CN102504920B - Polyurea calcium acetate lubricating grease and preparation method thereof - Google Patents
Polyurea calcium acetate lubricating grease and preparation method thereof Download PDFInfo
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- CN102504920B CN102504920B CN2011103317096A CN201110331709A CN102504920B CN 102504920 B CN102504920 B CN 102504920B CN 2011103317096 A CN2011103317096 A CN 2011103317096A CN 201110331709 A CN201110331709 A CN 201110331709A CN 102504920 B CN102504920 B CN 102504920B
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- lubricating grease
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- calcium acetate
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Abstract
The invention relates to polyurea calcium acetate lubricating grease and a preparation method thereof. The polyurea calcium acetate lubricating grease comprises the following components in percentage based on the total weight of the raw materials of the lubricating grease: 25-63% of base oil, 3-5% of 4,4'-methylene bis(phenyl isocyanate), 2-10% of organic amine, 20-55% of high-base-number calcium sulfonate, 10-15% of glacial acetic acid, 0.1-1% of antioxidant and 0.01-0.3% of corrosion inhibitor. Meanwhile, the invention also provides a preparation method realizing high yield and good quality. Compared with the common extreme pressure lithium-based lubricating grease and extreme pressure complex lithium-based lubricating grease, the polyurea calcium acetate lubricating grease provided by the invention has excellent anti-wear extreme pressure performance, antirust performance, colloid stability and water resistance without adding the additives such as extreme pressure anti-wear additives, antirust agents and the like.
Description
Technical field
The present invention relates to field of lubricant, particularly, relate to a kind of polyurea calcium acetate lubricating grease and preparation method thereof.
Background technology
Lubricating of the mechanical means of using under harsh working condition, lubricated as the mechanical means that turns round under the bad working environments conditions such as high temperature, heavy loading, humidity (water pouring), acid-alkali medium, adopt general extreme pressure lithium base lubricating grease or extreme pressure compound lithium base grease to be difficult to meet service requirements.For example the steelmaking equipment many places are drenched under operating mode and are worked in high temperature, humidity or water, and while adopting extreme pressure lithium base lubricating grease or extreme pressure compound lithium base grease, lubricating grease is easy thinning loss at high temperature.Simultaneously under the effect of water, the problem such as the colloidal stability extreme difference of these lubricating grease, also can cause the thinning loss of lubricating grease, thereby cause equipment lubrication bad, and work-ing life is short.
Polyurea calcium acetate lubricating grease has higher use temperature, good water repelling property, colloidal stability, resistance to acids and bases and lubricity, the lubricating requirement of the mechanical means of using under the harsh work condition environment of meeting a cassation.
Summary of the invention
The invention provides a kind of polyurea calcium acetate lubricating grease formula and prepare the product method, compare with the extreme pressure compound lithium base grease with extreme pressure lithium base lubricating grease, just there are fabulous extreme pressure and antiwear behavior, colloidal stability, water repelling property and rustless property etc. when not adding extreme-pressure anti-friction additive and rust-preventive agent; And provide a kind of easy and simple to handle, preparation method that quality product is high.
In order to solve the problems of the technologies described above, the invention provides following technical scheme:
A kind of polyurea calcium acetate lubricating grease, comprise following component, all to account for the percentage calculation of raw material for lubricating grease gross weight, 25～63% base oil, 3～5% 4,4'-methylene-bis phenylcarbimide, 2～10% organic amine, 20～55% calcium sulfonate with high base number, 10～15% glacial acetic acid, 0.1～1% oxidation inhibitor, 0.01～0.3% corrosion inhibitor.
Further, base oil is mineral oil, as: a kind of, two or more the mixture of No. 100 machinery oil, HVI500,120BS, 150BS etc., 100 ℃ of kinematic viscosity are 8～50mm
2/ s.
Further, organic amine is the primary amine such as aliphatic amide, Cycloalkyl amine, arylamine, as: a kind of, two or more the mixture of amino dodecane, stearylamine, aniline, para-totuidine, hexahydroaniline etc.
Further, calcium sulfonate with high base number is calcium mahogany sulfonate or calcium alkylbenzenesulfonate, can be also their mixture, and the total basicnumber of calcium sulfonate with high base number is 270～450mgKOH/g.
Further, oxidation inhibitor is phenol type, amine type oxidation inhibitor, as: the mixture of a kind of, two or more oxidation inhibitor of 2,6 ditertiary butyl p cresol (T501), di-iso-octyldiphenylamine, N-phenyl-a-naphthylamine (T531), N-Phenyl beta naphthylamine, pentanoic etc.
Further, corrosion inhibitor is 124 Triazole and derivative, thiadiazoles and derivative thereof, as: a kind of, two or more the mixture of T406, T551, T553, T561 T706 etc.
The preparation method of above-mentioned polyurea calcium acetate lubricating grease, step is as follows: (1) is by part base oil and whole 4,4'-methylene-bis phenylcarbimide adds in reaction vessel, be stirred and heated to 40～50 ℃, then the organic amine liquid that under agitation adds fusing, heat to 100～110 ℃, stir isothermal reaction 10 minutes; (2) again calcium sulfonate with high base number is added in the reaction vessel of step (1) to ice acetic acid slowly under stirring; Finish, stir and be warmed up to 150～160 ℃, add oxidation inhibitor and rut preventives and be uniformly mixed, stop heating; (3) add whole excess oil under the stirring, stir and be cooled to 80～100 ℃, the degassed product that obtains of homogenizing.
The invention has the beneficial effects as follows:
Polyurea calcium acetate lubricating grease of the present invention is compared with common extreme pressure lithium base lubricating grease and extreme pressure compound lithium base grease, just has following advantage when not adding the additives such as extreme-pressure anti-friction additive, rust-preventive agent:
1, outstanding abrasion resistant extreme-pressure performance, rustless property.Because calcium acetate itself is a kind of extreme pressure anti-wear additives, simultaneously because polyurea grease is the organic compound with polarity, polyurea thickening agent itself very easily is adsorbed on metallic surface, with this, when not adding extreme-pressure anti-friction additive, lubricating grease of the present invention just has outstanding abrasion resistant extreme-pressure performance and rustless property;
2, better colloid-stabilised performance.The reticulated structure that polyurea thickening agent forms, make the structure of lubricating grease more stable.Therefore, lubricating grease of the present invention has better colloidal stability;
3, better water repelling property.Polyurea thickening agent be polar organic compound, meet water and be difficult for emulsification and more be conducive to being adsorbed on metallic surface, therefore, lubricating grease of the present invention has better water repelling property, can meet the lubricated of high temperature, water drench, the severe rugged environments such as moist are used mechanical means.
Embodiment
Below the preferred embodiments of the present invention are described, should be appreciated that preferred embodiment described herein, only for description and interpretation the present invention, is not intended to limit the present invention.
Embodiment 1
In reaction vessel, add 180.5 kilograms of 120BS and 30 kilograms of MDI, stirring heating is warmed up to 40～50 ℃, adds the stearylamine of 64.6 kilograms of fusings, heats to 100～110 ℃, stirs isothermal reaction 10 minutes.395 kilograms of high base number calcium alkylbenzenesulfonates that is 300mgKOH/g by total basicnumber add in reaction vessel, ice acetic acid 120 kg slowly under stirring.Finish, stir and be warmed up to 150～160 ℃, add 1 kilogram of 10 kilograms, pentanoic oxidation inhibitor and 124 Triazole rut preventives, be uniformly mixed 5 minutes, stop heating.Add 198.9 kilograms of 120BS under stirring and be cooled to 80～100 ℃, obtaining product after homogenizing is degassed.The performance of the present embodiment products obtained therefrom is in Table 1.
Embodiment 2
In reaction vessel, add 180.5 kilograms of HVI500 and 30 kilograms of MDI, stirring heating is warmed up to 40～50 ℃, adds the stearylamine of 64.6 kilograms of fusings, heats to 100～110 ℃, stirs isothermal reaction 10 minutes.437 kilograms of high base number calcium mahogany sulfonates that is 270mgKOH/g by total basicnumber add in reaction vessel, ice acetic acid 120 kg slowly under stirring.Finish, stir and be warmed up to 150～160 ℃, add 2 kilograms, di-iso-octyldiphenylamine oxidation inhibitor and 3 kilograms of T561, be uniformly mixed 5 minutes, stop heating.Add 162.9 kilograms of 150BS under stirring and be cooled to 80～100 ℃, obtaining product after homogenizing is degassed.The performance of the present embodiment products obtained therefrom is in Table 1.
Embodiment 3
In reaction vessel, add 200 kilograms of No. 100 machinery oil and 40 kilograms of MDI, stirring heating is warmed up to 40～50 ℃, adds stearylamine and 19.8 kilograms of hexahydroaniline of 43 kilograms of fusings, heats to 100～110 ℃, stirs isothermal reaction 10 minutes.245 kilograms of high base number calcium mahogany sulfonates that is 400mgKOH/g by total basicnumber add in reaction vessel, 100 kilograms of ice acetic acids slowly under stirring.Finish, stir and be warmed up to 150～160 ℃, add 1 kilogram, di-iso-octyldiphenylamine oxidation inhibitor, 3 kilograms and 0.5 kilogram T551 of pentanoic, be uniformly mixed 5 minutes, stop heating.Add 347.7 kilograms of 150BS under stirring and be cooled to 80～100 ℃, obtaining product after homogenizing is degassed.The performance of the present embodiment products obtained therefrom is in Table 1.
Embodiment 4
In reaction vessel, add 200 kilograms of HVI500 and 55 kilograms of MDI, stirring heating is warmed up to 40～50 ℃, adds the para-totuidine of 47.1 kilograms of fusings, heats to 100～110 ℃, stirs isothermal reaction 10 minutes.132 kilograms of calcium mahogany sulfonates that 150 kilograms of high base number calcium mahogany sulfonates that is 400mgKOH/g by total basicnumber and total basicnumber are 290mgKOH/g add in reaction vessel, 100 kilograms of ice acetic acids slowly under stirring.Finish, stir and be warmed up to 150～160 ℃, add 5 kilograms of pentanoic and 1 kilogram of T706, be uniformly mixed 5 minutes, stop heating.Add 309.9 kilograms of 150BS under stirring and be cooled to 80～100 ℃, obtaining product after homogenizing is degassed.The performance of the present embodiment products obtained therefrom is in Table 1.
Embodiment 5
In reaction vessel, add 200 kilograms of No. 100 machinery oil and 40 kilograms of MDI, stirring heating is warmed up to 40～50 ℃, adds para-totuidine and 15.8 kilograms of hexahydroaniline of 17.2 kilograms of fusings, heats to 100～110 ℃, stirs isothermal reaction 10 minutes.369 kilograms of high base number calcium mahogany sulfonates that is 400mgKOH/g by total basicnumber add in reaction vessel, 150 kilograms of ice acetic acids slowly under stirring.Finish, stir and be warmed up to 150～160 ℃, add 5 kilograms of T501 and 3 kilograms of T561, be uniformly mixed 5 minutes, stop heating.Add 200 kilograms of 150BS under stirring and be cooled to 80～100 ℃, obtaining product after homogenizing is degassed.The performance of the present embodiment products obtained therefrom is in Table 1.
By analysis, the aspects such as the dropping point of the polyurea calcium acetate lubricating grease of embodiment 1-5 gained, water repelling property, Corrosion Protection, machinery peace performance, colloid-stabilised performance, abrasion resistant extreme-pressure performance all are better than common extreme pressure lithium base lubricating grease and extreme pressure compound lithium base grease.
Each embodiment performance analysis data of table 1
Finally it should be noted that: the foregoing is only the preferred embodiments of the present invention, be not limited to the present invention, although with reference to previous embodiment, the present invention is had been described in detail, for a person skilled in the art, its technical scheme that still can put down in writing aforementioned each embodiment is modified, or part technical characterictic wherein is equal to replacement.Within the spirit and principles in the present invention all, any modification of doing, be equal to replacement, improvement etc., within all should being included in protection scope of the present invention.
Claims (7)
1. a polyurea calcium acetate lubricating grease, it is characterized in that, comprise following component, all to account for the percentage calculation of raw material for lubricating grease gross weight, 25～63% base oil, 3～5% 4,4'-methylene-bis phenylcarbimide, 2～10% organic amine, 20～55% calcium sulfonate with high base number, 10～15% glacial acetic acid, 0.1～1% oxidation inhibitor, 0.01～0.3% corrosion inhibitor;
Described base oil is a kind of of mineral oil or any two above combinations, and 100 ℃ of kinematic viscosity are 8～50mm
2/ s;
A kind of or any two above combinations of the primary amine that described organic amine is aliphatic amide, Cycloalkyl amine, arylamine class;
Described calcium sulfonate with high base number is calcium mahogany sulfonate or calcium alkylbenzenesulfonate, or both mixtures, and the total basicnumber of calcium sulfonate with high base number is 270～450mgKOH/g.
2. polyurea calcium acetate lubricating grease according to claim 1 is characterized in that: described base oil is a kind of of No. 100 machinery oil, HVI500,120BS or 150BS or any two above combinations.
3. polyurea calcium acetate lubricating grease according to claim 1 is characterized in that: described organic amine is a kind of of amino dodecane, stearylamine, aniline, para-totuidine or hexahydroaniline or any two above combinations.
4. polyurea calcium acetate lubricating grease according to claim 1 is characterized in that: described oxidation inhibitor is a kind of of phenol type, amine type oxidation inhibitor or any two above combinations.
5. polyurea calcium acetate lubricating grease according to claim 4, it is characterized in that: described oxidation inhibitor is a kind of of 2,6 ditertiary butyl p cresol, di-iso-octyldiphenylamine, N-phenyl-a-naphthylamine, N-Phenyl beta naphthylamine or pentanoic or any two above combinations.
6. polyurea calcium acetate lubricating grease according to claim 1, is characterized in that: a kind of or any two above combinations that described corrosion inhibitor is 124 Triazole, thiadiazoles, T406, T551, T553, T561, T706.
7. the preparation method of the described polyurea calcium acetate lubricating grease of arbitrary claim in claim 1-6, is characterized in that, step is as follows:
(1) by part base oil and whole 4,4'-methylene-bis phenylcarbimide adds in reaction vessel, is stirred and heated to 40～50 ℃, then under agitation adds the organic amine liquid of fusing, heats to 100～110 ℃, stirs isothermal reaction 10 minutes;
(2) again calcium sulfonate with high base number is added in the reaction vessel of step (1) to ice acetic acid slowly under stirring; Finish, stir and be warmed up to 150～160 ℃, add oxidation inhibitor and rut preventives and be uniformly mixed, stop heating;
(3) add whole excess oil under the stirring, stir and be cooled to 80～100 ℃, the degassed product that obtains of homogenizing;
Described base oil is a kind of of mineral oil or any two above combinations, and 100 ℃ of kinematic viscosity are 8～50mm
2/ s;
A kind of or any two above combinations of the primary amine that described organic amine is aliphatic amide, Cycloalkyl amine, arylamine class;
Described calcium sulfonate with high base number is calcium mahogany sulfonate or calcium alkylbenzenesulfonate, or both mixtures, and the total basicnumber of calcium sulfonate with high base number is 270～450mgKOH/g.
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| CN2011103317096A CN102504920B (en) | 2011-10-27 | 2011-10-27 | Polyurea calcium acetate lubricating grease and preparation method thereof |
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|---|---|---|---|
| CN2011103317096A CN102504920B (en) | 2011-10-27 | 2011-10-27 | Polyurea calcium acetate lubricating grease and preparation method thereof |
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| CN102504920A CN102504920A (en) | 2012-06-20 |
| CN102504920B true CN102504920B (en) | 2013-12-04 |
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| CN109810767A (en) * | 2019-03-22 | 2019-05-28 | 山东奇士登润滑科技有限公司 | A kind of high-performance heavy load high temperature waterproof grease and preparation method |
| CN110669574A (en) * | 2019-10-22 | 2020-01-10 | 中国石油化工股份有限公司 | Extreme pressure anti-wear lubricating grease and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1657599A (en) * | 2004-02-18 | 2005-08-24 | 中国石油化工股份有限公司 | Polyurea grease composite |
| US7171110B1 (en) * | 2001-11-30 | 2007-01-30 | Keen Personal Media, Inc. | System and a method for storing audio/video programs on a hard disk drive for presentation to a viewer |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7171110B1 (en) * | 2001-11-30 | 2007-01-30 | Keen Personal Media, Inc. | System and a method for storing audio/video programs on a hard disk drive for presentation to a viewer |
| CN1657599A (en) * | 2004-02-18 | 2005-08-24 | 中国石油化工股份有限公司 | Polyurea grease composite |
Non-Patent Citations (1)
| Title |
|---|
| 宗明.EPU聚脲－醋酸钙复合润滑脂的研究及应用.《石油商技》.2004,第22卷(第4期),第12-14页. * |
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Granted publication date: 20131204 Termination date: 20201027 |