates
Zinc, two thio dialkyl amido formic acid molybdenums, two thio dialkyl amido lead formates, molybdenum disulfide, polytetrafluoroethylene (PTFE), dibutyl two
At least one of thiocarbamic acid antimony, tungsten disulfide, selenium disulfide, fluorographite, calcium carbonate and zinc oxide.
13. lubricant composition according to claim 9, wherein, the antirust agent is barium mahogany sulfonate, mahogany acid
At least one of sodium, benzothiazole, benzotriazole, zinc naphthenate and alkenyl succinic acid.
14. the preparation method of lubricant composition described in claim 1, the described method includes：
(1) by partial lubrication base oil and higher fatty acids Hybrid Heating, 80-105 DEG C is warming up to, adds in sodium hydroxide, is carried out
Then optionally saponification, adds in small molecule acid and carries out recombination reaction；
(2) 180-220 DEG C is warming up to be refined；
(3) remaining lubricating base oil is added in, 90-130 DEG C is cooled to, then adds in additive；
(4) ground 2-4 times by three-roller.
15. the method according to claim 11, wherein, on the basis of the weight of lubricant composition, lubricating base oil
Dosage is 70-90 weight %, by the dosage of sodium base thickening agent prepared by higher fatty acids, optional small molecule acid and sodium hydroxide
For 8-30 weight %, the dosage of additive is 0.5-10 weight %.
16. the method according to claims 14 or 15, wherein, on the basis of the weight of lubricant composition, shown in formula (I)
The dosage of the compound of structure is 0.1-10 weight %.
17. the method according to claim 11, wherein, on the basis of the weight of lubricant composition, structure shown in formula (I)
Compound dosage be 1-5 weight %.
18. the method according to claims 14 or 15, wherein, the partial lubrication base oil and the remaining lubrication base
The weight ratio of oil is 50-75:25-50.
19. the method according to claims 14 or 15, wherein, the molar ratio of higher fatty acids and optional small molecule acid is
1:0.1-2。
20. the method according to claims 14 or 15, wherein, in step (1), 80-95 DEG C is warming up to, the saponification time
For 0.1-1.5h, optional complex reaction time is 0.1-1h.
21. the method according to claims 14 or 15, wherein, in step (2), 190-210 DEG C is warming up to, the refining
Time is 5-15min.
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| CN107254341A (en) * | 2017-06-16 | 2017-10-17 | 佛山赛威光电技术有限公司 | A kind of compound potassium base grease and preparation method thereof |
| CN107502417B (en) * | 2017-08-01 | 2020-01-31 | 太原理工大学 | layered potassium calcium sodium phosphate grease composition and preparation method thereof |
| CN109679714B (en) * | 2017-10-18 | 2022-06-24 | 中国石油化工股份有限公司 | Composite sodium-based lubricating grease and preparation method thereof |
| CN112646652A (en) * | 2019-10-12 | 2021-04-13 | 中国石油化工股份有限公司 | Lubricating grease for textile machinery and preparation method thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5175224A (en) * | 1988-02-26 | 1992-12-29 | Petrochemie Danubia Gesellschaft M.B.H. | Polyimide from bis-maleimide having azole ring |
| JPH05142725A (en) * | 1991-11-22 | 1993-06-11 | Fuji Photo Film Co Ltd | Color reversal photographic sensitive material |
| US5336420A (en) * | 1991-05-08 | 1994-08-09 | Mobil Oil Corporation | Antioxidants for functional fluids |
| CN1946656A (en) * | 2004-02-17 | 2007-04-11 | 托马斯·E·约翰逊 | Methods, compositions, and apparatuses for forming macrocyclic compounds |
| CN102021068A (en) * | 2009-09-15 | 2011-04-20 | 俞磊 | Sodium aluminate soap grease for ship |
-
2014
- 2014-10-23 CN CN201410571340.XA patent/CN105586129B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5175224A (en) * | 1988-02-26 | 1992-12-29 | Petrochemie Danubia Gesellschaft M.B.H. | Polyimide from bis-maleimide having azole ring |
| US5336420A (en) * | 1991-05-08 | 1994-08-09 | Mobil Oil Corporation | Antioxidants for functional fluids |
| JPH05142725A (en) * | 1991-11-22 | 1993-06-11 | Fuji Photo Film Co Ltd | Color reversal photographic sensitive material |
| CN1946656A (en) * | 2004-02-17 | 2007-04-11 | 托马斯·E·约翰逊 | Methods, compositions, and apparatuses for forming macrocyclic compounds |
| CN102021068A (en) * | 2009-09-15 | 2011-04-20 | 俞磊 | Sodium aluminate soap grease for ship |
Non-Patent Citations (1)
| Title |
|---|
| 1,3,4-噻二唑衍生物的合成及其抗腐减摩性能;刘琳等;《石油化工》;20111031;第40卷(第10期);1089-1093 * |
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