CN1888036A - Composite calcium-base lubricating grease and its prepn - Google Patents
Composite calcium-base lubricating grease and its prepn Download PDFInfo
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Abstract
The present invention relates to one kind of composite calcium-base lubricating grease, which consists of base oil in 68-95 wt%, composite calcium-base thickener 4-30 wt% and titania 0.1-8 wt%, and the titania in the lubricant grease is preferably nanometer level particles. The present invention also provides three kinds of preparation process of the lubricant grease. The composite calcium-base lubricating grease of the present invention has the features of high oxidation stability, small surface hardening value change, high dropping point and high extreme pressure wear resistance, and may be used for lubricating at relatively high temperature and humidity condition and heavy load.
Description
Technical field
The present invention relates to lubricating grease and preparation method thereof, exactly is complex calcium lubricating grease and preparation method thereof.
Background technology
Complex calcium lubricating grease is a kind of heatproof, withstand voltage, broad-spectrum good lubricating grease, has mechanical stability and colloid stability preferably.
At present, the production technique of complex calcium lubricating grease can be divided into saponification, compound, be crowded into the fat three phases.As US 4,787, adopt C10～C20 synthetic fatty acid, middle molecule acid and Glacial acetic acid and calcium hydroxide reaction to form in 992.
In recent years,, introduce polyurea grease therein for improving the performance of composite calcium-base fat, this be because quicklime grease have case-hardened defective, use and storage aspect make troubles.It is mixed use with urea-base grease, both are had complementary advantages, overcome this drawback effectively.But this series products needs two kinds of fat of compound calcium and polyureas to mix, and raw materials for production and technology are all comparatively complicated.As US 5,084,193, US 4,902,435.CN1364859A discloses a kind of mixing thickened agent lubricant grease of high extreme pressure, described viscosifying agent is the mixture of polyurea thickening agent and composite calcium-base viscosifying agent, its preparation method is to obtain composite calcium-base fat and areidofat respectively, and then composite calcium-base fat and areidofat are mixed.
Summary of the invention
The present invention adopts new technology, and is keeping providing a kind of surface hardening value to change the complex calcium lubricating grease little, that extreme pressure property is good under the constant situation of the original every performance of compound calcium.
The present invention also provides the preparation method of above-mentioned composite calcium-base fat.
Complex calcium lubricating 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. composite calcium-base viscosifying agent, content are 4～30 heavy %, preferred 10～28 heavy %;
3. titanium dioxide, content are 0.1～8 heavy %, preferred 1.3～5 heavy %.
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 composite calcium-base viscosifying agent is to be formed by acid and calcium hydroxide or calcium oxide reaction, contains one or more C1～C8 small molecular organic acid and one or more C10～C24 long chain organic acid in the said acid at least.The mol ratio of small molecular organic acid and long chain organic acid is 15～50: 1, preferred 25～35: 1.Said small molecular organic acid preferable formic acid, acetate, propionic acid, sad, phenylformic acid, Whitfield's ointment or oxalic acid etc.Preferred 12 oxystearic acids of long chain organic acid or stearic acid.Can also optionally contain boric acid in the said acid, the mol ratio of boric acid and long chain organic acid is 0.5～5: 1, preferred 1.5～2.5: 1.
The existence form of said titanium dioxide in lubricating grease be nano_scale particle preferably.In infrared spectrum, the absorption peak of titanium dioxide appears at 650～670cm
-1, preferred 655～665cm
-1
Can also add additive as required in the quicklime grease provided by the invention, as oxidation inhibitor, extreme pressure anti-wear additives etc.Oxidation inhibitor can be amine antioxidants or phenolic antioxidant, or the mixture of the two.Said amine antioxidants can be an alkyl diphenylamine, as di-iso-octyldiphenylamine or dioctyl diphenylamine.Said phenolic antioxidant can be a shielding phenol, as 2, and 6-toluene di-tert-butyl phenol, 2,6-di-tert-butylphenol etc.Extreme pressure anti-wear additives can be the compound of molybdenumdisulphide, titaniferous or bismuth etc.
Can preparing of complex calcium lubricating grease provided by the invention by following three kinds of methods:
First kind of preparation method comprises:
At 25～120 ℃, in the mixed system that contains base oil, polar organic matter and tetrabutyl titanate, add bronsted lowry acids and bases bronsted lowry respectively, be warming up to 180～260 ℃ and carry out the high temperature refining, add quenching oil, cooling is ground, and adds additive as required, obtains lubricating grease of the present invention.By above reaction, tetrabutyl titanate is transformed into titanium oxide nanoparticles.
Bronsted lowry acids and bases bronsted lowry should add respectively, can add acid earlier, also can add alkali earlier.
The temperature of high temperature refining is preferably 200～240 ℃, and the refining time generally kept 10～60 minutes, preferred 20～40 minutes.The effect of high temperature refining is to make grease structure stable.
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.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 preferred C1 of said polar organic matter～C4 Fatty Alcohol(C12-C14 and C12-C18), acetone or tetrahydrofuran (THF) also can be these organic mixtures, wherein C1～preferred dehydrated alcohol of C4 Fatty Alcohol(C12-C14 and C12-C18), Virahol, isopropylcarbinol, propyl carbinol etc.
At least contain one or more C1～C8 small molecular organic acid and one or more C10～C24 long chain organic acid in the said acid.The mol ratio of small molecular organic acid and long chain organic acid is 50～15: 1, preferred 25～35: 1.Said small molecular organic acid preferable formic acid, acetate, propionic acid, sad, phenylformic acid, Whitfield's ointment or oxalic acid etc.Preferred 12 oxystearic acids of long chain organic acid or stearic acid.Can also optionally contain boric acid in the said acid, the mol ratio of boric acid and long chain organic acid is 5～0.5: 1, preferred 2.5～1.5: 1.
Said alkali is calcium hydroxide or calcium oxide.Calcium hydroxide or calcium oxide can be pressed powders, also can be suspension, preferred suspension.The solid content of suspension is 5～50 heavy %, preferred 10～12 heavy %.
Acid generates compound calcium viscosifying agent with calcium hydroxide or calcium oxide reaction.Total charging capacity of acid and calcium hydroxide or calcium oxide is considered as the weight of compound calcium viscosifying agent.Acid is roughly the same with calcium hydroxide or calcium oxide mole number, and the add-on of general acid can be 0.5～1.5 times of calcium hydroxide mole number, preferred 0.8～1.2 times.
Acid is about 1: 0.5 with the mol ratio of tetrabutyl titanate～and 5, preferred 1: 0.8～3.
Acid is about 1: 5 with the mol ratio of polar organic matter～and 20, preferred 1: 5～15.
Second kind of preparation method of complex calcium lubricating grease provided by the invention comprises:
Step 1: in non-polar organic solvent, add titanium tetrachloride, C1～C4 low-carbon alcohol and alkali and react, static, filtration, precipitation separation will react the filtrate water hydrolysis that contains pure titanium that generates, and stir to make it form gel.By above reaction, titanium tetrachloride is transformed into titanium oxide nanoparticles.
The mol ratio of low-carbon alcohol and titanium tetrachloride is 1: 1～10, preferred 1: 2～6.The add-on of alkali is controlled with the pH value, and the optimum range of pH value is 6～11, and preferred 6.5～9.
The temperature of reaction of titanium tetrachloride and low-carbon alcohol can be 5～80 ℃, and general normal temperature gets final product.Reaction times does not have special requirement, reaches higher conversion if wish reaction, then should react till precipitation no longer increases to the system.
Said non-polar organic solvent is conventional solvent, and the preferred aromatic hydrocarbons solvent is 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 ammonia or ammoniacal liquor, preferred ammoniacal liquor.The concentration of ammoniacal liquor can be 3～8mol/L.
Preferred 80～100 ℃ hot water of water that is used for hydrolysis filtrate, preferably boiling water.The volume of water is advisable to be fit to forming gel, generally is 1～5 times of filtrate volume, preferred 1～3 times.
C1～C4 low-carbon alcohol is selected from methyl alcohol, ethanol, propyl alcohol, Virahol or butanols, preferred Virahol.
Step 2: the gel that step 1 is obtained mixes with base oil, at 20～120 ℃, preferred 70～110 ℃ add acid and calcium hydroxide or calcium oxide respectively, 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.
Acid and calcium hydroxide or calcium oxide should add respectively, can add acid earlier, also can add alkali earlier.
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.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 %.
At least contain one or more C1～C8 small molecular organic acid and one or more C10～C24 long chain organic acid in the said acid.The mol ratio of small molecular organic acid and long chain organic acid is 50～15: 1, preferred 35～25: 1.Said small molecular organic acid preferable formic acid, acetate, propionic acid, sad, phenylformic acid, Whitfield's ointment or oxalic acid etc.Preferred 12 oxystearic acids of long chain organic acid or stearic acid.Can also optionally contain boric acid in the said acid, the mol ratio of boric acid and long chain organic acid is 0.5～5: 1, preferred 1.5～2.5: 1.
Acid is 1: 0.5～5 with the mol ratio of gel, preferred 1: 0.8～3.The mole number of gel is in the mole number of the titanium tetrachloride of adding in feeding intake.
Calcium hydroxide or calcium oxide can be pressed powders, also can be suspension, preferred suspension.The solid content of suspension is 5～50 heavy %, preferred 10～30 heavy %.
Acid generates compound calcium viscosifying agent with calcium hydroxide or calcium oxide reaction.Total charging capacity of acid and calcium hydroxide or calcium oxide is considered as the weight of compound calcium viscosifying agent.Acid is roughly the same with the mole number of calcium hydroxide or calcium oxide, and the add-on of general acid can be 0.5～1.5 times of calcium hydroxide mole number, preferred 0.8～1.2 times.
The temperature of high temperature refining is preferably 200～240 ℃, and the refining time generally kept 10～60 minutes, preferred 20～40 minutes.The effect of high temperature refining is to make grease structure stable.
The third preparation method of complex calcium lubricating grease provided by the invention comprises:
Titania powder is joined in the composite calcium-base plinth fat for preparing, and grinding evenly gets final product.The add-on of titania powder can be 0.1～8 heavy % of lubricating grease gross weight, preferred 1.3～5 heavy %.The particle diameter of titania powder is 5～100nm, preferred 20～80nm.Said composite calcium-base plinth fat can prepare according to ordinary method.
The complex calcium lubricating grease of the present invention's preparation has the advantages that oxidation stability is good, the surface hardening value changes little, high dropping point (greater than 300 ℃), extreme pressure anti-wear is good.Preparation technology is easy, easy handling.Prepared lubricating grease applicable to comparatively high temps and wet condition down in, heavy loading equipment lubricated.As aspects such as metallurgical rolling mill bearing, fire-resistant equipment kiln car bearing, casting knockout machinery, chemical industry roasting, mechanical workout thermal treatment, printing and dyeing burning machine, papermaking dry machine, rubber, plastic hot milling trains.
Description of drawings
Fig. 1 is the infrared spectrum of the lubricating grease of embodiment 1 preparation.661cm among the figure
-1The peak is the titanium dioxide absorption peak.
Fig. 2 is the infrared spectrum of the lubricating grease of embodiment 2 preparations.659cm among the figure
-1The peak is the titanium dioxide absorption peak.
Fig. 3 is the transmission electron microscope photo of the lubricating grease of embodiment 1 preparation.Show among the figure that titanium dioxide is nanoparticle.
Fig. 4 is the transmission electron microscope photo of the lubricating grease of embodiment 2 preparations.Show among the figure that titanium dioxide is nanoparticle.
Embodiment
Embodiment 1
Present embodiment adopts first method to prepare complex calcium lubricating grease.
The 500SN 630g that to get 100 ℃ of viscosity under the normal temperature be 15cSt, 1000ml dehydrated alcohol and tetrabutyl titanate 120g add in the system fat still, stir 2 hours, add 12-oxystearic acid 62g, 50 ℃ of constant temperature stirrings 4 hours.After this, add Glacial acetic acid 8.1g, n-caprylic acid 1.94g, after stirring, adding concentration is the calcium hydroxide suspension 40.8g of 16.6 heavy %, stirs, and continues to be warming up to 220 ℃, adds 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.Each component concentration is a base oil 89.9% in the lubricating grease, viscosifying agent 7.5%, titanium dioxide 2.6%.
Embodiment 2
Present embodiment adopts second method to prepare complex calcium lubricating grease.
Under evenly stirring, in the beaker that 100g benzene is housed, add titanium tetrachloride 47g, slowly add Virahol 427g, add 5mol/L ammoniacal liquor, till the pH value is 6.5.After reaction stops, resultant of reaction was filtered in static 10 hours again, chloride precipitation and titanium isopropylate are separated, with the boiling water hydrolysis, and vigorous stirring makes its formation gel with filtrate alcohol titanium.Be placed in the system fat still.
In this still, add the ester class oil that to fill 100 ℃ of viscosity of 600g be 20cSt, adding concentration is the calcium hydroxide suspension 728g of 12.5 heavy %, after stirring fast, add phenylformic acid 118.28g, boric acid 28.29g, add 12-oxystearic acid 98.18g in the time of 88 ℃, after this heat up gradually, add the 250g quenching oil until 240 ℃.Reduce to below 70 ℃ when temperature, go out still.Grind twice with the three-wheel barreling.Product performance are as shown in table 1.Each component concentration is a viscosifying agent content 27.8% in the lubricating grease, base oil content 70.5%, content of titanium dioxide 1.7%.
Embodiment 3
Present embodiment adopts first method to prepare complex calcium lubricating grease.
The 500SN 500g that to get 100 ℃ of viscosity under the normal temperature be 15cSt, 800ml acetone, tetrabutyl titanate 118g add in the system fat still, stir after 3 hours, add 12-oxystearic acid 66g, 60 ℃ were stirred after 6 hours, add Glacial acetic acid 66g, adding concentration is the aqua calcis 326g of 15 heavy %, and progressively heat temperature raising to 220 ℃ adds the 270g quenching oil.Reduce to below 70 ℃ when temperature, go out still.Grind twice with the three-wheel barreling.Each component concentration is a viscosifying agent content 18.4% in the lubricating grease, base oil content 78.6%, content of titanium dioxide 3.0%.Product composition and performance are as shown in table 1.
Embodiment 4
Present embodiment adopts second method to prepare complex calcium lubricating grease.
Under evenly stirring, in the beaker that 200g benzene is housed, add titanium tetrachloride 118g, slowly add Virahol 148g, and add 5mol/L ammoniacal liquor till the pH value is 9.After reaction stops, resultant of reaction was filtered in static 4 hours again, chloride precipitation and titanium isopropylate are separated, with the boiling water hydrolysis, and vigorous stirring makes its formation gel with filtrate alcohol titanium.
In this still, add ester class oil that to fill 100 ℃ of viscosity of 600g be 20cSt, add the calcium hydroxide suspension 216g that concentration is 15 heavy %, adding Glacial acetic acid 48.71g under the normal temperature, after treating that temperature is raised to 40 ℃, add n-caprylic acid 1.7g, be warmed up to 88 ℃, add 12-oxystearic acid 40.71g, heat up gradually, add the 325g quenching oil until 240 ℃.Reduce to below 70 ℃ when temperature, go out still.Grind twice with the three-wheel barreling.Product performance are as shown in table 1.Each component concentration is a viscosifying agent content 11.2% in the lubricating grease, base oil content 84.2%, content of titanium dioxide 4.6%.Grind twice with the three-wheel barreling.Product performance are as shown in table 1.
Embodiment 5
Present embodiment adopts the third method to prepare complex calcium lubricating grease.
The ﹠ Alpha ,-olefin oil oil 60g that to get 100 ℃ of viscosity be 20cSt adds in the system fat still, add 14.3 heavy % calcium hydroxide suspension 37.68g, 25 ℃ of following adding Glacial acetic acid 6.696g, add n-caprylic acid 1.607g, when being heated to 85 ℃, add 12-oxystearic acid 6.696g, stirring heating, continue to be warming up to 210 ℃, add the 25g quenching oil, add the 5g titania powder.Reduce to below 50 ℃ when temperature, go out still.Each component concentration is a viscosifying agent content 18.4% in the lubricating grease, base oil content 77%, content of titanium dioxide 4.6%.Grind twice with the three-wheel barreling.Product performance are as shown in table 1.
Comparative Examples 1
This Comparative Examples prepares complex calcium lubricating grease according to a conventional method.
The preparation method does not just add titanium dioxide with embodiment 5.Get prepare composite calcium-base fat 1000g, evaluate various performances.Product performance are as shown in table 1.
Comparative Examples 2
In Comparative Examples 1, add 1% di-iso-octyldiphenylamine, stir, grind twice with the three-wheel barreling.Product performance are as shown in table 1.
Table 1: PERFORMANCE OF GREASES
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | Comparative Examples 1 | Comparative Examples 2 | |
| Base oil, heavy % | 89.9 | 70.5 | 78.6 | 84.2 | 77.0 | 80 | 80 |
| Viscosifying agent, heavy % | 7.5 | 27.8 | 18.4 | 11.2 | 18.4 | 20 | 20 |
| Titanium dioxide, heavy % | 2.6 | 1.7 | 3.0 | 4.6 | 4.6 | ||
| 1/4 cone penetration, 0.1mm | 68 | 72 | 72 | 68 | 65 | 70 | 66 |
| Dropping point, ℃ | 325 | 318 | 324 | 316 | 316 | 324 | 301 |
| Oxidation onset temperature ℃ | 280.89 | 285.36 | 286.34 | 278.56 | 279.23 | 178.95. | 254.31 |
| Divide oil, % | 1.2 | 0.8 | 0.2 | 0.5 | 0.2 | 2.95 | 2.12 |
| The surface hardening value, (50 ℃, 24h) | 24 | 14 | 16 | 18 | 17 | 36 | 38 |
| P B，N | 85 | 80 | 85 | 80 | 85 | 75 | 80 |
| P D，N | 315 | 315 | 350 | 315 | 315 | 250 | 250 |
| d 20 30，mm | 0.35 | 0.36 | 0.37 | 0.35 | 0.36 | 0.60 | 0.62 |
| ZMZ | 44.78 | 43.25 | 42.95 | 45.21 | 44.58 | 40.23 | 42.63 |
As can be seen from the above table, adopt preparation technology of the present invention, the complex calcium lubricating grease that can obtain having good oxidation stability, the variation of surface hardening value is little, extreme pressure anti-wear is good.
Claims (28)
1. a complex calcium lubricating grease is a benchmark with the lubricating grease gross weight, contains following component:
1) base oil, content are 68～95 heavy %;
2) composite calcium-base viscosifying agent, content are 4～30 heavy %;
3) titanium dioxide, content are 0.1～8 heavy %.
2. according to the described lubricating grease of claim 1, it is characterized in that base oil content is 75～90 heavy %; Composite calcium-base viscosifying agent content is 10～28 heavy %; Content of titanium dioxide is 1.3～5 heavy %.
3. 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.
4. according to claim 1 or 3 described lubricating grease, it is characterized in that synthetic oil is ester class oil or polyolefin oil.
5. according to the described lubricating grease of claim 1, it is characterized in that, said composite calcium-base viscosifying agent is to be formed by acid and calcium hydroxide or calcium oxide reaction, at least contain one or more C1～C8 small molecular organic acid and one or more C10～C24 long chain organic acid in the said acid, the mol ratio of small molecular organic acid and long chain organic acid is 15～50: 1; Also optionally contain boric acid in the said acid, the mol ratio of boric acid and long chain organic acid is 5～0.5: 1.
6. according to the described lubricating grease of claim 5, it is characterized in that, small molecular organic acid is formic acid, acetate, propionic acid, sad, phenylformic acid, Whitfield's ointment or oxalic acid, and long chain organic acid is 12 oxystearic acids or stearic acid, and the mol ratio of small molecular organic acid and long chain organic acid is 25～35: 1.
7. according to the described lubricating grease of claim 1, it is characterized in that the existence form of titanium dioxide in lubricating grease is the Nano titanium dioxide particulate.
8. the preparation method of the described complex calcium lubricating grease of claim 1, comprise: at 25～120 ℃, in the mixed system that contains base oil, polar organic matter and tetrabutyl titanate, add acid and calcium hydroxide or calcium oxide respectively, be warming up to 180～260 ℃ and carry out the high temperature refining, add quenching oil, cooling is ground, and adds additive as required, gets final product; At least contain one or more C1～C8 small molecular organic acid and one or more C10～C24 long chain organic acid in the said acid, the mol ratio of small molecular organic acid and long chain organic acid is 15～50: 1.
9. according to the described preparation of greases method of claim 8, it is characterized in that the temperature of high temperature refining is 200～240 ℃.
10. according to the described preparation of greases method of claim 81, 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.
11., it is characterized in that said polar organic matter is ethanol, Virahol, isopropylcarbinol, propyl carbinol, acetone, tetrahydrofuran (THF) or its mixture according to the described preparation of greases method of claim 8.
12., it is characterized in that said small molecular organic acid is formic acid, acetate, propionic acid, sad, phenylformic acid, Whitfield's ointment or oxalic acid according to the described preparation of greases method of claim 8; Long chain organic acid is 12 oxystearic acids or stearic acid, and the mol ratio of small molecular organic acid and long chain organic acid is 25～35: 1.
13., it is characterized in that also optionally contain boric acid in the said acid, the mol ratio of boric acid and long chain organic acid is 5～0.5: 1 according to the described preparation of greases method of claim 8.
14., it is characterized in that acid is 1: 0.5～5 with the mol ratio of tetrabutyl titanate according to the described preparation of greases method of claim 8, acid is 1: 5～20 with the mol ratio of polar organic matter.
15., it is characterized in that acid is 1: 0.8～3 with the mol ratio of tetrabutyl titanate according to claim 1 or 14 described preparation of greases methods, acid is 1: 5～15 with the mol ratio of polar organic matter.
16. the preparation method of the described complex calcium lubricating grease of claim 1 comprises:
1) add titanium tetrachloride, C1～C4 low-carbon alcohol and alkali in non-polar organic solvent and react, static, filtration, precipitation separation with the filtrate water hydrolysis, stir and make it form gel; The mol ratio of low-carbon alcohol and titanium tetrachloride is 1: 1～10, and the scope of control pH value is 6～11;
2) gel that step 1 is obtained mixes with base oil, adds acid and calcium hydroxide or calcium oxide respectively at 20～120 ℃, is warming up to 180～260 ℃ and carries out the high temperature refining, adds quenching oil, and cooling is ground, and adds additive as required, gets final product; At least contain one or more C1～C8 small molecular organic acid and one or more C10～C24 long chain organic acid in the said acid, the mol ratio of small molecular organic acid and long chain organic acid is 15～50: 1.
17., it is characterized in that in the step 1), the mol ratio of low-carbon alcohol and titanium tetrachloride is 1: 2～6 according to the described preparation of greases method of claim 16, the scope of pH value is 6.5～9.
18., it is characterized in that in the step 1), said non-polar organic solvent is the aromatic solvent that is selected from benzene,toluene,xylene according to the described preparation of greases method of claim 16.
19., it is characterized in that in the step 1), said alkali is sodium hydroxide, potassium hydroxide, yellow soda ash, sodium bicarbonate, ammonia or ammoniacal liquor according to the described preparation of greases method of claim 16, the concentration of ammoniacal liquor is 3～8mol/L.
20., it is characterized in that in the step 1), what be used for hydrolysis filtrate is 80～100 ℃ hot water according to the described preparation of greases method of claim 16, the volume of water is 1～5 times of filtrate volume.
21., it is characterized in that in the step 1), said C1～C4 low-carbon alcohol is a Virahol according to the described preparation of greases method of claim 16.
22., it is characterized in that step 2 according to the described preparation of greases method of claim 16) in, said base oil is mineral oil, vegetables oil, synthetic oil or its mixture that 100 ℃ of viscosity are 10～20cSt.
23., it is characterized in that step 2 according to the described preparation of greases method of claim 16) in, also optionally containing boric acid in the said acid, the mol ratio of boric acid and long chain organic acid is 5～0.5: 1.
24. according to the described preparation of greases method of claim 16, it is characterized in that, step 2) in, said small molecular organic acid is selected from formic acid, acetate, propionic acid, sad, phenylformic acid, Whitfield's ointment or oxalic acid, and long chain organic acid is 12 oxystearic acids or stearic acid.
25., it is characterized in that step 2 according to the described preparation of greases method of claim 16) in, acid is 1: 0.5～5 with the mol ratio of gel.
26., it is characterized in that step 2 according to the described preparation of greases method of claim 16) in, the temperature of high temperature refining is 200～240 ℃.
27. the preparation method of the described complex calcium lubricating grease of claim 1 comprises: titania powder is joined in the composite calcium-base plinth fat, grind evenly.
28., it is characterized in that the particle diameter of titania powder is 5～100nm according to the described preparation of greases method of claim 27.
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