CN1796516A - Lithium base grease in high drop point, and preparation method - Google Patents
Lithium base grease in high drop point, and preparation method Download PDFInfo
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- CN1796516A CN1796516A CN 200510001686 CN200510001686A CN1796516A CN 1796516 A CN1796516 A CN 1796516A CN 200510001686 CN200510001686 CN 200510001686 CN 200510001686 A CN200510001686 A CN 200510001686A CN 1796516 A CN1796516 A CN 1796516A
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Abstract
A high dropping point lithium grease, comprising the following components based on the total weight of the grease: 1) base oil, 68-95 wt.%; 2) C6-C24 fatty-acid lithium salt densifier, 4-30 wt.%; 3) titanium oxide, 0.1-8 wt.%. The said grease has three characteristic peeks in the IR spectrum, i.e., the peak located at 1555cm-1-1530cm-1 characteristic of the O-Li asymmetric adsorption of fatty-acid lithium salt; the peak located at 1454cm-1-1430cm-1 characteristic of the O-Li symmetric adsorption of fatty-acid salt; and the peak located at 620cm-1-595cm-1 characteristic of the Ti-O skeleton vibration of titanium oxide. The lithium grease described in this invention has a high dropping point (higher than 280 deg.C) and low oil-separation, and reserve other outstanding properties of the lithium grease.
Description
Technical field
The invention belongs to lubricating grease, specifically lithium soap grease and preparation method thereof.
Background technology
Lithium saponify with its good performance, cheap price, has been widely used in countries in the world since 1949 come out, and its output is first of all kinds of lubricating grease.It has good water resisting property, thermotolerance, mechanical safety and anti-oxidant security, and life cycle is long, and wide ranges is a kind of comparatively ideal multi-usage, long lifetime lubricating grease.But also there are some defectives in lithium saponify, mainly is that dropping point is lower, is generally less than 200 ℃.
The conventional production methods of lithium soap grease is to adopt 12 monohydroxy stearic acid (or stearic acid) and lithium hydroxide reaction in base oil, and the heating saponification obtains final product, as US 3,980, and 572 disclosed methods.In recent years, lithium saponify on production technique and aspect the additive all constantly the development and perfect.As the prefabricated soap of US 20020022581 employing powder dried preparation lithium saponifies, simple to operate, made soap is stored convenient, can be during use according to required denseness, and the base oil of allotment suitable proportion.In order to improve the anti-attrition performance of lithium saponify, can add various additives, as US 20030087768, adding specific surface area in lithium saponify is 100m
2The TiO of/g
2, SiO
2Deng inorganic oxide.
Summary of the invention the invention provides a kind of lithium soap grease of high dropping point.
The present invention also provides the preparation method of above-mentioned lithium soap grease.
Lithium soap grease provided by the invention is a benchmark with the lubricating grease gross weight, contains following component:
1. base oil, content are 68～95 heavy %, preferred 75～90 heavy %;
2.C6～C24 lipid acid lithium salts viscosifying agent, content are 4～30 heavy %, preferred 10～25 heavy %;
3. titanium dioxide, content is heavy % O.1～8, preferred 0.3～5 heavy %.
Said lubricating grease contains following three characteristic peaks in infrared spectrum, that is: eigenwert is positioned at 1555cm
-1～1530cm
-1, preferred 1550cm
-1～1535cm
-1Between, more preferably 1545cm
-1～1540cm
-1Between the asymmetric absorption peak of O-Li of fatty acid lithium; Eigenwert is positioned at 1454cm
-1～1430cm
-1Between, preferred 1450cm
-1～1435cm
-1Between, more preferably 1450cm
-1～1440cm
-1Between the O-Li symmetry absorption peak of fatty acid lithium; Be positioned at 620cm
-1～595cm
-1Between, preferred 615cm
-1～600cm
-1Between, more preferably 615cm
-1～605cm
-1Between the Ti-O skeleton structure vibration peak of titanium dioxide.
Said base oil is mineral oil, vegetables oil, synthetic oil or its mixture that 100 ℃ of viscosity are 10～20cSt, and vegetables oil can be Viscotrol C, rapeseed oil, peanut oil, soya-bean oil etc., and synthetic oil can be ester class oil, polyolefine wet goods.
Lipid acid in the said lipid acid lithium salts viscosifying agent is C6～C24 lipid acid, preferred C8～C20 lipid acid, more preferably 12-oxystearic acid, stearic acid etc.
Can also add additive as required in the lithium soap grease provided by the invention, as oxidation inhibitor, extreme pressure anti-wear additives, rust-preventive agent etc.Oxidation inhibitor can be amine antioxidants or phenolic antioxidant, or the mixture of the two.Said amine antioxidants can be di-iso-octyldiphenylamine, dioctyl diphenylamine or with the pentanoic of other alkyl, said phenolic antioxidant can be 2,6 toluene di-tert-butyl phenols, 2,6 di-tert-butylphenols etc.Extreme pressure anti-wear additives can be chloride a, sulfur-bearing, phosphorous and contain sulfur phosphorus compound etc., said chloride extreme pressure anti-wear additives can be a clorafin, said sulfur-bearing extreme pressure anti-wear additives can be sulfurized olefin cotton oil, sulfide isobutene, said phosphorous extreme pressure anti-wear additives can be a tritolyl phosphate, and sulfur-bearing phosphorus extreme pressure anti-wear additives can be dialkyl dithiophosphate (as zinc salt, antimonic salt, a molybdenum salt etc.).Rust-preventive agent can be one or both in barium mahogany sulfonate, zinc naphthenate, the benzotriazole.
Can preparing of lithium soap grease provided by the invention by following two kinds of methods:
First kind of preparation method comprises:
In base oil, add organic solvent, tetrabutyl titanate and C6～C24 lipid acid, at 25～120 ℃, stirring reaction under preferred 40～90 ℃ temperature, at 50～120 ℃, preferred 80～110 ℃ add lithium hydroxide solution, be warming up to 180～260 ℃, be preferably 200～240 ℃ and carry out the high temperature refining, add quenching oil, cooling is ground, add additive as required, obtain lubricating grease of the present invention.By above reaction, tetrabutyl titanate is transformed into titanium dioxide.
Said base oil is mineral oil, vegetables oil, synthetic oil or its mixture that 100 ℃ of viscosity are 10～20cSt, and vegetables oil can be Viscotrol C, rapeseed oil, peanut oil, soya-bean oil etc., and synthetic oil can be ester class oil, polyolefine wet goods.
Said organic solvent is a polar organic solvent, as tetrahydrofuran (THF), C1～C4 lipid acid, C2～C4 low-carbon alcohol, acetone etc., also can be these solvent mixtures.
The carbon number of said lipid acid is C6～C24, preferred C8～C20.Lipid acid commonly used has 12-oxystearic acid, stearic acid etc.
The gross weight of lipid acid and lithium hydroxide accounts for 4～30 heavy % of lubricating grease gross weight, preferred 8～25 heavy %.Lipid acid and lithium hydroxide reaction generate lipid acid lithium salts viscosifying agent.Lipid acid and lithium hydroxide mole number are roughly the same, and for example the add-on of lipid acid can be 0.5～1.5 times of lithium hydroxide mole number, preferred 0.8～1.2 times.The mol ratio of lipid acid and tetrabutyl titanate is about 1: 0.5～and 5, preferred 1: 0.8～3.The mol ratio of lipid acid and organic solvent is about 1: 5～and 20, preferred 1: 5～15.Quenching oil is the base oil that adds in the reaction later stage, and its add-on is generally 15～50 heavy % of base oil gross weight, preferred 25～35 heavy %.The concentration of lithium hydroxide solution is 5～50 heavy %, preferred 10～30 heavy %.
The reaction of tetrabutyl titanate and C6～C24 lipid acid can be carried out 2～72 hours, preferred 12～48 hours.Reaction times is long more, and transformation efficiency is high more.Even but reaction not exclusively, residual reactant can not produce detrimentally affect to capability of lubricating grease yet.
The time of high temperature refining was generally kept preferred 20～40 minutes 10～60 minutes.The effect of high temperature refining is to make grease structure stable.This step belongs to techniques well known.
Second kind of preparation method of lithium soap grease provided by the invention comprises:
Step 1: in organic solvent, add titanium tetrachloride, alkali and low-carbon alcohol and react, static, filter, precipitation separation, the filtrate that will contain pure titanium is with 80～100 ℃, preferred 90～100 ℃ hot water hydrolysis, and vigorous stirring makes its formation gel.The mol ratio of low-carbon alcohol and titanium tetrachloride is 1: 1～10, preferred 1: 2～6.The mol ratio of alkali and titanium tetrachloride is 1～10, preferred 2～6.By above reaction, titanium tetrachloride is transformed into titanium dioxide.
Temperature of reaction can be 5～80 ℃, and general normal temperature gets final product.Should reach peak rate of conversion if negate, then should react till precipitation no longer increases to the system,, then react and precipitation occurs to the system and get final product if do not require the transformation efficiency of reaction.
Said organic solvent is a non-polar organic solvent, as benzene,toluene,xylene etc.
Said alkali can be solid alkali, as sodium hydroxide, potassium hydroxide, yellow soda ash, sodium bicarbonate etc., also can be gas alkali, as ammonia, and preferred ammonia.
The preferred boiling water of said hot water.The volume of hot water is 1～5 times of filtrate volume, preferred 1～3 times.
Low-carbon alcohol is C1～C4 low-carbon alcohol, as methyl alcohol, ethanol, propyl alcohol, Virahol, butanols, and preferred Virahol.
Step 2: the gel that step 1 is obtained mixes with base oil and C6～C24 lipid acid, at 50～120 ℃, preferred 70～110 ℃ add lithium hydroxide solution, be warming up to 180～260 ℃, be preferably 200～240 ℃ and carry out the high temperature refining, add quenching oil, cooling is ground, add additive as required, obtain lubricating grease of the present invention.
Said base oil is mineral oil, vegetables oil, synthetic oil or its mixture that 100 ℃ of viscosity are 10～20cSt, and vegetables oil can be Viscotrol C, rapeseed oil, peanut oil, soya-bean oil etc., and synthetic oil can be ester class oil, polyolefine wet goods.
Lipid acid carbon number be C6～C24, preferred C8～C20.Lipid acid commonly used has 12-oxystearic acid, stearic acid etc.
The mol ratio of lipid acid and gel is 1: 0.5～5, preferred 1: 0.8～3.The mole number of gel is in the mole number of the pure titanium that wherein contains.
The gross weight of lipid acid and lithium hydroxide accounts for 4～30 heavy % of lubricating grease gross weight, preferred 8～25 heavy %.Wherein, the add-on of lipid acid is 0.5～1.5 times of mole number of lithium hydroxide, preferred 0.8～1.2 times.Quenching oil is the base oil that adds in the reaction later stage, and its add-on is generally 15～50 heavy % of base oil gross weight, preferred 25～35 heavy %.
The concentration of lithium hydroxide solution is 5～50 heavy %, preferred 10～30 heavy %.
The time of high temperature refining was generally kept preferred 20～40 minutes 10～60 minutes.The effect of high temperature refining is to make grease structure stable.This step belongs to techniques well known.
Lithium soap grease provided by the invention has high dropping point (greater than 280 ℃), divides oil little characteristics, and kept other premium properties of lithium saponify.This lubricating grease can be used for the rolling bearing of various mechanical means and lubricating of friction positions such as automobile hub bearing, chassis, water pump and generator, also can be used for the high temperature lubricating occasion.
Description of drawings
Fig. 1 is a universal lithium base grease typical case infrared spectrum, it is characterized in that 1580cm
-1Near and 1454cm
-1Near strong peak belongs to the asymmetric of 12-hydroxy lithium stearate and symmetric vibration peak respectively, and this is the lithium soap characteristic peak;
The lithium soap grease that Fig. 2 prepares for Comparative Examples 1 directly adds the infrared spectrum of nano titanium dioxide powder, it is characterized in that removing the original 1580cm of reservation
-1Near and 1454cm
-1Near the asymmetric and symmetrical peak of carboxylic acid lithium outside, at low band 588cm
-1Near new peak also appears, this peak is the Ti-O skeleton structure vibration peak of titanium dioxide.
Fig. 3 is the infrared spectrum of the lithium soap grease of example 1 preparation, it is characterized in that the asymmetric absorption peak eigenwert of carboxylic acid lithium falls to being positioned at 1545cm
-1About; Symmetry absorption peak eigenwert is positioned at 1442cm
-1At low band 607cm
-1About keep the Ti-O skeleton structure vibration peak of titanium dioxide.
Fig. 4 is the infrared spectrum of the lithium soap grease of example 2 preparations, it is characterized in that the asymmetric absorption peak eigenwert of carboxylic acid lithium falls to being positioned at 1545cm
-1About; Symmetry absorption peak eigenwert is positioned at 1448cm
-1At low band 611cm
-1About keep the Ti-O skeleton structure vibration peak of titanium dioxide.
Fig. 5 is the infrared spectrum of the lithium soap grease of example 4 preparations, it is characterized in that the asymmetric absorption peak eigenwert of carboxylic acid lithium falls to being positioned at 1543cm
-1About; Symmetry absorption peak eigenwert is positioned at 1444cm
-1At low band 607cm
-1About keep the Ti-O skeleton structure vibration peak of titanium dioxide.
Fig. 6 is the infrared spectrum of the lithium soap grease of example 5 preparations, it is characterized in that the asymmetric absorption peak eigenwert of carboxylic acid lithium falls to being positioned at 1541cm
-1About; Symmetry absorption peak eigenwert is positioned at 1442cm
-1At low band 613cm
-1About keep the Ti-O skeleton structure vibration peak of titanium dioxide.
Embodiment
The 500SN 630g that to get 100 ℃ of viscosity be 15cSt adds in the system fat still, adds the 200ml dehydrated alcohol, and heated constant temperature to 50 ℃ adds tetrabutyl titanate 28.8g and 12-oxystearic acid 50.8g, and constant temperature stirred 30 hours.After this, temperature is elevated to 95 ℃, adding concentration is the lithium hydroxide solution 17.8g of 20 heavy %, and 220 ℃ of heat temperature raisings add the 320g quenching oil.Reduce to below 70 ℃ when temperature, go out still.Grind twice with the three-wheel barreling.Product composition and performance are as shown in table 1.
Embodiment 2
The Viscotrol C 500g that to get 100 ℃ of viscosity be 18.8cSt adds in the system fat still, add the 800ml dehydrated alcohol, heated constant temperature to 50 ℃, add tetrabutyl titanate 144g and 12-oxystearic acid 254g, constant temperature stirred 10 hours, after this, temperature is elevated to 105 ℃, adding concentration is the lithium hydroxide solution 88.9g of 20 heavy %, and 240 ℃ of heat temperature raisings add the 250g quenching oil.Reduce to below 70 ℃ when temperature, go out still.Grind twice with the three-wheel barreling.Product composition and performance are as shown in table 1.
Embodiment 3
The ester class oil 440g that to get 100 ℃ of viscosity be 20cSt adds in the system fat still, adds the 200ml dehydrated alcohol, and heated constant temperature to 70 ℃ adds tetrabutyl titanate 68g and 12-oxystearic acid 120g, and constant temperature stirred 48 hours.After this, temperature is elevated to 95 ℃, adding concentration is the lithium hydroxide solution 42g of 20 heavy %, and 220 ℃ of heat temperature raisings add the 66g quenching oil.Reduce to below 70 ℃ when temperature, go out still.Grind twice with the three-wheel barreling.Product composition and performance are as shown in table 1.
Embodiment 4
Under evenly stirring, in the beaker that 100g benzene is housed, add titanium tetrachloride 47g, feed ammonia, and slowly add Virahol 60g and reacted 4 hours with 0.5mol/hr speed.After reaction stops, resultant of reaction was being filtered in static 10 hours, chloride precipitation and titanium isopropylate are separated, with the boiling water hydrolysis, and vigorous stirring makes its formation gel with filtrate alcohol titanium.Its adding is filled in the system fat still of ester class oil that 100 ℃ of viscosity of 600g are 20cSt, 74g 12-oxystearic acid, be elevated to 100 ℃, adding concentration is the lithium hydroxide solution 104g of 10 heavy %, and 240 ℃ of heat temperature raisings add the 300g quenching oil.Reduce to below 70 ℃ when temperature, go out still.Grind twice with the three-wheel barreling.Product performance are as shown in table 1.
Embodiment 5
Under evenly stirring, in the beaker that 200g benzene is housed, add titanium tetrachloride 118g, feed ammonia, and slowly add Virahol 148g and reacted 10 hours with 0.8mol/hr speed.After reaction stops, resultant of reaction was being filtered in static 4 hours, chloride precipitation and titanium isopropylate are separated, with the boiling water hydrolysis, and vigorous stirring makes its formation gel with filtrate alcohol titanium.In the system fat still with its adding 500SN that to fill 100 ℃ of viscosity of 500g be 20cSt, 186g 12-oxystearic acid, be elevated to 80 ℃, adding concentration is the lithium hydroxide solution 130g of 20 heavy %, and 200 ℃ of heat temperature raisings add the 250g quenching oil.Reduce to below 70 ℃ when temperature, go out still.Grind twice with the three-wheel barreling.Product composition and performance are as shown in table 1.
Comparative Examples 1
Prepare lubricating grease according to US 20030087768 disclosed methods.The paraffin base lubricating oil 70g that to get 100 ℃ of viscosity be 20cSt adds in the system fat still, and adding 12-oxystearic acid 8.4g stirring heating, when temperature is raised to 90 ℃, accelerate to stir, add 16.7 heavy % lithium hydroxide solution 6.72g, continue to be warming up to 220 ℃, add 21g surplus quenching oil, reduce to below 70 ℃ when temperature, go out still.Add 2.8 heavy % titania nanoparticles additives, after mixing, grind twice with the three-wheel barreling.Product composition and performance are as shown in table 1.
Table 1 grease composition and performance
| Embodiment |
| 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | Comparative Examples 1 | |
| Base oil, heavy % | 94 | 71 | 78 | 90 | 75 | 88 |
| Viscosifying agent, heavy % | 5.4 | 25.7 | 19.8 | 8.4 | 21 | 9.2 |
| Titanium dioxide, heavy % | 0.6 | 3.3 | 2.2 | 1.6 | 4.0 | 2.8 |
| 1/4 cone penetration, 0.1mm | 82 | 63 | 68 | 75 | 66 | 68 |
| Dropping point, ℃ | 298 | 293 | 281 | 260 | 255 | 183 |
| Oxidation onset temperature, ℃ | 193 | 197 | 199 | 194 | 196 | 173 |
| Divide oil, % | 0.3 | 0.0 | 0.2 | 0.18 | 0.11 | 2.3 |
| P B，N | 50 | 32 | 55 | 50 | 55 | 28 |
| P D，N | 200 | 200 | 160 | 160 | 160 | 160 |
| d 20 30，mm | 0.35 | 0.46 | 0.43 | 0.37 | 0.39 | 0.63 |
| ZMZ | 35.73 | 35.35 | 28.42 | 33.46 | 30.79 | 28.26 |
As can be seen from the above table, adopt preparation technology of the present invention, can obtain the lithium soap grease of high dropping point, and compare with the fat that prior art makes, have little branch oil, good oxidation stability, its extreme pressure and antiwear behavior also is better than the basic fat that traditional technology is made.
Claims (21)
1. the lithium soap grease of a high dropping point is a benchmark with the lubricating grease gross weight, contains following component:
1) base oil, content are 68～95 heavy %;
2) C6～C24 lipid acid lithium salts viscosifying agent, content are 4～30 heavy %;
3) titanium dioxide, content are 0.1～8 heavy %;
Said lubricating grease contains following three characteristic peaks in infrared spectrum, that is: eigenwert is positioned at 1555cm
-1～1530cm
-1Between the asymmetric absorption peak of O-Li of fatty acid lithium; Eigenwert is positioned at 1454cm
-1～1430cm
-1Between the O-Li symmetry absorption peak of fatty acid lithium; Eigenwert is positioned at 620cm
-1～595cm
-1Between the Ti-O skeleton structure vibration peak of titanium dioxide.
2. according to the described lubricating grease of claim 1, it is characterized in that the content of base oil is 75～90 heavy %, the content of lipid acid lithium salts viscosifying agent is 8～25 heavy %, and the content of titanium dioxide is 0.3～5 heavy %.
3. according to the described lubricating grease of claim 1, it is characterized in that the asymmetric absorption peak of the O-Li of fatty acid lithium is positioned at 1550cm
-1～1535cm
-1Between; The O-Li symmetry absorption peak of fatty acid lithium is positioned at 1450cm
-1～1435cm
-1Between; Titanium dioxide Ti-O skeleton structure vibration peak is positioned at 615cm
-1～600cm
-1Between.
4. according to the described lubricating grease of claim 1, it is characterized in that said base oil is mineral oil, vegetables oil, synthetic oil or its mixture that 100 ℃ of viscosity are 10～20cSt.
5. according to the described lubricating grease of claim 1, it is characterized in that the lipid acid in the said lipid acid lithium salts viscosifying agent is C8～C20 lipid acid.
6. according to claim 1 or 5 described lubricating grease, it is characterized in that the lipid acid in the said lipid acid lithium salts viscosifying agent is 12-oxystearic acid or stearic acid.
7. the preparation method of the described lithium base grease in high drop point of claim 1, comprise: in base oil, add organic solvent, tetrabutyl titanate and C6～C24 lipid acid, stirring reaction under 25～120 ℃ temperature, add lithium hydroxide solution at 50～120 ℃, be warming up to 180～260 ℃ and carry out the high temperature refining, add quenching oil, cooling is ground, wherein the gross weight of lipid acid and lithium hydroxide accounts for 4～30 heavy % of lubricating grease gross weight, and the mol ratio of lipid acid and tetrabutyl titanate is 1: 0.5～5.
8. according to the described preparation method of claim 7, it is characterized in that, in base oil, add polar organic solvent, tetrabutyl titanate and C8～C20 lipid acid, 40～90 ℃ of stirring reactions 2～72 hours, add lithium hydroxide solution at 80～110 ℃, be warming up to 200～240 ℃ of refinings 10～60 minutes, add quenching oil, cooling is ground.
9. according to the described preparation method of claim 7, it is characterized in that said base oil is mineral oil, vegetables oil, synthetic oil or its mixture that 100 ℃ of viscosity are 10～20cSt.
10. according to the described lubricating grease of claim 7, it is characterized in that said organic solvent is selected from tetrahydrofuran (THF), C1～C4 lipid acid, C2～C4 low-carbon alcohol, acetone or its mixture.
11., it is characterized in that said lipid acid is 12-oxystearic acid or stearic acid according to the described preparation method of claim 7.
12. according to the described preparation method of claim 7, it is characterized in that, the gross weight of lipid acid and lithium hydroxide accounts for 8～25 heavy % of lubricating grease gross weight, the add-on of lipid acid is 0.5～1.5 times of lithium hydroxide mole number, the mol ratio of lipid acid and tetrabutyl titanate is 1: 0.8～3, the mol ratio of lipid acid and organic solvent is 1: 5～20, and the add-on of quenching oil is 15～50 heavy % of base oil gross weight, and the concentration of lithium hydroxide solution is 5～50 heavy %.
13. the preparation method of the described lithium base grease in high drop point of claim 1 comprises:
1) adding titanium tetrachloride, alkali and C1～C4 low-carbon alcohol in organic solvent reacts, static, filtration, precipitation separation, the filtrate that to contain pure titanium is with 80～100 ℃ hot water hydrolysis, make it form gel, wherein the mol ratio of low-carbon alcohol and titanium tetrachloride is 1: 1～10, and the mol ratio of alkali and titanium tetrachloride is 1～10;
2) gel that step 1 is obtained mixes with base oil and C6～C24 lipid acid, add lithium hydroxide solution at 50～120 ℃, be warming up to 180～260 ℃ and carry out the high temperature refining, add quenching oil, cooling is ground, wherein the mol ratio of lipid acid and gel is 1: 0.5～5, and the gross weight of lipid acid and lithium hydroxide accounts for 4～30 heavy % of lubricating grease gross weight.
14., it is characterized in that the temperature of reaction of step 1 is 5～80 ℃ according to the described preparation method of claim 13, the mol ratio of low-carbon alcohol and titanium tetrachloride is 1: 2～6, the mol ratio of alkali and titanium tetrachloride is 2～6.
15., it is characterized in that the said organic solvent of step 1 is the non-polar organic solvent that is selected from benzene,toluene,xylene according to the described lubricating grease of claim 13.
16., it is characterized in that the said alkali of step 1 is ammonia according to the described preparation method of claim 13.
17., it is characterized in that the said low-carbon alcohol of step 1 is a Virahol according to the described preparation method of claim 13.
18. according to the described preparation method of claim 13, it is characterized in that, step 2 is that gel is mixed with base oil and C8～C20 lipid acid, add lithium hydroxide solution at 70～110 ℃, be warming up to 200～240 ℃ of refinings 10～60 minutes, add quenching oil, cooling is ground, the mol ratio of lipid acid and gel is 1: 0.8～3, and the gross weight of lipid acid and lithium hydroxide accounts for 8～25 heavy % of lubricating grease gross weight.
19., it is characterized in that base oil is mineral oil, vegetables oil, synthetic oil or its mixture that 100 ℃ of viscosity are 10～20cSt according to the described preparation method of claim 13.
20., it is characterized in that lipid acid is 12-oxystearic acid, stearic acid according to the described preparation method of claim 13.
21., it is characterized in that the add-on of lipid acid is 0.5～1.5 times of lithium hydroxide mole number according to the described preparation method of claim 13, the add-on of quenching oil is 15～50 heavy % of base oil gross weight, the concentration of lithium hydroxide solution is 5～50 heavy %.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101200670B (en) * | 2006-12-12 | 2010-05-19 | 中国石油天然气集团公司 | Composite lithium-base grease and method for making same |
| CN101892114A (en) * | 2010-06-29 | 2010-11-24 | 长安大学 | Lubricating grease composition specially for centralized lubrication of vehicle chassis |
| CN102137918A (en) * | 2008-08-11 | 2011-07-27 | 国际壳牌研究有限公司 | Lubricating compositions comprising a metal sulphide and an organosulphur compound |
| CN101205496B (en) * | 2006-12-18 | 2012-06-27 | 中国石油化工股份有限公司 | Grease additive, grease containing the same and preparation thereof |
| CN108822939A (en) * | 2018-07-19 | 2018-11-16 | 广州联博科技发展有限公司 | A kind of white and prepares method at lithium base grease |
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| JPS5216723B2 (en) * | 1974-07-31 | 1977-05-11 | ||
| US6474870B1 (en) * | 1999-10-05 | 2002-11-05 | Emerson Power Transmission Manufacturing, L.P. | Lubricated bearing assembly and method |
| DE10152432A1 (en) * | 2001-10-24 | 2003-05-08 | Trw Fahrwerksyst Gmbh & Co | Grease composition |
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2005
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101200670B (en) * | 2006-12-12 | 2010-05-19 | 中国石油天然气集团公司 | Composite lithium-base grease and method for making same |
| CN101205496B (en) * | 2006-12-18 | 2012-06-27 | 中国石油化工股份有限公司 | Grease additive, grease containing the same and preparation thereof |
| CN102137918A (en) * | 2008-08-11 | 2011-07-27 | 国际壳牌研究有限公司 | Lubricating compositions comprising a metal sulphide and an organosulphur compound |
| CN101892114A (en) * | 2010-06-29 | 2010-11-24 | 长安大学 | Lubricating grease composition specially for centralized lubrication of vehicle chassis |
| CN101892114B (en) * | 2010-06-29 | 2013-03-06 | 长安大学 | Lubricating grease composition specially for centralized lubrication of vehicle chassis |
| CN108822939A (en) * | 2018-07-19 | 2018-11-16 | 广州联博科技发展有限公司 | A kind of white and prepares method at lithium base grease |
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| CN100389183C (en) | 2008-05-21 |
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