CN113122354B - Composite calcium-based lubricating grease and preparation method thereof - Google Patents
Composite calcium-based lubricating grease and preparation method thereof Download PDFInfo
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- CN113122354B CN113122354B CN202110423746.3A CN202110423746A CN113122354B CN 113122354 B CN113122354 B CN 113122354B CN 202110423746 A CN202110423746 A CN 202110423746A CN 113122354 B CN113122354 B CN 113122354B
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- Prior art keywords
- lubricating grease
- emulsion
- calcium
- based lubricating
- stirring
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Classifications
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M169/00—Lubricating compositions characterised by containing as components a mixture of at least two types of ingredient selected from base-materials, thickeners or additives, covered by the preceding groups, each of these compounds being essential
- C10M169/02—Mixtures of base-materials and thickeners
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
- C10M2207/10—Carboxylix acids; Neutral salts thereof
- C10M2207/12—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms
- C10M2207/125—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids
- C10M2207/126—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids monocarboxylic
- C10M2207/1265—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids monocarboxylic used as thickening agent
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
- C10M2207/10—Carboxylix acids; Neutral salts thereof
- C10M2207/12—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms
- C10M2207/125—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids
- C10M2207/128—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids containing hydroxy groups; Ethers thereof
- C10M2207/1285—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids containing hydroxy groups; Ethers thereof used as thickening agents
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2229/00—Organic macromolecular compounds containing atoms of elements not provided for in groups C10M2205/00, C10M2209/00, C10M2213/00, C10M2217/00, C10M2221/00 or C10M2225/00 as ingredients in lubricant compositions
- C10M2229/04—Siloxanes with specific structure
- C10M2229/042—Siloxanes with specific structure containing aromatic substituents
- C10M2229/0425—Siloxanes with specific structure containing aromatic substituents used as base material
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Organic Chemistry (AREA)
- Lubricants (AREA)
Abstract
The invention provides a preparation method of composite calcium-based lubricating grease, which comprises the following steps: mixing most of lime emulsion with base oil to obtain a mixture; mixing the mixture with fatty acid, adding the rest part of lime emulsion, and slowly stirring and keeping the temperature to obtain the composite calcium-based lubricating grease; the mass ratio of the most lime emulsion to the rest lime emulsion is (15-25): 1. the preparation method of the composite calcium-based lubricating grease provided by the invention is simple in operation method, and the prepared product has good quality stability. The invention also provides the composite calcium-based lubricating grease.
Description
Technical Field
The invention belongs to the technical field of lubricating grease, and particularly relates to composite calcium-based lubricating grease and a preparation method thereof.
Background
With the rapid development of industries such as automobiles, wind power, steel and the like, grease with high performance, long service life and high cost performance is getting more and more attention. The composite calcium-based lubricating grease has the characteristics of higher dropping point, good extreme pressure abrasion resistance, rust resistance, excellent water resistance and the like, and has wide raw material sources and obvious price advantage compared with common composite lithium, polyurea and other high-temperature lubricating grease, thus having good development prospect.
Disclosure of Invention
In view of the above, the invention aims to provide the composite calcium-based lubricating grease and the preparation method thereof, and the preparation method provided by the invention is simple in operation and good in quality stability of the prepared product.
The invention provides a preparation method of composite calcium-based lubricating grease, which comprises the following steps:
mixing most of lime emulsion with base oil to obtain a mixture;
mixing the mixture with fatty acid, adding the rest part of lime emulsion, and slowly stirring and keeping the temperature to obtain the composite calcium-based lubricating grease;
the mass ratio of the most lime emulsion to the rest lime emulsion is (15-25): 1.
preferably, the preparation method of the lime emulsion comprises the following steps:
mixing and stirring alkali and water to obtain lime emulsion;
the alkali is one or more selected from calcium oxide, calcium hydroxide and calcium acetate;
the water is deionized water;
the mass ratio of the alkali to the water is (0.5-1.5): (1-3).
Preferably, the base oil is selected from one or more of hydrogenated oil, poly alpha-olefin and silicone oil.
Preferably, the mass ratio of the lime emulsion to the base oil is (1-2): (10-15);
the mass ratio of the mixture to the fatty acid is (1-1.5): (3-4).
Preferably, the fatty acid is selected from one or more of stearic acid and dodecahydroxystearic acid.
Preferably, the temperature of the lime emulsion added in the rest part is 105-115 ℃.
Preferably, the temperature of the slow stirring is 220-240 ℃.
Preferably, the constant temperature is 245-255 ℃.
Preferably, the slow stirring speed is 20-60 rpm/min.
The invention provides the composite calcium-based lubricating grease prepared by the method.
The preparation method of the composite calcium-based lubricating grease provided by the invention is simple in operation method, and the prepared product has better quality stability.
Detailed Description
The following description of the technical solutions in the embodiments of the present invention will be clear and complete, and it is obvious that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other examples of modifications and alterations will be apparent to those skilled in the art based on the examples herein, and are intended to be within the scope of the invention. It should be understood that the embodiments of the present invention are only used for illustrating the technical effects of the present invention, and are not used for limiting the scope of the present invention. In the examples, the methods used are conventional methods unless otherwise specified.
The invention provides a preparation method of composite calcium-based lubricating grease, which comprises the following steps:
mixing most of lime emulsion with base oil to obtain a mixture;
mixing the mixture with fatty acid, adding the rest part of lime emulsion, and slowly stirring and keeping the temperature to obtain the composite calcium-based lubricating grease;
the mass ratio of the most lime emulsion to the rest lime emulsion is (15-25): 1.
in the present invention, the preparation method of the lime emulsion preferably comprises:
and mixing and stirring alkali and water to obtain lime emulsion.
In the present invention, the base is preferably one or more of calcium oxide, calcium hydroxide and calcium acetate, more preferably one or two of calcium oxide and calcium acetate, and most preferably calcium oxide and calcium acetate.
In the present invention, the water is preferably deionized water.
In the present invention, the mass ratio of the alkali to the water is preferably (0.5 to 1.5): (1 to 3), more preferably (0.5 to 1.3): (1 to 2.8), more preferably (0.6 to 0.9): (1.5 to 2.5), most preferably (0.7 to 0.8): (1.8-2.2).
In the present invention, the preparation method of the lime emulsion more preferably includes:
and adding water into calcium oxide for digestion, adding calcium acetate, and mixing and stirring to obtain lime emulsion.
In the invention, the mass ratio of the calcium oxide to the water is preferably (3-3.5): (8-9), more preferably (3.1-3.3): (8.2 to 8.8), more preferably (3.1 to 3.2): (8.4 to 8.6), most preferably 3.1:8.5; the mass of the calcium acetate is preferably 2.5 to 3.5 times, more preferably 2.8 to 3.2 times, and most preferably 3 times the mass of water.
In the present invention, the base oil is preferably one or more selected from hydrogenated oil, polyalphaolefin and silicone oil, more preferably silicone oil, and most preferably benzyl silicone oil.
In the invention, the mass ratio of the lime emulsion to the base oil is preferably (1-2): (10 to 15), more preferably (1 to 1.8): (10 to 13), most preferably (1.3 to 1.5): (11-12).
In the present invention, the lime emulsion and the base oil are preferably mixed uniformly for a period of preferably 5 to 15 minutes, more preferably 8 to 12 minutes, and most preferably 10 minutes.
In the present invention, the fatty acid is preferably one or more selected from stearic acid and dodecahydroxystearic acid, more preferably stearic acid.
In the present invention, the mass ratio of the mixture to the fatty acid is preferably (1 to 1.5): (3 to 4), more preferably (1 to 1.3): (3 to 3.8), most preferably (1.1 to 1.2): (3.3-3.5).
In the present invention, the method of mixing the mixture and the fatty acid preferably comprises:
after adding fatty acid to the mixture, stirring.
In the present invention, the stirring time is preferably 1 to 3 minutes, more preferably 1.5 to 2.5 minutes, and most preferably 2 minutes.
In the invention, the mass ratio of the most lime emulsion to the rest lime emulsion is preferably (18-22): 1, more preferably 20:1.
in the present invention, the temperature of the lime emulsion added to the remainder is preferably 105 to 115 ℃, more preferably 108 to 112 ℃, and most preferably 110 ℃.
In the invention, the temperature of the slow stirring is preferably 225-235 ℃, more preferably 228-232 ℃ and most preferably 230 ℃; the speed of the slow stirring is preferably 20 to 60rpm/min, more preferably 20 to 40rpm/min, and most preferably 30rpm/min.
In the present invention, the constant temperature is preferably 245 to 255 ℃, more preferably 248 to 252 ℃, and most preferably 250 ℃; the constant temperature is preferably maintained for 20 to 40 minutes, more preferably 25 to 35 minutes, and most preferably 30 minutes.
In the present invention, the constant temperature preferably further comprises:
and cooling and grinding the product after constant temperature into grease to obtain the composite calcium-based lubricating grease.
The invention also provides the composite calcium-based lubricating grease prepared by the method.
The preparation method of the composite calcium-based lubricating grease provided by the invention is simple in operation method, and the prepared product has better quality stability, and particularly, the composite calcium-based lubricating grease with better performance is prepared by adopting a slow stirring constant temperature process.
The raw materials used in the following examples of the present invention are all commercially available.
Example 1
Adding 8.5g of water into 3.1g of calcium oxide for digestion, adding calcium acetate (the mass is 3 times of the mass of water), mixing and stirring, adding most of the mixed emulsion into benzyl silicone oil, stirring for 10min, adding 13g of stearic acid, stirring for 2min, adding the rest emulsion at 110 ℃, slowly stirring at 230 ℃ (the mass ratio of the rest emulsion to the rest emulsion is 20:1), keeping the temperature at 250 ℃ for 20min, cooling and grinding to form grease, and obtaining the composite calcium-based lubricating grease.
Example 2
3.1g of calcium oxide is added with 8.5g of water for digestion, then calcium acetate (the mass is 3 times of the mass of water) is added, mixing and stirring are carried out, most of the mixed emulsion is added into benzyl silicone oil, stirring is carried out for 10min, 13g of stearic acid is added, stirring is carried out for 2min, the rest emulsion (the mass ratio of most of the emulsion to the rest emulsion is 20:1) is added at 110 ℃, and the temperature is increased to 230 ℃, and cooling and grinding are carried out, so as to obtain the composite calcium-based lubricating grease.
Example 3
3.1g of calcium oxide is added with 8.5g of water for digestion, then calcium acetate (the mass is 3 times of the mass of water) is added, the mixture is mixed and stirred, all the mixed emulsion is added into benzyl silicone oil, the mixture is stirred for 10min, 13g of stearic acid is added, the mixture is stirred for 2min, the mixture is slowly stirred at 230 ℃ for 20min at the constant temperature of 250 ℃, and the mixture is cooled and milled to form grease, thus obtaining the composite calcium-based grease.
Example 4
Adding 8.5g of water into 3.1g of calcium oxide for digestion, adding calcium acetate (the mass is 3 times of the mass of water), mixing and stirring, adding most of the mixed emulsion into benzyl silicone oil, stirring for 10min, adding 13g of stearic acid, stirring for 2min, adding the rest emulsion at 110 ℃, slowly stirring at 230 ℃ at the speed of 60rpm/min, keeping the temperature at 250 ℃ for 20min, cooling and grinding to form grease, and obtaining the composite calcium-based lubricating grease.
Performance detection
The complex calcium-based greases prepared in examples 1 to 4 of the present invention were subjected to performance test of working cone penetration (measured according to GB/T269 standard) and dropping point (measured according to SH/T0115 standard), the test results are shown in Table 1, and Table 1 shows the performance test results of the complex calcium-based greases prepared in examples of the present invention.
TABLE 1 Performance test results of composite calcium-based grease prepared in the examples of the present invention
| Example 1 | Example 2 | Example 3 | Example 4 | |
| 1/4 working cone penetration, 0.1mm | 71 | 86 | 74 | 82 |
| Drop point, DEG C | 220 | 202 | 161 | 207 |
The preparation method of the composite calcium-based lubricating grease provided by the invention is simple in operation method, and the prepared product has better quality stability, and particularly, the composite calcium-based lubricating grease with better performance is obtained through a slow stirring constant temperature process and a method of adding lime emulsion step by step.
While the invention has been described with respect to the preferred embodiments, it should be noted that modifications and adaptations to those skilled in the art may be made without departing from the principles of the present invention and are intended to be within the scope of the present invention.
Claims (1)
1. A preparation method of composite calcium-based lubricating grease comprises the following steps:
adding 8.5g of water into 3.1g of calcium oxide for digestion, adding calcium acetate with the mass of 3 times of the mass of the water, mixing and stirring to obtain lime emulsion, adding most of the emulsion into benzyl silicone oil, stirring for 10min, adding 13g of stearic acid, stirring for 2min, adding residual emulsion at 110 ℃, wherein the mass ratio of most of the emulsion to the residual emulsion is 20: slowly stirring at 1,230deg.C at 30rpm for 20min at 250deg.C, cooling, and grinding to obtain composite calcium-based grease.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110423746.3A CN113122354B (en) | 2021-04-20 | 2021-04-20 | Composite calcium-based lubricating grease and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110423746.3A CN113122354B (en) | 2021-04-20 | 2021-04-20 | Composite calcium-based lubricating grease and preparation method thereof |
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| Publication Number | Publication Date |
|---|---|
| CN113122354A CN113122354A (en) | 2021-07-16 |
| CN113122354B true CN113122354B (en) | 2023-08-15 |
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| CN202110423746.3A Active CN113122354B (en) | 2021-04-20 | 2021-04-20 | Composite calcium-based lubricating grease and preparation method thereof |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4483776A (en) * | 1983-06-17 | 1984-11-20 | Texaco Inc. | Lithium complex soap thickened grease containing calcium acetate |
| CN1075746A (en) * | 1992-02-22 | 1993-09-01 | 中国石油化工总公司石油化工科学研究院 | A kind of lubricating grease for sugar press and preparation method thereof that is used for |
| JP2009249419A (en) * | 2008-04-02 | 2009-10-29 | Chuo Yuka Kk | Calcium complex grease |
| CN101935573A (en) * | 2010-10-11 | 2011-01-05 | 长沙众城石油化工有限责任公司 | Complex calcium lubricating grease and production technology thereof |
| CN102604723A (en) * | 2012-02-09 | 2012-07-25 | 中山大学 | Lubricating grease composition and preparation method thereof |
| CN111718778A (en) * | 2020-06-23 | 2020-09-29 | 长沙众城石油化工有限责任公司 | Composite calcium-based lubricating grease and preparation method thereof |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE102010006745A1 (en) * | 2010-02-02 | 2011-08-04 | Fuchs Petrolub AG, 68169 | Greases containing lignosulfonate, their preparation and use |
-
2021
- 2021-04-20 CN CN202110423746.3A patent/CN113122354B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4483776A (en) * | 1983-06-17 | 1984-11-20 | Texaco Inc. | Lithium complex soap thickened grease containing calcium acetate |
| CN1075746A (en) * | 1992-02-22 | 1993-09-01 | 中国石油化工总公司石油化工科学研究院 | A kind of lubricating grease for sugar press and preparation method thereof that is used for |
| JP2009249419A (en) * | 2008-04-02 | 2009-10-29 | Chuo Yuka Kk | Calcium complex grease |
| CN101935573A (en) * | 2010-10-11 | 2011-01-05 | 长沙众城石油化工有限责任公司 | Complex calcium lubricating grease and production technology thereof |
| CN102604723A (en) * | 2012-02-09 | 2012-07-25 | 中山大学 | Lubricating grease composition and preparation method thereof |
| CN111718778A (en) * | 2020-06-23 | 2020-09-29 | 长沙众城石油化工有限责任公司 | Composite calcium-based lubricating grease and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 陈东 陈英 主编.《工作锥入度测定》.《油气质量检验教程》.海洋出版社,2017, * |
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