CN108219914B - Preparation method of sol antifriction lubricating oil - Google Patents
Preparation method of sol antifriction lubricating oil Download PDFInfo
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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
- C10M177/00—Special methods of preparation of lubricating compositions; Chemical modification by after-treatment of components or of the whole of a lubricating composition, not covered by other classes
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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
- C10M141/00—Lubricating compositions characterised by the additive being a mixture of two or more compounds covered by more than one of the main groups C10M125/00 - C10M139/00, each of these compounds being essential
- C10M141/10—Lubricating compositions characterised by the additive being a mixture of two or more compounds covered by more than one of the main groups C10M125/00 - C10M139/00, each of these compounds being essential at least one of them being an organic phosphorus-containing compound
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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
- C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
- C10M2201/06—Metal compounds
- C10M2201/062—Oxides; Hydroxides; Carbonates or bicarbonates
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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
- C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
- C10M2201/10—Compounds containing silicon
- C10M2201/105—Silica
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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
- C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
- C10M2201/14—Inorganic compounds or elements as ingredients in lubricant compositions inorganic compounds surface treated with organic compounds
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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
- 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
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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
- C10M2215/00—Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
- C10M2215/02—Amines, e.g. polyalkylene polyamines; Quaternary amines
- C10M2215/04—Amines, e.g. polyalkylene polyamines; Quaternary amines having amino groups bound to acyclic or cycloaliphatic carbon atoms
- C10M2215/042—Amines, e.g. polyalkylene polyamines; Quaternary amines having amino groups bound to acyclic or cycloaliphatic carbon atoms containing hydroxy groups; Alkoxylated derivatives thereof
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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
- C10M2223/00—Organic non-macromolecular compounds containing phosphorus as ingredients in lubricant compositions
- C10M2223/02—Organic non-macromolecular compounds containing phosphorus as ingredients in lubricant compositions having no phosphorus-to-carbon bonds
- C10M2223/04—Phosphate esters
- C10M2223/047—Thioderivatives not containing metallic elements
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2010/00—Metal present as such or in compounds
- C10N2010/02—Groups 1 or 11
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
- C10N2030/06—Oiliness; Film-strength; Anti-wear; Resistance to extreme pressure
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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 discloses a preparation method of sol antifriction lubricating oil, which adopts saponification dispersion of inorganic composite filler, not only can effectively and uniformly disperse the composite filler in the lubricating oil, but also can increase the thickness of an oil film, improve the bearing capacity of the lubricating oil, and because the composite filler also has self-lubricating effect, the modified composite filler can be uniformly and stably dispersed in base oil, can be placed for a long time without precipitation, and has wide application prospect.
Description
Technical Field
The invention belongs to the field of lubricating oil, and particularly relates to a preparation method of sol antifriction lubricating oil.
Background
Lubricating oils are generally composed of two parts, a base oil and additives. The base oil is the main component of the lubricating oil, determines the basic properties of the lubricating oil, and the additive can make up and improve the deficiency in the performance of the base oil, endows certain new performances and is an important component of the lubricating oil. The lubricating oil base oil mainly comprises mineral base oil, synthetic base oil and biological base oil. The mineral base oil has wide application and large using amount, but some application occasions need to use a product prepared by synthetic base oil and biological oil base oil, so the two base oils are rapidly developed;
the use of friction reducing antiwear agents has long been a lack of desirable products. The graphite and the molybdenum disulfide of the inorganic substance have good friction reduction and wear resistance, and play a good role as a solid lubricant, but are difficult to use in liquid lubricating materials due to poor oil solubility. Although the organic matter containing non-metal sulfur, phosphorus, boron and chlorine solves the problem of oil solubility, the non-metal characteristic of the organic matter is limited in the performance of friction reduction and wear resistance, so how to improve the dispersion effect of the inorganic matter in the lubricating oil is the focus of research at present.
Disclosure of Invention
The invention aims to provide a preparation method of sol antifriction lubricating oil aiming at the defects and shortcomings of the prior art.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of sol antifriction lubricating oil comprises the following steps:
(1) adding 0.8-1 part by weight of dialkyl dithiophosphate into deionized water with the weight 14-20 times of that of the dialkyl dithiophosphate, and uniformly stirring to obtain a phosphoric acid solution;
(2) adding 10-16 parts by weight of ethyl orthosilicate into deionized water which is 10-15 times of the weight of the ethyl orthosilicate, adding soda, adjusting the pH to 11-12, stirring for reacting for 3-4 hours, adding the phosphoric acid solution, raising the temperature to 60-65 ℃, preserving the temperature and stirring for 20-30 minutes to obtain a sol solution;
(3) adding 2-3 parts by weight of saponification solution into 10-14 times of anhydrous ethanol, uniformly stirring, adding 4-5 parts by weight of triethanolamine, performing ultrasonic treatment for 3-5 minutes, and distilling to remove ethanol to obtain pretreated alcohol amine;
(4) adding 1-2 parts by weight of molybdenum dioxide into the sol solution, uniformly stirring, filtering, washing the precipitate with water, and drying at the temperature of 50-55 ℃ for 1-2 hours in vacuum to obtain molybdenum dioxide composite sol;
(5) mixing 7-9 parts by weight of oleic acid with the molybdenum dioxide composite sol, feeding the mixture into a reaction kettle, adding a solvent which is 1.5-2 times of the weight of the mixture, stirring and mixing for 2-3 hours, and removing the solvent by reduced pressure distillation to obtain an oleic acid composite sol;
(6) and (2) adding the pretreated alcohol amine into the oil acidification composite sol, uniformly stirring, adding 0.01-0.02 part by weight of catalyst, raising the temperature to 90-95 ℃, keeping the temperature, stirring for 2-3 hours, cooling, adding 60-70 parts by weight of base oil, and uniformly stirring to obtain the sol antifriction lubricating oil.
The solvent is dimethyl carbonate.
The catalyst is nickel oxide.
The saponification liquid is prepared from the following raw materials in parts by weight:
20-30 parts of ricinoleic acid ester, 1.4-2 parts of ammonium molybdate and 36-41 parts of 0.8-1mol/l sodium hydroxide solution.
The preparation method of the saponification liquid comprises the following steps:
adding ammonium molybdate into deionized water with the weight 10-16 times of that of the ammonium molybdate, and uniformly stirring;
and (2) feeding ricinoleic acid ester into a constant-temperature water bath at 50-65 ℃, adding the ammonium molybdate aqueous solution, keeping the temperature and stirring for 10-20 minutes, dropwise adding the 0.8-1mol/l sodium hydroxide solution, raising the temperature of the water bath to 85-90 ℃ after dropwise adding, keeping the temperature and stirring for 30-40 minutes, discharging and cooling to obtain the saponification solution.
The sol antifriction lubricating oil is prepared by the preparation method of the sol antifriction lubricating oil.
The invention has the advantages that:
the invention takes molybdenum dioxide and silica sol as inorganic lubricating fillers, and in the process of treating the composite filler, tetraethoxysilane is taken as a precursor, the hydrolyzed sol is mixed with the molybdenum dioxide, oleic acid is adopted for treatment, the surface activity of the molybdenum dioxide is improved, and then the molybdenum dioxide and triethanolamine are mixed to generate a saponification activating agent under the action of a catalyst, so that the dispersion compatibility of the composite filler in lubricating oil is further improved, and meanwhile, the generated saponification activating agent also has a certain lubricating effect The alkaline solution is used as a raw material, and the lubricant ammonium molybdate is introduced in the saponification reaction process, so that the lubricating effect is further improved.
Detailed Description
Example 1
A preparation method of sol antifriction lubricating oil comprises the following steps:
(1) adding 1 part by weight of dialkyl dithiophosphate into deionized water with the weight being 20 times of that of the dialkyl dithiophosphate, and uniformly stirring to obtain a phosphoric acid solution;
(2) adding 16 parts by weight of tetraethoxysilane into deionized water 15 times the weight of tetraethoxysilane, adding soda, adjusting the pH value to 12, stirring and reacting for 4 hours, adding the phosphoric acid solution, raising the temperature to 65 ℃, preserving the temperature and stirring for 30 minutes to obtain a sol solution;
(3) adding 3 parts by weight of saponification solution into 14 times of absolute ethyl alcohol, uniformly stirring, adding 5 parts by weight of triethanolamine, carrying out ultrasonic treatment for 5 minutes, and distilling to remove the ethyl alcohol to obtain pretreated alcohol amine;
(4) adding 2 parts by weight of molybdenum dioxide into the sol solution, uniformly stirring, filtering, washing the precipitate with water, and drying at 55 ℃ in vacuum for 2 hours to obtain molybdenum dioxide composite sol;
(5) mixing 9 parts by weight of oleic acid with the molybdenum dioxide composite sol, feeding the mixture into a reaction kettle, adding a solvent which is 2 times of the weight of the mixture, stirring and mixing the mixture for 3 hours, and removing the solvent by reduced pressure distillation to obtain an oleic acid composite sol;
(6) and (2) adding the pretreated alcohol amine into the oil acidification composite sol, uniformly stirring, adding 0.02 part by weight of catalyst, raising the temperature to 95 ℃, keeping the temperature and stirring for 3 hours, cooling, adding 70 parts by weight of base oil, and uniformly stirring to obtain the sol antifriction lubricating oil.
The solvent is dimethyl carbonate.
The catalyst is nickel oxide.
The saponification liquid is prepared from the following raw materials in parts by weight:
ricinoleic acid ester 20, ammonium molybdate 1.4, 0.8mol/l sodium hydroxide solution 36.
The preparation method of the saponification liquid comprises the following steps:
adding ammonium molybdate into deionized water with the weight being 10 times of that of the ammonium molybdate, and uniformly stirring;
and (2) feeding ricinoleate into a constant-temperature water bath at 50 ℃, adding the ammonium molybdate aqueous solution, preserving heat and stirring for 10 minutes, dropwise adding the 0.1mol/l sodium hydroxide solution, raising the temperature of the water bath to 85 ℃ after dropwise adding, preserving heat and stirring for 30 minutes, discharging and cooling to obtain the saponification solution.
Example 2
A preparation method of sol antifriction lubricating oil comprises the following steps:
(1) adding 0.8 weight part of dialkyl dithiophosphate into deionized water with the weight 14 times of that of the dialkyl dithiophosphate, and uniformly stirring to obtain a phosphoric acid solution;
(2) adding 10 parts by weight of ethyl orthosilicate into deionized water which is 10 times of the weight of the ethyl orthosilicate, adding soda, adjusting the pH to 11, stirring and reacting for 3 hours, adding the phosphoric acid solution, raising the temperature to 60 ℃, preserving the temperature and stirring for 20 minutes to obtain a sol solution;
(3) adding 2 parts by weight of saponification solution into 10 times of anhydrous ethanol, uniformly stirring, adding 4 parts by weight of triethanolamine, performing ultrasonic treatment for 3 minutes, and distilling to remove ethanol to obtain pretreated alcohol amine;
(4) adding 1 part by weight of molybdenum dioxide into the sol solution, uniformly stirring, filtering, washing the precipitate with water, and drying at the temperature of 50 ℃ for 1 hour in vacuum to obtain molybdenum dioxide composite sol;
(5) mixing 7 parts by weight of oleic acid with the molybdenum dioxide composite sol, feeding the mixture into a reaction kettle, adding a solvent which is 1.5 times of the weight of the mixture, stirring and mixing for 2 hours, and removing the solvent by reduced pressure distillation to obtain an oleic acid composite sol;
(6) and (2) adding the pretreated alcohol amine into the oil acidification composite sol, uniformly stirring, adding 0.01 part by weight of catalyst, raising the temperature to 90 ℃, keeping the temperature and stirring for 2 hours, cooling, adding 6 parts by weight of base oil, and uniformly stirring to obtain the sol antifriction lubricating oil.
The solvent is dimethyl carbonate.
The catalyst is nickel oxide.
The saponification liquid is prepared from the following raw materials in parts by weight:
ricinoleic acid ester 30, ammonium molybdate 2, and 1mol/l sodium hydroxide solution 41.
The preparation method of the saponification liquid comprises the following steps:
adding ammonium molybdate into deionized water with the weight 16 times of that of the ammonium molybdate, and uniformly stirring;
and (2) feeding ricinoleate into a constant-temperature water bath at 65 ℃, adding the ammonium molybdate aqueous solution, preserving heat and stirring for 20 minutes, dropwise adding the 1mol/l sodium hydroxide solution, raising the water bath temperature to 90 ℃ after dropwise adding, preserving heat and stirring for 40 minutes, discharging and cooling to obtain the saponification solution.
And (3) performance testing:
appearance: no precipitation, no layering and no crystal precipitation;
and (3) wear resistance test:
the sol antifriction lubricant of example 1, the sol antifriction lubricant of example 2, the commercially available molybdenum thiophosphate friction reducer, and the commercially available molybdenum carbamate friction reducer of the present invention were added to the national standard SJ10W30 oil in a proportion of 0.5%. The antifriction and antiwear performances are measured by a four-ball method. The experimental conditions were: the oil temperature is 80 ℃, the time is 30min, the load is 392N, and the test result is as follows:
embodiment 1 of the present invention:
the diameter of the abrasion marks: 0.38mm, average coefficient of friction: 0.057;
embodiment 2 of the present invention:
the diameter of the abrasion marks: 0.40mm, average coefficient of friction: 0.060;
commercial molybdenum thiophosphate friction reducers:
the diameter of the abrasion marks: 0.49mm, average coefficient of friction: 0.087;
commercial molybdenum carbamate friction reducer:
the diameter of the abrasion marks: 0.53mm, average coefficient of friction: 0.101.
the test results show that the sol antifriction lubricating oil has excellent antifriction and antiwear performances and wide application prospect.
Claims (4)
1. The preparation method of the sol antifriction lubricating oil is characterized by comprising the following steps:
(1) adding 0.8-1 part by weight of dialkyl dithiophosphate into deionized water with the weight 14-20 times of that of the dialkyl dithiophosphate, and uniformly stirring to obtain a phosphoric acid solution;
(2) adding 10-16 parts by weight of ethyl orthosilicate into deionized water which is 10-15 times of the weight of the ethyl orthosilicate, adding soda, adjusting the pH to 11-12, stirring for reacting for 3-4 hours, adding the phosphoric acid solution, raising the temperature to 60-65 ℃, preserving the temperature and stirring for 20-30 minutes to obtain a sol solution;
(3) adding 2-3 parts by weight of saponification solution into 10-14 times of anhydrous ethanol, uniformly stirring, adding 4-5 parts by weight of triethanolamine, performing ultrasonic treatment for 3-5 minutes, and distilling to remove ethanol to obtain pretreated alcohol amine;
(4) adding 1-2 parts by weight of molybdenum dioxide into the sol solution, uniformly stirring, filtering, washing the precipitate with water, and drying at the temperature of 50-55 ℃ for 1-2 hours in vacuum to obtain molybdenum dioxide composite sol;
(5) mixing 7-9 parts by weight of oleic acid with the molybdenum dioxide composite sol, feeding the mixture into a reaction kettle, adding a solvent which is 1.5-2 times of the weight of the mixture, stirring and mixing for 2-3 hours, and removing the solvent by reduced pressure distillation to obtain an oleic acid composite sol;
(6) adding the pretreated alcohol amine into the oil acidification composite sol, uniformly stirring, adding 0.01-0.02 part by weight of catalyst, raising the temperature to 90-95 ℃, keeping the temperature and stirring for 2-3 hours, cooling, adding 60-70 parts by weight of base oil, and uniformly stirring to obtain the sol antifriction lubricating oil
The catalyst is nickel oxide, and the nickel oxide,
the saponification liquid is prepared from the following raw materials in parts by weight:
20-30 parts of ricinoleic acid ester, 1.4-2 parts of ammonium molybdate and 36-41 parts of 0.8-1mol/l sodium hydroxide solution.
2. The method of claim 1, wherein the solvent is dimethyl carbonate.
3. The method for preparing the sol antifriction lubricating oil according to claim 1, characterized in that the method for preparing the saponification solution comprises the following steps:
adding ammonium molybdate into deionized water with the weight 10-16 times of that of the ammonium molybdate, and uniformly stirring;
and (2) feeding ricinoleic acid ester into a constant-temperature water bath at 50-65 ℃, adding the ammonium molybdate aqueous solution, keeping the temperature and stirring for 10-20 minutes, dropwise adding the 0.8-1mol/l sodium hydroxide solution, raising the temperature of the water bath to 85-90 ℃ after dropwise adding, keeping the temperature and stirring for 30-40 minutes, discharging and cooling to obtain the saponification solution.
4. A sol friction reducing lubricating oil obtainable by the process for the preparation of a sol friction reducing lubricating oil according to any one of claims 1 to 3.
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| JPS5224193B2 (en) * | 1972-03-21 | 1977-06-29 | ||
| US4284518A (en) * | 1978-06-12 | 1981-08-18 | Michael Ebert | Stabilized hybrid lubricant |
| JPH01278599A (en) * | 1988-05-02 | 1989-11-08 | Nippon Mektron Ltd | Production of electroviscous fluid |
| US8680030B2 (en) * | 2005-11-18 | 2014-03-25 | Exxonmobil Research And Engineering Company | Enhanced deposit control for lubricating oils used under sustained high load conditions employing glycerine derivative with a grafted hindered phenolic and/or a hindered phenolic containing a thioether group |
| CN105289659B (en) * | 2015-09-29 | 2018-01-16 | 合肥学院 | A kind of SiO2‑MoS2Composite mesoporous nano material and its preparation method and application |
| CN106350175A (en) * | 2016-08-29 | 2017-01-25 | 四川正梁机械有限公司 | Lubricant for automobile chassis stampings and a preparing method thereof |
| CN107267254A (en) * | 2017-05-16 | 2017-10-20 | 蚌埠市宏大制药机械有限公司 | A kind of antiwear additive for universal machinery lubricating oil in pharmaceutical industry |
| CN107090004B (en) * | 2017-05-31 | 2019-03-01 | 张卫东 | A kind of organic molybdenum lube oil fat additives and preparation method thereof |
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