CN102757845B - Low-noise lithium-based lubricating grease composition and preparation method thereof - Google Patents
Low-noise lithium-based lubricating grease composition and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a lithium-based lubricating grease composition. Based on the total weigh of lubricating grease, the lithium-based lubricating grease composition comprises the following components: (1) 75 to 94 percent of base oil; (2) 5 to 15 percent of lithium soap thickening agent; and (3) 0.1 to 4 percent of alkenyl diimide dispersing agent. The lubricating grease composition has excellent bearing vibrating performance, can be applied to medium and small-sized sealing bearings and is applicable to lubrication of motor bearings of official automated equipment and household appliances.
Description
Technical field
The invention belongs to lubricant, is exactly a kind of grease composition.
Background technology
Motor in business automation equipment and household electrical appliance, requirement provides the ball bearing of low noise and low vibration, and these bearing great majority are disposable deep groove ball bearings of minor diameter, band sealing, generally adopt lubricating grease to be lubricated.But the Of Super Quality Lubricant Grease that this class is small-sized and miniature bearings uses needs import conventionally, and price comparison is expensive, therefore, the lubricating grease that preparation has good noise performance is necessary very much.The kind of conventional low noise bearing lubricating grease comprises lithium soap grease and urea-base grease etc.Low-noise lubricating grease is except impurity can affect the noise performance of lubricating grease, and the aspects such as soap fibrous texture, base oil kind and viscosity, aftertreatment technology can affect the noise performance of lubricating grease equally.
In some patents propose by adjust base oil kind and viscosity, take different aftertreatment technologys to reduce the noise of lubricating grease.In CN100572510, propose, adopting mineral oil, synthetic hydrocarbon oil and polymkeric substance ester oil is base oil, prepares low noise lithium soap grease, adopts cooling and three-wheel barreling fast to grind to obtain sample.In CN101087868, mentioning and adopting ester class oil and synthetic hydrocarbon oil is that mixing oil is prepared lithium soap grease, and aftertreatment technology adopts cooling fast, can reduce the bearing vibration value of lubricating grease.These technology are the restriction of existence foundation oil raw material on the one hand, and aftertreatment technology is more complicated on the other hand, is unfavorable for operation and controls.
Summary of the invention
The invention provides a kind of compound lithium base grease and preparation method thereof, this lubricating grease has good noise performance.
Compound lithium base grease provided by the invention, taking lubricating grease gross weight as benchmark, comprises following component:
(1) base oil, content is 75%～94%;
(2) lithium soap viscosifying agent, content is 5%～15%;
(3) allyl butyrate imide class dispersion agent, content is 0.1%～4%.
Said base oil, can be selected from one or more in mineral oil, alkene oil, ester class oil, ethers oil, silicone oil etc.Its mineral oil in fluid is paraffin base mineral oil, (as 150BS, 500SN, 650SN, 500N, 100 DEG C of viscosity are 5～100mm to naphthenic mineral oil
2/ s) etc. one or more, polyolefin oil comprises that (100 DEG C of viscosity are 4～300mm to polyalphaolefin
2/ s), and one or more in dioctyl sebacate, Uniflex DBS, Octyl adipate, dibutyl phthalate, dioctyl phthalate (DOP), pentaerythritol ester and trihydroxymethylpropanyl ester etc. of ester class grease separation, 100 DEG C of viscosity are 2mm
2/ s～100mm
2/ s, ethers oil comprises polyether oil, 100 DEG C of viscosity are 5mm
2/ s～300mm
2/ s, silicone oil can be methyl-silicone oil, ethyl silicon oil, toluene machine silicone oil etc., 100 DEG C of viscosity are 2mm
2/ s～300mm
2/ s.The preferred mineral oil of described base oil (500SN, 650SN etc.), alkene oil (100 DEG C of viscosity 2mm
2/ s, 4mm
2/ s, 6mm
2/ s, 10mm
2/ s), dioctyl sebacate, trimethylolpropane tris oleic acid ester, dibutyl phthalate, pentaerythritol ester etc., most preferably 500SN (100 DEG C of viscosity 11mm
2/ s), alkene oil (100 viscosity 6mm
2/ s, 10mm
2/ s), dioctyl sebacate (40 DEG C of viscosity 12.5mm
2/ s), trimethylolpropane tris oleic acid ester (40 DEG C of viscosity 47.5mm
2/ s) etc., the content of base oil is 75%～94%, preferably 85%～92%.
Said lithium soap viscosifying agent, can be one or both the mixture in lithium 12-hydroxy stearate soap, stearic acid lithium soap, and the content of viscosifying agent is 5%～15%, preferably 7%～10%.
Said allyl butyrate imide class dispersion agent, effect is to make the fibrous texture of viscosifying agent tiny, thereby improve the noise performance of lubricating grease, specifically can be selected from mono alkenyl succimide (code name T151), diene base succimide (code name T154), polyene-based succimide (code name T155), polymer succimide (code name T161), the content of dispersion agent is 0.1%～4%, preferably 0.4%～2.5%.
In addition, in grease composition of the present invention, also can add sanitas.Anticorrosive additive can be selected from one or more in barium mahogany sulfonate (code name T701), zinc naphthenate (code name T704), dinonyl naphthalene barium mahogany sulfonate (code name T705), dodecenylsuccinic acid (code name T746) and dodecenylsuccinic acid half ester (code name T747) etc.Taking lubricating grease gross weight as benchmark, the content of sanitas is 0.1%～1%, preferably 0.2%～0.6%.
In addition, in grease composition of the present invention, can also add other additive, as oxidation inhibitor, extreme pressure anti-wear additives, oiliness improver, metal passivator etc.Wherein oxidation inhibitor can be S-P-Zn compound and/or phenolic compound, and S-P-Zn compound is sulphur phosphorus fourth octyl group zinc salt (code name T202), the two octyl group zinc salts (code name T203) of sulphur phosphorus, sulphur phosphorus brothers alcohol radical zinc salt (code name T204), sulphur phosphorus secondary alcohol groups zinc salt (code name T205) etc. such as; Such as 2,6 ditertiary butyl p cresol of phenolic compound (code name T501), mixed type shielding phenol (code name T502) etc.Taking lubricating grease gross weight as benchmark, antioxidant content is generally 0.1%～1%.Extreme pressure anti-wear additives kind comprises di-n-butyl phosphite (code name T304), tritolyl phosphate (code name T306), phosphoric acid ester (code name T451) etc.Oiliness improver can add 124 Triazole lipid acid amine salt (code name T406), and metal passivator can add 124 Triazole derivative (code name T551), thiadiazoles derivative (code name T561) etc.
Lubricating grease of the present invention can adopt following methods preparation:
(1) in reactor, add 40%～70% of whole base oils, and ten dihydroxystearic acids or stearic acid and dispersion agent, heat up and fully mix;
(2) reach after 75 DEG C～90 DEG C, add equimolar lithium hydroxide (water dissolution of 3～4 times of its quality for lithium hydroxide) to carry out saponification reaction;
(3) be warmed up to 120 DEG C～170 DEG C, add 10～20% of whole base oils;
(4) be warming up to 180 DEG C～210 DEG C, add residue base oil as quenching oil, circulation temperature lowering;
(5) while being cooled to 100 DEG C～120 DEG C, add additive, grind, obtain lubricating grease finished product.
Lubricating grease of the present invention can also adopt following method preparation:
(1) in reactor, add 40%～70% base oil, add lithium 12-hydroxy stearate or lithium stearate and dispersion agent, heat up and fully mix;
(2) be warming up to 180 DEG C～210 DEG C, add residue base oil as quenching oil, circulation temperature lowering;
(3) while being cooled to 100 DEG C～120 DEG C, add additive, grind, obtain lubricating grease finished product.
Lithium 12-hydroxy stearate wherein or lithium stearate are preparations like this: in a certain amount of water, add ten dihydroxystearic acids or the stearic acid of 0.1～0.2 times of quality, be heated to 85 DEG C～90 DEG C, add and ten dihydroxystearic acids or the equimolar lithium hydroxide of stearic acid (water dissolution of 3～4 times of its quality for lithium hydroxide), fully stir 0.5h～1h, reactant toasts 1h～2h in the baking oven of 100 DEG C, makes lithium 12-hydroxy stearate sample.
Grease composition of the present invention has good bear vibration performance, can be used in medium and small sealing bearing, is applicable to the lubricated of motor bearings in business automation equipment and household electrical appliance.
Embodiment
The measurement standard of grease composition bear vibration is JB/T7047-1999 " rolling bearing-deep groove ball bearing vibration (acceleration) technical qualification ", the bearing using is 6202 type deep groove ball bearings, between steel ball and raceway, fill the grease composition in the present invention, the S0901 type bearing vibration measuring instrument that the instrument of use is Dalian Bearing Instrument Factory.When measurement, record the decibel value (dB) of bear vibration, record the situation of beating of bearing peak value pointer (dB-mv) in operation process simultaneously, number≤2 of pointer in 1min, the lubricating grease noise that this bearing use is described is few, if pointer number >=2, illustrate that the lubricating grease noise of this bearing use is many.Can also vibrate the crest number producing by counter records 1min neck bearing, crest number is many, illustrates that the vibration performance of bearing is poor simultaneously.
In embodiment and comparative example, using the content of lipid acid as viscosifying agent content.
Embodiment 1
In reactor, add the 500SN of 30kg, ten dihydroxystearic acids of 8kg, 1kg allyl butyrate imide (code name T154), be heated to 90 DEG C, between 15min～40min, add 4kg lithium hydroxide aqueous solution (1.12kg lithium hydroxide+2.88kg water), be warming up to 160 DEG C, add gradually the 500SN of 30kg, continue to be warming up to 200 DEG C, material dissolves completely, add 30.5kg500SN, start circulation shear (pressure 0.5MPa～0.7MPa) cooling, when temperature is down to 100 DEG C, add 0.5kgT203, 0.5kgT704, go out still and make lubricating grease sample.
Embodiment 2
In reactor, add the dioctyl sebacate of 60kg, the lithium 12-hydroxy stearate of 8kg, the diene base succimide (code name T154) of 2kg, is heated with stirring to 210 DEG C gradually, and lithium 12-hydroxy stearate dissolves completely, add gradually the dioctyl sebacate of 29.5kg, start circulation shear cooling (pressure 0.5MPa～0.7MPa), temperature, in the time of 100 DEG C～120 DEG C, adds 0.2kgT202,0.3kgT705, goes out still and makes lubricating grease sample.
Embodiment 3
In reactor, add poly-a-olefin oil (100 DEG C of viscosity 5.9mm of 30kg
2/ s), ten dihydroxystearic acids of 8kg, 0.5kg polyene-based succimide (code name T155), be heated to 85 DEG C, between 15min～40min, add 5kg lithium hydroxide aqueous solution (1.12kg lithium hydroxide+3.88kg water), be warming up to 165 DEG C, add gradually poly-a-olefin oil (100 DEG C of viscosity 5.9mm of 30kg
2/ s), continuing to be warming up to 200 DEG C, material dissolves completely, adds 31kg poly-a-olefin oil (100 DEG C of viscosity 5.9mm
2/ s), starting circulation shear cooling (pressure 0.5MPa～0.7MPa), temperature, in the time of 110 DEG C, adds 0.5kgT701, goes out still and makes lubricating grease sample.
Embodiment 4
In reactor, add the polymethylphenyl siloxane fluid (code name 255-150A) of 29.8kg, ten dihydroxystearic acids of 9kg, 0.4kg mono alkenyl succimide (code name T151), be heated to 85 DEG C, between 15min～40min, add 5kg lithium hydroxide aqueous solution (1.26kg lithium hydroxide+3.74kg water), be warming up to 150 DEG C, add gradually the polymethylphenyl siloxane fluid (code name 255-150A) of 29.8kg, continue to be warming up to 200 DEG C, material dissolves completely, add 30kg polymethylphenyl siloxane fluid (code name 255-150A), start circulation shear cooling (pressure 0.5MPa～0.7MPa), temperature is in the time of 100 DEG C, add 0.5kgT202, 0.5kgT747, go out still and make lubricating grease sample.
Embodiment 5
In reactor, add poly-a-olefin oil (100 DEG C of viscosity 10mm of 30.1kg
2/ s), ten dihydroxystearic acids of 8kg, 0.5kg diene base succimide (code name T154), be heated to 85 DEG C, between 15min～40min, add 5kg lithium hydroxide aqueous solution (1.12kg lithium hydroxide+3.88kg water), be warming up to 165 DEG C, add gradually poly-a-olefin oil (100 DEG C of viscosity 5.9mm of 30.1kg
2/ s), continuing to be warming up to 205 DEG C, material dissolves completely, adds 30.3kg poly-a-olefin oil (100 DEG C of viscosity 10mm
2/ s), starting circulation shear cooling (pressure 0.5MPa～0.7MPa), temperature, in the time of 100 DEG C, adds 0.2kgT202, and 0.3kgT704 goes out still and makes lubricating grease sample.
Embodiment 6
In reactor, add the 500SN of 30kg, ten dihydroxystearic acids of 7kg, 1kg mono alkenyl succimide (code name T151), be heated to 85 DEG C, between 15min～40min, add 4kg lithium hydroxide aqueous solution (0.98kg lithium hydroxide+3.02kg water), be warming up to 160 DEG C, add gradually the 500SN of 30kg, continue to be warming up to 180 DEG C～210 DEG C, material dissolves completely, adds 32kg500SN, starts circulation shear (pressure 0.5MPa～0.7MPa) cooling, when temperature is down to 110 DEG C, goes out still and make lubricating grease sample.
Embodiment 7
In reactor, add the dioctyl sebacate of 60kg, the lithium stearate of 8kg, the polyene-based succimide (code name T155) of 2kg, be heated with stirring to gradually 200 DEG C, lithium 12-hydroxy stearate dissolves completely, adds gradually the dioctyl sebacate of 30kg, starts circulation shear cooling (pressure 0.5MPa～0.7MPa), temperature, in the time of 100 DEG C, goes out still and makes lubricating grease sample.
Embodiment 8
In reactor, add the trishydroxymethyl trioleate of 60kg, the lithium 12-hydroxy stearate of 7kg, the mono alkenyl succimide (code name T151) of 1kg, be heated with stirring to gradually 200 DEG C, lithium 12-hydroxy stearate dissolves completely, adds gradually the trishydroxymethyl trioleate of 31.5kg, start circulation shear cooling (pressure 0.5MPa～0.7MPa), temperature, in the time of 110 DEG C, adds 0.5kgT701, goes out still and makes lubricating grease sample.
Embodiment 9
In reactor, add the trishydroxymethyl trioleate of 60kg, the lithium 12-hydroxy stearate of 7kg, the diene base succimide (code name T154) of 1kg, be heated with stirring to gradually 210 DEG C, lithium 12-hydroxy stearate dissolves completely, adds gradually the trishydroxymethyl trioleate of 32kg, starts circulation shear cooling (pressure 0.5MPa～0.7MPa), temperature, in the time of 100 DEG C, goes out still and makes lubricating grease sample.
Comparative example 1
Contrast with embodiment 1.In reactor, add the 500SN of 30kg, ten dihydroxystearic acids of 8kg, be heated to 90 DEG C, between 15min～40min, add 4kg lithium hydroxide aqueous solution (1.12kg lithium hydroxide+2.88kg water), be warming up to 160 DEG C, add gradually the 500SN of 30kg, continue to be warming up to 200 DEG C, material dissolves completely, add 31.5kg500SN, start circulation shear (pressure 0.5MPa～0.7MPa) cooling, when temperature is down to 100 DEG C, add 0.5kgT704, go out still and make lubricating grease sample.
Comparative example 2
Contrast with embodiment 2.
In reactor, add the dioctyl sebacate of 60kg, the lithium 12-hydroxy stearate of gkg, be heated with stirring to gradually 210 DEG C, lithium 12-hydroxy stearate dissolves completely, add gradually the dioctyl sebacate of 31.5kg, start circulation shear cooling (pressure 0.5MPa～0.7MPa), temperature is in the time of 100 DEG C～120 DEG C, add 0.5kgT705, go out still and make lubricating grease sample.
Claims (12)
1. a preparation method for compound lithium base grease, comprising:
(1) in reactor, add 40%～70% of whole base oil quality, and ten dihydroxystearic acids or stearic acid and allyl butyrate imide class dispersion agent, heat up and fully mix;
(2) reach after 75 DEG C～90 DEG C, add lithium hydroxide aqueous solution to carry out saponification reaction;
(3) be warmed up to 120 DEG C～170 DEG C, add 10～20% of whole base oils;
(4) be warming up to 180 DEG C～210 DEG C, add residue base oil as quenching oil, circulation temperature lowering;
(5) while being cooled to 100 DEG C～120 DEG C, add additive, grind, obtain lubricating grease finished product, described additive comprises anticorrosive additive;
In the lubricating grease obtaining, taking lubricating grease gross weight as benchmark, the content of base oil is 85%～92%, and the content of viscosifying agent is 7%～15%, and the content of dispersion agent is 0.4%～2.5%, and the content of anticorrosive additive is 0.2%～0.6%.
2. according to preparation method claimed in claim 1, wherein base oil is selected from one or more in mineral oil, alkene oil, ester class oil, ethers oil, silicone oil.
3. according to preparation method claimed in claim 1, wherein base oil is selected from one or more in 500SN mineral oil, poly-a-olefin oil, polymethylphenyl siloxane fluid, two dioctyl phthalates, trimethylolpropane tris oleic acid ester.
4. according to preparation method claimed in claim 1, wherein allyl butyrate imide class dispersion agent is selected from one or more of mono alkenyl succimide, diene base succimide, polyene-based succimide and polymer succimide.
5. according to preparation method claimed in claim 1, described anticorrosive additive is selected from one or more in barium mahogany sulfonate, zinc naphthenate, dinonyl naphthalene barium mahogany sulfonate, dodecenylsuccinic acid and dodecenylsuccinic acid half ester.
6. the compound lithium base grease that the described method of one of claim 1-5 obtains.
7. a preparation method for compound lithium base grease, comprising:
(1) in reactor, add 40%～70% of whole base oil quality, and lithium 12-hydroxy stearate or lithium stearate and allyl butyrate imide class dispersion agent, heat up and fully mix;
(2) be warming up to 180 DEG C～210 DEG C, add residue base oil as quenching oil, circulation temperature lowering;
(3) while being cooled to 100 DEG C～120 DEG C, add additive, grind, obtain lubricating grease finished product, described additive comprises anticorrosive additive;
In the lubricating grease obtaining, taking lubricating grease gross weight as benchmark, the content of base oil is 85%～92%, and the content of viscosifying agent is 7%～15%, and the content of dispersion agent is 0.4%～2.5%, and the content of anticorrosive additive is 0.2%～0.6%.
8. according to preparation method claimed in claim 7, wherein base oil is selected from one or more in mineral oil, alkene oil, ester class oil, ethers oil, silicone oil.
9. according to preparation method claimed in claim 7, wherein base oil is selected from one or more in 500SN mineral oil, poly-a-olefin oil, polymethylphenyl siloxane fluid, two dioctyl phthalates, trimethylolpropane tris oleic acid ester.
10. according to preparation method claimed in claim 7, wherein allyl butyrate imide class dispersion agent is selected from one or more of mono alkenyl succimide, diene base succimide, polyene-based succimide and polymer succimide.
11. according to preparation method claimed in claim 7, and described anticorrosive additive is selected from one or more in barium mahogany sulfonate, zinc naphthenate, dinonyl naphthalene barium mahogany sulfonate, dodecenylsuccinic acid and dodecenylsuccinic acid half ester.
The grease composition that one of 12. claim 7-11 described method obtains.
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| CN104560281B (en) * | 2013-10-25 | 2017-04-26 | 中国石油化工股份有限公司 | Sulfonate, preparation method thereof, lubricating grease containing sulfonate and preparation method of lubricating grease |
| CN104560283B (en) * | 2013-10-25 | 2017-04-26 | 中国石油化工股份有限公司 | Sulfonate, preparation method thereof, lubricating grease containing sulfonate and preparation method of lubricating grease |
| CN104479832A (en) * | 2014-10-25 | 2015-04-01 | 中国石油化工股份有限公司 | Automobile assembly line conveyor belt special-purpose grease and preparation method |
| CN106032484B (en) * | 2015-03-11 | 2019-01-08 | 中国石油化工股份有限公司 | Lubricant composition and preparation method thereof |
| CN105132102A (en) * | 2015-08-25 | 2015-12-09 | 石海旺 | Special lubricating grease for plastic gears |
| CN107353963A (en) * | 2017-06-08 | 2017-11-17 | 吴国呈 | Oil additives |
| CN107353986A (en) * | 2017-08-26 | 2017-11-17 | 东莞市欧迪斯润滑剂科技有限公司 | A kind of low noise lithium saponify and preparation method |
| CN111100735B (en) * | 2018-10-26 | 2022-04-08 | 中国石油化工股份有限公司 | Lubricating grease for medium-sized truck hub bearing and preparation method thereof |
| CN112195054A (en) * | 2019-12-23 | 2021-01-08 | 新协同（宁波）油脂有限公司 | Low-noise bearing lubricating grease and preparation method thereof |
| CN113667522B (en) * | 2021-07-28 | 2023-01-10 | 中国石油化工股份有限公司 | Fretting wear resistant low-noise lubricating grease for air conditioner motor bearing and preparation method thereof |
| CN115305129B (en) * | 2022-08-12 | 2023-06-20 | 中国石油化工股份有限公司 | Barium-based lubricating grease composition and preparation method and application thereof |
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