CN115074170A - Preparation method of lubricating grease, lubricating grease and automobile - Google Patents

Preparation method of lubricating grease, lubricating grease and automobile Download PDF

Info

Publication number
CN115074170A
CN115074170A CN202110280055.2A CN202110280055A CN115074170A CN 115074170 A CN115074170 A CN 115074170A CN 202110280055 A CN202110280055 A CN 202110280055A CN 115074170 A CN115074170 A CN 115074170A
Authority
CN
China
Prior art keywords
grease
base oil
thickener
lubricating grease
intermediate product
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN202110280055.2A
Other languages
Chinese (zh)
Inventor
克里斯托夫·施密茨
周喆翔
安-卡特琳·劳赫
马克西米利安·艾哈德
M·施密德-阿梅伦克森
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Klueber Lubrication Shanghai Co Ltd
Original Assignee
Klueber Lubrication Shanghai Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Klueber Lubrication Shanghai Co Ltd filed Critical Klueber Lubrication Shanghai Co Ltd
Priority to CN202110280055.2A priority Critical patent/CN115074170A/en
Publication of CN115074170A publication Critical patent/CN115074170A/en
Pending legal-status Critical Current

Links

Classifications

    • 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
    • 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
    • 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
    • C10M2201/1056—Silica 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
    • C10M2205/00—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions
    • C10M2205/02—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions containing acyclic monomers
    • C10M2205/0206—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions containing acyclic monomers used as base material
    • 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
    • C10M2207/127—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 polycarboxylic
    • 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
    • C10M2207/127—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 polycarboxylic
    • C10M2207/1276—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 polycarboxylic 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
    • C10M2213/00—Organic macromolecular compounds containing halogen as ingredients in lubricant compositions
    • C10M2213/06—Perfluoro polymers
    • C10M2213/062—Polytetrafluoroethylene [PTFE]
    • C10M2213/0626—Polytetrafluoroethylene [PTFE] 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
    • C10M2215/00—Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
    • C10M2215/02—Amines, e.g. polyalkylene polyamines; Quaternary amines
    • C10M2215/06—Amines, e.g. polyalkylene polyamines; Quaternary amines having amino groups bound to carbon atoms of six-membered aromatic rings
    • C10M2215/064—Di- and triaryl amines
    • 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
    • C10M2219/00—Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions
    • C10M2219/04—Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions containing sulfur-to-oxygen bonds, i.e. sulfones, sulfoxides
    • C10M2219/044—Sulfonic acids, Derivatives thereof, e.g. neutral salts

Landscapes

  • 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 embodiment of the invention relates to a preparation method of lubricating grease, the lubricating grease prepared by the method and an automobile comprising the lubricating grease. A preparation method of lubricating grease comprises the following steps: performing a saponification reaction in a first base oil comprising one or more polyalphaolefins to obtain a first intermediate product comprising a first thickener; dehydrating the first intermediate product at the dehydration temperature range of 70-120 ℃ and under the negative pressure environment to obtain a second intermediate product; and mixing the second intermediate product with a second base oil, and, optionally, additives, to obtain the grease, the second base oil comprising one or more of polyalphaolefins. The embodiment of the invention can be beneficial to reducing the odor of the lubricating grease, reducing the risk of air pollution in the space such as the interior of an automobile and the like while meeting other performance indexes of the lubricating grease at lower cost.

Description

Preparation method of lubricating grease, lubricating grease and automobile
Technical Field
The invention relates to the technical field of lubrication, in particular to a preparation method of lubricating grease, the lubricating grease prepared by the method and an automobile comprising the lubricating grease.
Background
In recent years, the rapid development of social economy has led to the progress of the automobile industry and improved the life of people. With the improvement of the consumption capability, when a consumer selects and purchases the automobile, the smell in the automobile also becomes one of important sensory indexes for evaluating the comfort of the automobile for the consumer.
However, as one of the indispensable components of the automobile interior, the conventional grease often has a certain odor, which may cause air pollution in the automobile and degrade the sensory experience of the customer. Even some greases may be slightly less odorous, but are expensive.
Accordingly, there is a need to improve existing grease manufacturing processes, greases, and automobiles that include greases.
Disclosure of Invention
The technical problems solved by the invention include that the existing preparation method of the lubricating grease, the lubricating grease and the automobile comprising the lubricating grease have a space for improving the odor of the lubricating grease.
One aspect of an embodiment of the present invention relates to a method for preparing grease, including: performing a saponification reaction in a first base oil comprising one or more polyalphaolefins to obtain a first intermediate product comprising a first thickener; dehydrating the first intermediate product at the dehydration temperature range of 70-120 ℃ and under the negative pressure environment to obtain a second intermediate product; and mixing the second intermediate product with a second base oil, and optionally additives, to obtain the grease, the second base oil comprising one or more of polyalphaolefins.
Optionally, the water removal temperature range includes 85 ℃ to 115 ℃, or 100 ℃ to 110 ℃.
Optionally, the pressure range of the negative pressure environment comprises-0.2 bar to-1 bar, -0.2bar to-0.7 bar, or-0.2 bar to-0.3 bar.
Optionally, the polyalphaolefin has a viscosity at 40 ℃ in the range comprising 65mm 2 /s～3000mm 2 /s。
Optionally, the grease is prepared at a temperature in the range of up to 70 ℃ to 120 ℃, 85 ℃ to 115 ℃, or 100 ℃ to 110 ℃.
Another aspect of embodiments of the present invention relates to a grease prepared by the above-described method of preparing a grease.
Optionally, the range of the sum of the mass percentages of the first base oil and the second base oil relative to the grease comprises 55% wt to 90% wt.
Optionally, the range of mass percent of the first thickener relative to the grease comprises 5% wt to 30% wt.
Optionally, the first thickener comprises the reaction product of lithium hydroxide and one or more organic acids.
Optionally, the grease is characterized by comprising a second thickener, the second thickener comprising at least one of silica and polytetrafluoroethylene.
Optionally, the range of the sum of the mass percentages of the first thickener and the second thickener relative to the grease comprises 5% wt to 30% wt.
Optionally, the mass percentage range of the additive relative to the lubricating grease comprises 0-15% wt.
Optionally, the additive comprises one or more of a rust inhibitor, an antiwear agent, an antioxidant.
Optionally, the rust inhibitor comprises one or more of a carboxylate, a sulfonate, a carboxylate amine salt, an alkyl amine salt.
Optionally, the antioxidant comprises one or more of an organic aminic antioxidant or a phenolic antioxidant.
Yet another aspect of an embodiment of the present invention relates to an automobile comprising the grease as described above.
The technical scheme of the embodiment of the invention can be beneficial to reducing the odor of the lubricating grease, reducing the risk of air pollution in the space such as the interior of an automobile and the like while meeting other performance indexes of the lubricating grease at lower cost.
The following further describes embodiments of the present invention.
Detailed Description
One aspect of an embodiment of the present invention relates to a method for preparing grease, including: performing a saponification reaction in a first base oil comprising one or more polyalphaolefins to obtain a first intermediate product comprising a first thickener; dehydrating the first intermediate product at the dehydration temperature range of 70-120 ℃ and under the negative pressure environment to obtain a second intermediate product; and mixing the second intermediate product with a second base oil, and optionally additives, to obtain the grease, the second base oil comprising one or more of polyalphaolefins.
The embodiment of the invention can be beneficial to reducing the odor of the lubricating grease, reducing the risk of air pollution in the space such as the interior of an automobile and the like while meeting other performance indexes of the lubricating grease at lower cost.
The preparation method of the lubricating grease provided by the embodiment of the invention has the advantages of low cost of raw materials, short preparation time, low required highest temperature and low cost, and can be helpful for obtaining the lubricating grease with low price and reducing the cost of the lubricating grease.
In the embodiments of the present invention, unless otherwise specifically noted, the grease may function as lubrication, auxiliary cooling, rust prevention, cleaning, sealing, buffering, and the like. Grease may be applied between two objects that move relative to each other to reduce friction and wear of the two objects due to contact. Grease may be used on various types of machinery to protect machinery and work pieces.
In the embodiments of the present invention, unless otherwise specifically indicated, numerical values may include errors such as a metering error, an accuracy error, a measurement error, and the like, for example, an error within a range of plus or minus 5%. For example, 70 may comprise a number in the range of 70 × (1 ± 5%), i.e. a number in the interval 66.5 to 73.5.
In the present examples, unless otherwise specifically indicated, numerical ranges may include any subrange therein, e.g., 70 ℃ to 120 ℃ may include 71 ℃ to 119 ℃, 85 ℃ to 115 ℃, 100 ℃ to 110 ℃, and so forth.
The water removal temperature range may be a range at which the temperature at which water removal is performed on the first intermediate product is performed. Optionally, the water removal temperature range includes 85 ℃ to 115 ℃, or 100 ℃ to 110 ℃. In this way, it is possible to facilitate the removal of water from the first intermediate product at a lower temperature with respect to the prior art.
The pressure of the sub-atmospheric environment may be a sub-atmospheric pressure at which the first intermediate product is subjected to water removal. Optionally, the pressure range of the negative pressure environment comprises-0.2 bar to-1 bar, -0.2bar to-0.7 bar, or-0.2 bar to-0.3 bar. In this way, the grease can be facilitated to be prepared in a shorter time.
The viscosity of the polyalphaolefin can be within a range that meets the application requirements. Optionally, the polyalphaolefin has a viscosity at 40 ℃ in the range comprising 65mm 2 /s～3000mm 2 And s. Thus, the grease can have better high-temperature performance and low-temperature performance.
The preparation method may facilitate the preparation of the grease at lower maximum temperatures. The maximum temperature may be the highest value of the temperatures involved in all steps of the preparation process. Optionally, the grease is prepared at a temperature in the range of up to 70 ℃ to 120 ℃, 85 ℃ to 115 ℃, or 100 ℃ to 110 ℃. As such, the grease can be advantageously prepared at lower temperatures.
Another aspect of embodiments of the present invention relates to a grease prepared by the above-described method of preparing a grease.
The embodiment of the invention can be beneficial to reducing the odor of the lubricating grease, reducing the risk of air pollution in the space such as the interior of an automobile and the like while meeting other performance indexes of the lubricating grease at lower cost.
The preparation method of the lubricating grease provided by the embodiment of the invention has the advantages of low cost of raw materials, short preparation time, low required highest temperature and low cost, and can be helpful for obtaining the lubricating grease with low price and reducing the cost of the lubricating grease.
The first base oil and the second base oil may be the same or different. The mass percentages of the first base oil and the second base oil with respect to the grease may be the same or different. Optionally, the range of the sum of the mass percentages of the first base oil and the second base oil relative to the grease comprises 55% wt to 90% wt. In this manner, it is possible to contribute to ensuring the lubricating performance of the grease.
Optionally, the range of mass percent of the first thickener relative to the grease comprises 5% wt to 30% wt. Thus, it is possible to contribute to ensuring the thickening property of the grease.
Optionally, the first thickener comprises the reaction product of lithium hydroxide and one or more organic acids. In this manner, it is possible to help ensure the thickening performance of the grease. The lithium hydroxide may include lithium hydroxide monohydrate. The lithium hydroxide may be contacted with one or more organic acids in the form of an aqueous solution of lithium hydroxide monohydrate to effect the reaction.
Optionally, the grease includes a second thickener including at least one of silica and polytetrafluoroethylene. The second thickener may be advantageous to ensure the consistency of the grease. The polytetrafluoroethylene can also improve the anti-wear properties of the grease.
Optionally, the range of the sum of the mass percentages of the first thickener and the second thickener relative to the grease comprises 5% wt to 30% wt. In this way, the viscosity-related properties of the grease may be facilitated. The first thickener and the second thickener may be the same or different in mass percentage from each other with respect to the grease.
The additive can be helpful for further improving the performance of the lubricating grease according to different needs. Optionally, the mass percentage range of the additive relative to the lubricating grease comprises 0-15% wt.
Optionally, the additive comprises one or more of a rust inhibitor, an antiwear agent, an antioxidant. As such, the additives may be beneficial in improving one or more of the performance of the grease in rust prevention, antiwear, antioxidant properties. The antiwear agent can prevent the abrasion, scratch and even sintering of the metal surface under the condition that the metal surface bears load. The antiwear agent can generally form a protective film with a metal surface under local high-temperature and high-pressure conditions.
Optionally, the rust inhibitor comprises one or more of a carboxylate, a sulfonate, a carboxylate amine salt, an alkyl amine salt. The rust inhibitor can help to improve the performance of the grease in terms of rust prevention. The antirust agent can form a firm adsorption film on the metal surface, isolate the metal surface from contacting with water or oxygen in the air, and destroy the conditions of electrochemical reaction, thereby preventing the generation of corrosion.
Optionally, the antioxidant comprises one or more of an organic aminic antioxidant or a phenolic antioxidant. The antioxidant can be beneficial to improving the performance of the lubricating grease in oxidation resistance. The antioxidant can delay the oxidation of the base oil during storage and use, thereby prolonging the service life of the lubricating grease.
Yet another aspect of an embodiment of the present invention relates to an automobile comprising the grease as described above. The vehicle may include a seat mount track, gear shift lever, or other vehicle interior trim, which may include grease as described above.
The embodiment of the invention can be beneficial to reducing the smell of the lubricating grease, reducing the risk of air pollution in the space such as the interior of an automobile and the like while meeting other performance indexes of the lubricating grease at lower cost.
The preparation method of the lubricating grease provided by the embodiment of the invention has the advantages of low raw material cost, short preparation time, low required highest temperature and low cost, and can be beneficial to obtaining the lubricating grease with low price, reducing the cost of the lubricating grease, and further correspondingly reducing the cost of automobiles comprising the lubricating grease, and the like.
The following examples may be used to aid in the understanding of embodiments of the present invention and are not intended to be limiting of the claims.
Examples of the invention
Examples 1 to 4 and comparative examples 1 to 4 described below are each a production process of several batches, and the mass of raw materials of different batches may be different, but the mass percentage (% wt) of each raw material is the same, and specific values of the mass percentage are listed in each example, and the temperature, the pressure and the time are regulated within certain ranges according to actual conditions, and are listed in a numerical range manner accordingly. Unless otherwise specifically indicated, the mass percent of each raw material refers to the percentage of the mass of the raw material relative to the total mass of all raw materials in the example.
Example 1
Polyalphaolefin (PAO)1300/40 (first base oil, 40 ℃ viscosity: 1300 mm) in the autoclave 2 /s, 20% wt) is heated to 90-95 ℃. Dodecahydroxystearic acid (organic acid, 14.38 wt%) was dissolved in PAO 1300/40 and stirred well. Slowly adding 2.12 wt% of lithium hydroxide monohydrate aqueous solution at 90-95 ℃, stirring at constant temperature for about 30 minutes, and performing saponification reaction to obtain a first intermediate product comprising a first thickening agent.
Closing an air vent valve of the reaction kettle, slowly pumping air to reduce the pressure in the kettle to-0.2 bar to-0.3 bar approximately, stirring for about 1-2 hours at 100-105 ℃, and removing water from the first intermediate product. Meanwhile, a sample is sampled to detect the water content (the mass percentage of water in the sample relative to the total mass of the sample) so as to observe the water vapor condition in the reaction kettle, and after the water content reaches 0.02 wt%, a second intermediate product is obtained.
P-dioctyldiphenylamine (antioxidant, 2% wt), PAO400/40 (second base oil, viscosity at 40 ℃ C.: 400 mm) were added to the second intermediate 2 60% wt)/s), cooling to below 60 deg.C, adding calcium sulfonate (antirust agent, 1.5% wt), stirring, and mixing to obtain the grease.
Assuming that the water is completely removed, calculating the percentages of the mass of the base oils (first and second base oils), first thickener, additives (antioxidant and rust inhibitor) relative to the total mass of the grease, one can obtain: 81.4% wt base oil, 15% wt first thickener and 3.6% wt additives.
The preparation time is 6-7 hours in total, and the maximum temperature is 105 ℃ in the process.
Example 2
PAO 1300/40 (first base oil, viscosity at 40 ℃ C.: 1300 mm) in the autoclave was added 2 25% wt) is heated to 100-110 ℃,two organic acids, 6.1 wt% of dodecahydroxystearic acid and 3.1 wt% of azelaic acid, are dissolved in PAO 1300/40 and stirred uniformly. Slowly adding 2.3 wt% of aqueous solution of lithium hydroxide monohydrate at the temperature of 105-110 ℃, stirring for about 30 minutes at constant temperature, and performing saponification reaction to obtain a first reaction product.
Closing an air vent valve of the reaction kettle, slowly pumping air to reduce the pressure in the kettle to-0.2 bar to-0.3 bar approximately, stirring at 105-110 ℃ for about 1-2 hours, and removing water. Sampling and detecting the water content of the sample, observing the water vapor condition in the kettle, and obtaining a second intermediate product after the water content reaches 0.03 wt%.
2% by weight of p-dioctyldiphenylamine (antioxidant), 60% by weight of PAO400/40 (second base oil, viscosity at 40 ℃ C.: 400 mm) were added to the second intermediate product 2 And/s), reducing the temperature to below 60 ℃, adding 1.5 wt% of sodium sebacate (antirust agent), uniformly stirring, and mixing to obtain the lubricating grease.
Assuming that the water is completely removed, calculating the percentages of the mass of the base oil (first base oil and second base oil), the first thickener, the additives (antioxidant and rust inhibitor) relative to the total mass of the grease, one can obtain: 86.7 wt% of base oil, 9.7 wt% of first thickening agent and 3.6 wt% of additive.
The preparation time is 6-7 hours in total, and the maximum temperature is 110 ℃ in the process.
Example 3
In a reaction vessel, PAO 10 (first base oil, viscosity at 40 ℃ C.: 65 mm) 2 24.5 wt%) is heated to 90-95 deg.C, stearic acid (organic acid, 8.5 wt%) is dissolved in PAO 10, and stirred uniformly. Slowly adding 1.5 wt% of lithium hydroxide monohydrate aqueous solution at 90-95 ℃, stirring at constant temperature for about 30 minutes, and performing saponification reaction to obtain a first intermediate product.
Closing the vent valve of the reaction kettle, slowly exhausting air to reduce the pressure in the kettle to-0.7 bar approximately, stirring for about 30 minutes to 1 hour at 70-100 ℃ (the pressure is lower, the boiling point of water is reduced, the temperature in the reaction kettle is reduced to about 70 ℃ along with the evaporation of water, and the temperature gradually rises to 100 ℃ along with the volatilization of water vapor, and removing water. Sampling and detecting the water content of the sample, observing the water vapor condition in the kettle, and obtaining a second intermediate product after the water content reaches 0.02 percent by weight.
2% by weight of 2, 6-di-tert-butylphenol (antioxidant), 58% by weight of PAO400/40 (second base oil, viscosity at 40 ℃ C.: 400 mm) were added to the second intermediate product 2 S), reducing the temperature to below 60 ℃, adding 1.5 wt% of sodium sebacate (antirust agent) and 4 wt% of PTFE (second thickening agent with anti-wear and thickening effects), uniformly stirring, and mixing to obtain the lubricating grease.
Calculating the percentages of the mass of the base oils (first base oil and second base oil), thickeners (first thickener and second thickener), additives (antioxidant and rust inhibitor) relative to the total mass of the grease, assuming that the water is completely removed, can give: 83.6 wt% of base oil, 12.9 wt% of thickening agent and 3.5 wt% of additive.
This example uses a lower negative pressure, increasing the rate of water removal, and the preparation time amounts to 5-6 hours, during which the maximum temperature is 100 ℃.
Example 4
In a reaction vessel, PAO 1300/40 (first base oil, viscosity at 40 ℃ C.: 1300 mm) 2 22.6 percent by weight) is heated to 100-110 ℃, two organic acids of 6.1 percent by weight of dodecahydroxystearic acid and 3.2 percent by weight of azelaic acid are melted in the mixture and stirred evenly. Slowly adding 2.1 wt% of lithium hydroxide monohydrate aqueous solution at 105-110 ℃, stirring at constant temperature for about 30 minutes, and performing saponification reaction to obtain a first intermediate product.
Closing the vent valve of the reaction kettle, slowly pumping air to reduce the pressure in the kettle to-0.7 bar approximately, and stirring at 105-110 ℃ for about 30 minutes-1 hour to remove water. Sampling and detecting the water content of the sample, observing the water vapor condition in the kettle, and obtaining a second intermediate product after the water content reaches 0.02 percent by weight.
To the second intermediate product was added 1% by weight of p-dioctyldiphenylamine (antioxidant), 60% by weight of PAO400/40 (second base oil, viscosity at 40 ℃ C.: 400 mm) 2 And/s), reducing the temperature to below 60 ℃, adding 1 wt% of sodium sebacate (antirust agent) and 4 wt% of silicon dioxide powder (second thickening agent), uniformly stirring, and mixing to obtain the lubricating grease.
Calculating the percentages of the mass of the base oils (first base oil and second base oil), thickeners (first thickener and second thickener), additives (antioxidant and rust inhibitor) relative to the total mass of the grease, assuming that the water is completely removed, can give: 84.1 wt% of base oil, 13.9 wt% of thickening agent and 2 wt% of additive.
The preparation time is 6-7 hours in total, and the maximum temperature is 110 ℃ in the process.
Comparative example 1
Heating 20 wt% of PAO 1300/40 to 90-95 ℃ in a reaction kettle, dissolving 15 wt% of dodecahydroxystearic acid in PAO 1300/40, and uniformly stirring. An aqueous solution of 2.2% by weight of lithium hydroxide monohydrate was slowly added thereto at 90 to 95 ℃ and stirred at a constant temperature for about 30 minutes to carry out saponification.
And then, heating to 135-150 ℃ at normal pressure, stirring for about 1-2 hours, removing water, and sampling and detecting until the water content of the sample reaches 0.01 wt%.
And continuously heating to 205-220 ℃ to melt the soap base, and adding 59.3 wt% of PAO400/40 when the soap base in the kettle is completely melted. Rapidly cooling to 180 ℃, stirring for 1 hour at constant temperature, continuously cooling to 105-120 ℃, adding 2 wt% of p-dioctyl diphenylamine, cooling to below 60 ℃, adding 1.5 wt% of calcium sulfonate, stirring uniformly, and mixing to obtain the lubricating grease.
Calculating the percentage of the mass of base oil, thickener, additives relative to the total mass of the grease, assuming that the water is completely removed, gives: 80.8 wt% of base oil, 15.6 wt% of thickening agent and 3.6 wt% of additive.
The preparation time is 7-8 hours in total, and the maximum temperature is 220 ℃ during the preparation.
Comparative example 2
Heating 25 wt% of PAO 1300/40 to 100-110 ℃ in a reaction kettle, melting 6.1 wt% of dodecahydroxystearic acid and 3 wt% of azelaic acid in PAO 1300/40, and uniformly stirring. An aqueous solution of 2.3% by weight of lithium hydroxide monohydrate was slowly added thereto at 105 to 110 ℃ and stirred at a constant temperature for about 30 minutes to conduct saponification.
Closing an air vent valve of the reaction kettle, slowly pumping air to reduce the pressure in the kettle to-0.2 bar to-0.3 bar approximately, continuously heating to 130-150 ℃, and stirring for about 1-2 hours to remove water until the water content of the sample reaches 0.02 wt%.
Adding 60.1 wt% of PAO400/40, cooling to 105-120 ℃, stirring at constant temperature for 1 hour, adding 2 wt% of p-dioctyl diphenylamine, cooling to below 60 ℃, adding 1.5 wt% of sodium sebacate, stirring uniformly, and mixing to obtain the lubricating grease.
Assuming that the water is completely removed, calculating the percentage of the mass of base oil, thickener, additives with respect to the total mass of the grease, one can obtain: 86.7 wt% of base oil, 9.7 wt% of thickening agent and 3.6 wt% of additive.
The preparation time is 5-6 hours in total, and the maximum temperature is 150 ℃ in the preparation process.
Comparative example 3
Heating 24.5 wt% of mineral oil (viscosity at 40 ℃ is 110) in a reaction kettle to 90-95 ℃, dissolving 10 wt% of dodecahydroxystearic acid in the mineral oil, and uniformly stirring. An aqueous solution of 1.8% by weight of lithium hydroxide monohydrate was slowly added between 90 ℃ and 95 ℃ and stirred at a constant temperature for about 30 minutes to carry out saponification.
Closing the vent valve of the reaction kettle, slowly pumping air to reduce the pressure in the kettle to-0.7 bar approximately, and stirring at 100-105 ℃ for about 30 minutes to 1 hour to remove water. Samples were taken to check the water content of the samples until 0.02% wt was reached.
2 wt% of 2, 6-di-tert-butylphenol and 56.2 wt% of mineral oil are added, the temperature is reduced to below 60 ℃, and 1.5 wt% of sodium sebacate and 4 wt% of PTFE are added. Stirring evenly and mixing to obtain the lubricating grease.
Calculating the percentage of the mass of base oil, thickener, additives relative to the total mass of the grease, assuming that the water is completely removed, gives: 82 wt% of base oil, 14.5 wt% of thickening agent and 3.5 wt% of additive.
The preparation time is 6-7 hours in total, and the maximum temperature is 105 ℃ in the process.
Comparative example 4
Heating 25% of wtPAO 1300/40 to 100-110 ℃ in a reaction kettle, melting 6.1 wt% of dodecahydroxystearic acid and 3.1 wt% of azelaic acid in the reaction kettle, and uniformly stirring. An aqueous solution of 2.3% by weight of lithium hydroxide was slowly added between 105 ℃ and 110 ℃ to conduct saponification.
Stirring at 105-110 deg.C for 4-5 hr under normal pressure to remove water. Samples were taken to check the water content of the samples until 0.02% wt was reached.
Adding 2 wt% of p-dioctyl diphenylamine and 60 wt% of PAO400/40, reducing the temperature to below 60 ℃, adding 1.5 wt% of sodium sebacate, uniformly stirring, and mixing to obtain the lubricating grease.
Calculating the percentage of the mass of base oil, thickener, additives relative to the total mass of the grease, assuming that the water is completely removed, gives: 86.7 wt% of base oil, 9.7 wt% of thickening agent and 3.6 wt% of additive.
The comparative example does not adopt negative pressure, but reduces the water removal temperature to 105-110 ℃, the preparation time is 10-12 hours in total, and the maximum temperature is 110 ℃.
The base oils, water removal temperature, water removal pressure, preparation time, maximum temperature of examples 1 to 4 and comparative examples 1 to 4 are listed in table 1 below. The grease samples prepared in examples 1 to 4 and comparative examples 1 to 4 were subjected to performance tests, and the results are shown in Table 1 below, with the relevant descriptions being set forth in Table 1 below.
TABLE 1
Figure BDA0002978438730000101
Figure BDA0002978438730000111
1) The working cone penetration value measured according to DIN ISO 2137 represents the hardness degree of the grease, the working cone penetration value from small to large sequentially represents the hard to soft property of the grease, and the larger the value, the softer the grease. The working penetration data for the grease samples in table 1 are acceptable.
2) The corrosion values of copper sheets determined in accordance with DIN 51811 represent the effect of the grease on the copper sheets, the smaller the values, the smaller the effect, the better the corrosion resistance. The copper sheet corrosion test conditions for the grease samples in table 1 include: the data at 100 ℃ and 24h all meet the requirements of automobile application.
3) The EMCOR corrosion data measured according to DIN 51802 characterise the degree of corrosion of the grease on the bearing steel ring, with smaller values representing less influence and better corrosion resistance. The EMCOR corrosion test conditions for the grease samples in Table 1 include: distilled water, 168h, the data all meet the requirements of automotive applications.
4) The flow pressure data measured at-40 ℃ according to DIN 51805 characterizes the flow ability of the grease at-40 ℃ in a low-temperature environment, and the smaller the pressure required, the better the flow of the grease and the better the low-temperature performance. The flow pressure data for the grease samples in table 1 are all within acceptable ranges for automotive applications.
5) The volatilization loss measured according to DIN 58397 is the mass percent volatilization loss of the grease under specific time and temperature conditions, and the smaller the volatilization loss value is, which represents that the smaller the volatilization amount of the base oil is, the smaller the property change after high temperature is, and the higher the temperature performance of the grease can be evaluated. The data testing conditions for the grease samples in table 1 include: the data are within acceptable ranges for automotive applications at 130 ℃ for 168 h.
6) The dropping point, measured according to DIN ISO 2176, refers to the temperature at which the grease changes phase from solid to liquid and is commonly used to evaluate the high temperature performance of greases. The drop point data for the grease samples in table 1 are all within acceptable ranges for automotive applications.
7) ASTM oil separation, measured according to ASTM D6184, characterizes the mass percent oil separated by a grease at a particular temperature, with the tendency for lower values to be better. The test conditions for the grease samples in table 1 included: the data are within acceptable ranges for automotive applications at 100 ℃ for 30 h.
8) DIN oil separation measured according to DIN 51817 characterizes the mass percentage of oil separated by the grease at a particular temperature, with the tendency to be better at lower values. The test conditions for the grease samples in table 1 include: the data are within the acceptable range for automotive applications at 40 ℃ for 168h, but the oil separation rate of comparative example 3 is 4.5% in comparison, which is in the higher category.
9) Static water resistance measured according to DIN 51807 characterizes the static water resistance of a grease at a particular temperature, with a smaller value representing better water resistance. The test conditions for the grease samples in table 1 include: the data are within acceptable ranges for automotive applications at 90 ℃ for 3 h.
10) The VKA four-ball joint measured according to DIN 51350part 4 characterizes the load-bearing properties of the grease, the experimental values representing the risk of cold welding of the parts beyond a maximum load corresponding to the grease. The data for the grease samples in table 1 are within acceptable limits for application in automotive interiors.
11) The VS-00.28-L-06021 and VDA270 data characterize the odor performance of greases, with smaller numbers giving smaller odors.
The VS-00.28-L-06021 odor test consists in placing a 20 cm square tinfoil coated with 5g of a grease sample in a volumetric flask with a volume of 1 litre, taking the average after placing for 2h at 65 ℃ giving the evaluation value by a rating of not less than 5 for the odor intensity of the interior of the car. According to the requirement of automobile manufacturers on the odor test, namely, the average value is less than or equal to 3, whether the automobile is qualified is judged, and the data can be seen by referring to the data in the table 1: the samples of examples 1-4 all passed, and the samples of comparative examples 1-4 all failed.
The VDA270 odor test comprises placing a tin foil coated with a 1g grease sample having a thickness of 20 mm in a volumetric flask having a volume of 1 liter, and taking an average value after giving evaluation values by not less than 5 ginseng after standing at 80 ℃ for 2 hours. According to the requirement of automobile manufacturers on the odor test, namely, the average value is less than or equal to 3, whether the automobile is qualified is judged, and the data can be seen by referring to the data in the table 1: the samples of examples 1-4 all passed, and the samples of comparative examples 1-4 all failed.
As can be seen from the above, the grease prepared by using polyalphaolefin as base oil and removing water at 70-120 ℃ in negative pressure environment in examples 1-4 can meet the standards of automobile manufacturers for testing the odor of automobile interiors while meeting other performance requirements of the grease. The cost of the grease was lower due to the lower cost of the raw materials used, the shorter preparation time, and the lower maximum temperature required for examples 1-4. However, in the comparative example, the grease prepared by changing at least one of the base oil, the water removal temperature and the water removal pressure does not meet the odor test standard required by the automobile manufacturer. Moreover, in comparative examples 1 to 4, some preparation time was long, some required high maximum temperature, and there was room for improvement in efficiency, temperature, and the like.
Although the present invention is disclosed above, the present invention is not limited thereto. Various changes and modifications may be effected therein by one skilled in the art without departing from the spirit and scope of the invention as defined in the appended claims.

Claims (16)

1. A method for preparing lubricating grease is characterized by comprising the following steps:
performing a saponification reaction in a first base oil comprising one or more polyalphaolefins to obtain a first intermediate product comprising a first thickener;
dehydrating the first intermediate product in a dehydration temperature range of 70-120 ℃ and a negative pressure environment to obtain a second intermediate product; and
mixing the second intermediate product with a second base oil, and optionally additives, to obtain the grease, the second base oil comprising one or more of polyalphaolefins.
2. The method of claim 1, wherein the water removal temperature range comprises 85 ℃ to 115 ℃, or 100 ℃ to 110 ℃.
3. The method of claim 1, wherein the pressure of the negative pressure environment ranges from-0.2 bar to-1 bar, -0.2bar to-0.7 bar, or-0.2 bar to-0.3 bar.
4. The method of preparing a grease of claim 1 wherein the polyalphaolefin has a viscosity at 40 ℃ in the range including 65mm 2 /s～3000mm 2 /s。
5. A method of preparing a grease according to claim 1 wherein the grease is prepared at a temperature in the range of up to 70 ℃ to 120 ℃, 85 ℃ to 115 ℃, or 100 ℃ to 110 ℃.
6. A grease prepared by the method of preparing a grease according to any one of claims 1 to 5.
7. The grease of claim 6, wherein the range of the sum of the mass percentages of the first base oil and the second base oil relative to the grease comprises 55% wt to 90% wt.
8. The grease of claim 6, wherein the range of mass percent of the first thickener relative to the grease comprises 5% wt to 30% wt.
9. The grease of claim 6, wherein the first thickener comprises a reaction product of lithium hydroxide and one or more organic acids.
10. The grease of claim 9, comprising a second thickener comprising at least one of silica and polytetrafluoroethylene.
11. The grease of claim 10, wherein the range of the sum of the mass percentages of the first thickener and the second thickener relative to the grease comprises 5% wt to 30% wt.
12. The grease of claim 6, wherein the additive comprises 0 to 15% by weight of the grease.
13. The grease of claim 12, wherein the additives comprise one or more of rust inhibitors, anti-wear agents, antioxidants.
14. The grease of claim 13, wherein the rust inhibitor comprises one or more of a carboxylate, a sulfonate, a carboxylate amine salt, and an alkylamine salt.
15. The grease of claim 13, wherein the antioxidant comprises one or more of an organic aminic antioxidant or a phenolic antioxidant.
16. An automobile comprising a grease according to any one of claims 6-15.
CN202110280055.2A 2021-03-16 2021-03-16 Preparation method of lubricating grease, lubricating grease and automobile Pending CN115074170A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202110280055.2A CN115074170A (en) 2021-03-16 2021-03-16 Preparation method of lubricating grease, lubricating grease and automobile

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202110280055.2A CN115074170A (en) 2021-03-16 2021-03-16 Preparation method of lubricating grease, lubricating grease and automobile

Publications (1)

Publication Number Publication Date
CN115074170A true CN115074170A (en) 2022-09-20

Family

ID=83245511

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202110280055.2A Pending CN115074170A (en) 2021-03-16 2021-03-16 Preparation method of lubricating grease, lubricating grease and automobile

Country Status (1)

Country Link
CN (1) CN115074170A (en)

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109054934A (en) * 2018-07-23 2018-12-21 中国石油化工股份有限公司 A kind of composition and preparation method of low smell automobile seat electric sliding rail lubricating grease
CN110511806A (en) * 2019-07-10 2019-11-29 杭州新港润滑科技有限公司 A kind of high temperature water resistant urea-base grease and its preparation process
CN112375606A (en) * 2020-11-09 2021-02-19 武汉博达特种润滑技术有限公司 Low-odor automobile switch lubricating grease composition and preparation method thereof

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109054934A (en) * 2018-07-23 2018-12-21 中国石油化工股份有限公司 A kind of composition and preparation method of low smell automobile seat electric sliding rail lubricating grease
CN110511806A (en) * 2019-07-10 2019-11-29 杭州新港润滑科技有限公司 A kind of high temperature water resistant urea-base grease and its preparation process
CN112375606A (en) * 2020-11-09 2021-02-19 武汉博达特种润滑技术有限公司 Low-odor automobile switch lubricating grease composition and preparation method thereof

Similar Documents

Publication Publication Date Title
EP1764407B1 (en) Use of lubricant compositions for lubrication of bearings
JP5249584B2 (en) Lubricating composition
KR101841083B1 (en) Aqueous lubricant composition for plastic working on metal material
JP4048758B2 (en) Lubricating grease composition
EP3746529B1 (en) Lubricant composition
CN114350431B (en) Multifunctional lubricating grease, and preparation method and application thereof
CN115074170A (en) Preparation method of lubricating grease, lubricating grease and automobile
CN107312590B (en) Leveling anti-rust oil for cold-rolled steel sheets and preparation method thereof
CN104893807A (en) Lubricating grease for guide rail lead screw mechanism of dust-free room
CN111471029B (en) Liquid multi-effect lubricating oil oiliness agent and preparation method thereof
KR102509151B1 (en) Grease composition, method for producing the grease composition, and method for using the grease composition
CN111205909B (en) Composite lithium-based lubricating grease and preparation method thereof
US20140336090A1 (en) Grease composition and bearing
EP3060635B1 (en) Use of calcium salicylate to improve roll stability in a grease composition
CN109563432A (en) Lubricant composition
CN101205499B (en) Aluminum-magnesium alloy wiredrawing lubricant
JP4829549B2 (en) Lubricating oil for plastic working
JP2009209239A (en) Lubricant oil composition for plastic working
CN104479832A (en) Automobile assembly line conveyor belt special-purpose grease and preparation method
CN106497648B (en) Molding oil and preparation method thereof
CN107916161A (en) A kind of ceramic polishing machine drive bearing lubricating oil/fat composition
CN117467494B (en) Special engine oil for long-life energy-saving screw air compressor and preparation method
Rogoś The non-normative tests of the operational suitability of biodegradable hydraulic oils
CN106701267A (en) Lubricating oil and preparation method thereof
JP2023026889A (en) grease composition

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination