CN100378209C - High-dropping-point lubricating grease and prefabricated soap making method - Google Patents
High-dropping-point lubricating grease and prefabricated soap making method Download PDFInfo
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Abstract
The present invention provides a preparation method of prefabricated soap capable of being prepared into lubricating grease with high dropping point, which comprises: organic solvent, tetrabutyl titanate and the fatty acid of C6 to C24 are mixed to react by being stirred at the temperature of 25 to 120 DEGC, the mixed liquor of metal hydroxide and water is added at the temperature of 40 to 80 DEGC, the temperature is raised to 100 to 120 DEG C, the mixed solution is baked until moisture is completely vaporized, and the prefabricated soap is obtained; lubricating oil as base oil and the prefabricated soap prepared according to the method of the present invention are mixed and stirred, the mixture of the lubricating oil and the prefabricated soap is heated until the prefabricated soap is completely dissolved in the base oil, the constant temperature is kept for 0 to 2 hours, quenching oil is added or is not added, the mixture is cooled, an additive is added as required, and the grinding operation is performed as required so that the lubricating grease with high dropping point can be obtained.
Description
Technical field
The invention belongs to the lubricating grease field, relate in particular to the preparation of greases method.
Background technology
Usually the manufacture method of soap base grease can be divided into prefabricated soap method and two kinds of direct saponification methods.
The prefabricated soap method is with alkali soap fat or lipid acid, makes fatty acid metal soap class in advance, and soap class dewatered drying is standby.When making lubricating grease, the more fatty metallic soap of this dewatered drying is accurately measured by forming percentage ratio, drop into system fat in the refining still.
Directly saponification method promptly be under the part base oil exists with fat or the direct saponification of lipid acid, make the soap base transpiring moisture then, add remaining base oil and additive again, directly make lubricating grease.
Selecting for use of these two kinds of manufacture method mainly makes according to base oil and decides with the different of soap base type and to the requirement of finished product lubricating grease.As: among the ZL96120874.0, because hydrolytic action easily takes place in base oil in the presence of alkali and water, cause some performances of lubricating grease to be affected, can only adopt the preparation method of prefabricated soap in preparation of greases, it adopts is that oxyhydroxide that the preparation method of common soap base viscosifying agent is about to fat material (or lipid acid) and basic metal or alkaline-earth metal reacts and makes.
In recent years, lubricating grease on production technique or aspect the additive all constantly the development and perfect.Adopt the prefabricated soap of powder dried preparation lithium saponify as US20020022581, make in this way soap, simple to operate, it is convenient to store, can be during use according to required denseness, the base oil of allotment suitable proportion.But the prefabricated soap that this method makes is after making lubricating grease, and lubricating grease does not possess high dropping point performance.
Summary of the invention
The present invention adopts novel technical route, and a kind of preparation method who can be made into the prefabricated soap of high dropping point grease is provided.
The present invention also provides the preparation method of above-mentioned high dropping point grease.
The preparation method who can be made into the prefabricated soap of high dropping point grease provided by the invention comprises:
Organic solvent, tetrabutyl titanate and C6～C24 lipid acid is mixed, at 25～120 ℃, under preferred 40～90 ℃ temperature behind the stirring reaction, at 40～80 ℃, preferred 50～60 ℃ of mixed solutions that add metal hydroxides and water, be warmed up to 100～120 ℃, be baked to moisture and evaporate fully, promptly get prefabricated soap.
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.Metal hydroxides comprises the oxyhydroxide of first, second and third main group metal element, the oxyhydroxide of preferred lithium Li, calcium Ca, sodium Na, barium Ba, aluminium Al.Water furnishing mixed solution before the metal hydroxides powdered reaction is convenient to reaction evenly, and its concentration can be 5～50 heavy %, preferred 10～30 heavy %.
Wherein, the reaction of lipid acid and metal hydroxides generates the soap viscosifying agent.Best and the metal hydroxides complete reaction of lipid acid, the add-on of lipid acid can be 0.5～1.5 times of its complete reaction requirement, preferred 0.8～1 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.
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 preparation method of high dropping point grease provided by the invention comprises;
Lubricant base and prefabricated soap are mixed, stir, heat up, be dissolved in the base oil fully to prefabricated soap.Constant temperature 0～2 hour adds or does not add quenching oil, and cooling adds additive as required, promptly gets high dropping point grease of the present invention after grinding as required.
Usually, lithium soap grease, barium based grease need to add quenching oil in preparation process; Sodium base grease, quicklime grease and aluminium soap grease can not add quenching oil in preparation process.Lithium soap grease, barium based grease, sodium base grease can grind in preparation process.More than be those skilled in the art's general knowledge.
Said base oil is vegetables oil, synthetic oil, mineral oil and the mixing oil thereof 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 25～50 heavy %.
The add-on of prefabricated soap is 5～30 heavy % of base oil gross weight, preferred 15～25 heavy %.
Said additive can be 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 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 molybdenumdisulphide, naphthenic acid bismuth, zinc dialkyl dithiophosphate etc.
The lubricating grease made from the prefabricated soap of the inventive method preparation has characteristics such as high dropping point, high extreme pressure property, and kept other premium properties of lubricating grease.Preparation technology is easy, easy handling.
Embodiment
Embodiment 1:
The 50ml dehydrated alcohol, heated constant temperature to 60 ℃ adds tetrabutyl titanate 5.4g and 12-oxystearic acid 9.54g, and constant temperature stirred 30 hours.After this, temperature is elevated to 70 ℃, adding concentration is the lithium hydroxide solution 0.76g of 20 heavy %, and saponification reaction to moisture evaporates substantially, and reaction product is a partially dried powder, and oven dry is 36 hours in 120 ℃ baking oven, obtains prefabricated soap.The vegetables oil 55g that to get 11g prefabricated soap and 100 ℃ of viscosity be 13cSt mixes in system fat still, and 220 ℃ of heat temperature raisings add the 55g quenching oil.When temperature is reduced to below 70 ℃, add the 0.55g alkylated diphenylamine, go out still.Grind twice with the three-wheel barreling.Product composition and performance are as shown in table 1.
Embodiment 2:
The 200ml dehydrated alcohol adds 68g tetrabutyl titanate and stearic acid 113.6g, and constant temperature stirred 4 hours, continues reaction 30 hours.Be warmed up to 70 ℃, adding concentration is the aqua calcis 74g of 20 heavy %, and saponification reaction to moisture evaporates substantially, and reaction product is a partially dried powder, and oven dry is 24 hours in 150 ℃ baking oven, obtains prefabricated soap.After this, get another reactor B, the paraffin base lubricating oil 170g of 20cSt and prefabricated soap solid 30g when adding 100 ℃ stir, and temperature is elevated to 150 ℃, and constant temperature 2 hours is cooled to room temperature and goes out still.Product performance are as shown in table 1.
Embodiment 3:
200ml dehydrated alcohol and tetrabutyl titanate 20.95g and 12-oxystearic acid 37g are together, be heated to 70 ℃, constant temperature stirred 4 hours, temperature is elevated to 83 ℃, adding concentration is the barium hydroxide solution 10.48g of 20 heavy %, saponification reaction to moisture evaporates substantially, reaction product is a partially dried powder, oven dry is 24 hours in 120 ℃ baking oven, obtain prefabricated soap, the mineral oil that to take out with 100 ℃ of viscosity be 20cSt and the mixing oil 100g of ester class oil together add in the system fat still, and heat temperature raising to 220 ℃ adds the 50g quenching oil.Cool to room temperature grinds three times with the three-wheel barreling.Product performance are as shown in table 1.
Comparative Examples 1:
With embodiment 1 contrast, adopt prior art for preparing lithium base ester.
12-oxystearic acid 62g and 10ml water mix, temperature is elevated to 87 ℃, adding concentration is the lithium hydroxide solution 21g of 20 heavy %, saponification reaction to moisture evaporates substantially, and reaction product is a partially dried powder, and oven dry is 36 hours in 120 ℃ baking oven, obtain prefabricated soap, take out and 100 ℃ of vegetables oil 50g mixing that viscosity is 13cSt, 220 ℃ of heat temperature raisings add the 50g quenching oil.Temperature is reduced to room temperature.Add the 0.5g alkylated diphenylamine, go out still, grind three times with the three-wheel barreling.Product performance are as shown in table 1.
Comparative Examples 2:
With embodiment 2 contrasts, adopt prior art for preparing calcium base ester.
12-oxystearic acid 60g and 20ml water mix, temperature is elevated to 70 ℃, adds 20 heavy % calcium hydroxide suspension 37g, saponification reaction to moisture evaporates substantially, reaction product is a partially dried powder, oven dry is 24 hours in 150 ℃ baking oven, obtains prefabricated soap, takes out and base oil 400g that 100 ℃ of viscosity is 20cSt together adds and makes in the fat still, saponification is heated to 160 ℃, constant temperature 2 hours is reduced to below 50 ℃ when temperature, goes out still.Product performance are as shown in table 1.
Comparative Examples 3:
With embodiment 3 contrasts, adopt prior art for preparing barium base ester.
12-oxystearic acid 37g and 35ml water are together, be heated to 86 ℃, adding concentration is the barium hydroxide solution 10.48g of 20 heavy %, saponification reaction to moisture evaporates substantially, reaction product is a partially dried powder, and oven dry is 48 hours in 120 ℃ baking oven, obtains prefabricated soap, the mineral oil that to take out with 100 ℃ of viscosity be 20cSt and the mixing oil 100g of ester class oil together add in the system fat still 220 ℃ of heat temperature raisings, add the 50g quenching oil.Cool to room temperature grinds three times with the three-wheel barreling.Product performance are as shown in table 1.
Table 1: PERFORMANCE OF GREASES value among each embodiment
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Comparative Examples 1 | Comparative Examples 2 | Comparative Examples 3 | |
| 1/4 cone penetration, 0.1mm | 70 | 70 | 63 | 70 | 66 | 73 |
| Dropping point, ℃ | 253 | 121 | 189 | 176 | 90 | 159 |
| Oxidation onset temperature ℃ | 220.3 | / | 196.3 | 179.0 | / | 176.8 |
| Branch oil (100 ℃, 24h) % | 0.2 | 3 | / | 2.4 | 5 | / |
| The water pouring (38 ℃, 1h), % | / | / | 0.38 | / | / | 2.0 |
| P B，N | 550 | / | 980 | 200 | / | 200 |
| d 20 30，mm | 0.40 | 0.43 | 0.38 | 0.62 | 0.6 | 0.63 |
| ZMZ，N | 324.1 | 303.7 | 404.9 | 284.2 | 280 | 287.3 |
As can be seen from the above table, adopt the lubricating grease of the inventive method preparation, compare with the fat that prior art makes, have little branch oil, good anti-water drenching energy, good oxidation stability, its extreme pressure and antiwear behavior also is better than the basic fat that traditional technology is made.
Claims (15)
1. preparation method who can be made into the prefabricated soap of high dropping point grease, comprise: ethanol, tetrabutyl titanate and C6～C24 lipid acid or 12-oxystearic acid are mixed, at 25～120 ℃ of stirring reaction 2-72 hours, at 40～80 ℃ of mixed solutions that add metal hydroxides and water, be warmed up to 100～120 ℃, be baked to moisture and evaporate fully, promptly get prefabricated soap.
2. preparation method according to claim 1 is characterized in that, ethanol, tetrabutyl titanate and C6～C24 lipid acid is mixed, 40～90 ℃ of stirring reactions 12～48 hours, at 50～60 ℃ of mixed solutions that add metal hydroxidess and water.
3. preparation method according to claim 1 is characterized in that, the carbon number of lipid acid is C8～C20.
4. according to claim 1 or 3 described preparation methods, it is characterized in that lipid acid is stearic acid.
5. preparation method according to claim 1 is characterized in that, metal hydroxides is the oxyhydroxide of first main group, second main group or the 3rd main group metal element.
6. preparation method according to claim 1 is characterized in that, metal hydroxides is one or more in the oxyhydroxide of lithium, calcium, sodium, barium and aluminium.
7. preparation method according to claim 1 is characterized in that, the add-on of lipid acid is 0.5～1.5 times of its complete reaction requirement, and the mol ratio of lipid acid and tetrabutyl titanate is 1: 0.5～5, and lipid acid and alcoholic acid mol ratio are 1: 5～20.
8. according to claim 1 or 7 described preparation methods, it is characterized in that the add-on of lipid acid is 0.8～1 times of its complete reaction requirement, the mol ratio of lipid acid and tetrabutyl titanate is 1: 0.8～3, and lipid acid and alcoholic acid mol ratio are 1: 5～15.
9. the preparation method of a high dropping point grease comprises; The prefabricated soap of lubricant base and claim 1 preparation is mixed stirring, being heated to prefabricated soap is dissolved in the base oil fully, constant temperature 0～2 hour, add or do not add quenching oil, cooling, add additive as required, grind and get final product, wherein the add-on of prefabricated soap is 5～30 weight % of base oil gross weight.
10. preparation method according to claim 9 is characterized in that, base oil is one or more in 100 ℃ of viscosity be 10～20cSt vegetables oil, synthetic oil and mineral oil.
11. preparation method according to claim 9 is characterized in that, the add-on of quenching oil is 15～50 heavy % of base oil gross weight.
12. preparation method according to claim 9 is characterized in that, the add-on of prefabricated soap is 15～25 heavy % of base oil gross weight.
13. preparation method according to claim 9 is characterized in that, said additive is oxidation inhibitor and/or extreme pressure anti-wear additives.
14. preparation method according to claim 13, it is characterized in that, oxidation inhibitor is amine antioxidants or phenolic antioxidant or the mixture of the two, said amine antioxidants is di-iso-octyldiphenylamine, dioctyl diphenylamine or with the pentanoic of other alkyl, said phenolic antioxidant is 2,6 toluene di-tert-butyl phenols and/or 2,6 di-tert-butylphenols.
15. preparation method according to claim 13 is characterized in that, extreme pressure anti-wear additives is one or more in molybdenumdisulphide, naphthenic acid bismuth and the zinc dialkyl dithiophosphate.
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| CNB2005100049589A CN100378209C (en) | 2005-01-31 | 2005-01-31 | High-dropping-point lubricating grease and prefabricated soap making method |
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Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101407746B (en) * | 2007-10-11 | 2011-05-18 | 中国石油化工股份有限公司 | Modified vegetable oil |
| CN101845354B (en) * | 2010-02-02 | 2013-06-19 | 新疆现代石油化工股份有限公司 | Cotton picker spindle oil and preparation method thereof |
| CN104830436B (en) * | 2015-05-08 | 2017-11-17 | 江苏大学 | A kind of preparation method of high dropping point composite titan-based grease |
| CN108822939B (en) * | 2018-07-19 | 2022-04-01 | 广州联博科技发展有限公司 | White lithium-based lubricating grease and preparation method thereof |
| CN112980541B (en) * | 2019-12-16 | 2022-07-26 | 深圳市优宝新材料科技有限公司 | Prefabricated soap powder and preparation method thereof, lubricating grease and preparation method thereof |
| CN115851340B (en) * | 2022-11-10 | 2024-02-09 | 江苏龙蟠科技股份有限公司 | Preparation method of high-dropping-point single-lithium soap lubricating grease |
| CN116426328A (en) * | 2023-05-29 | 2023-07-14 | 泰奥星（天津）有限公司 | Lubricating grease, preparation method and application thereof |
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| JP2004099847A (en) * | 2002-07-16 | 2004-04-02 | Nsk Ltd | Grease composition and rolling device |
| CN1493673A (en) * | 2002-10-30 | 2004-05-05 | 中国石油化工股份有限公司 | Preparation method of polyurea-composite calcium lubricating grease |
| US20040092408A1 (en) * | 2002-10-31 | 2004-05-13 | Tomlin Scientific, Inc. | Rock bit grease composition |
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2005
- 2005-01-31 CN CNB2005100049589A patent/CN100378209C/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1218105A (en) * | 1997-09-09 | 1999-06-02 | 株式会社日立制作所 | Refrigerating machine oil composition and refrigeration and compressor using refrigerating machine oil composition |
| JP2004099847A (en) * | 2002-07-16 | 2004-04-02 | Nsk Ltd | Grease composition and rolling device |
| CN1493673A (en) * | 2002-10-30 | 2004-05-05 | 中国石油化工股份有限公司 | Preparation method of polyurea-composite calcium lubricating grease |
| US20040092408A1 (en) * | 2002-10-31 | 2004-05-13 | Tomlin Scientific, Inc. | Rock bit grease composition |
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