CN107937088B - Lubricating grease and preparation method thereof - Google Patents

Lubricating grease and preparation method thereof Download PDF

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Publication number
CN107937088B
CN107937088B CN201711129520.2A CN201711129520A CN107937088B CN 107937088 B CN107937088 B CN 107937088B CN 201711129520 A CN201711129520 A CN 201711129520A CN 107937088 B CN107937088 B CN 107937088B
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grease
gallium
parts
liquid metal
stirring
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CN107937088A (en
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田煜
白鹏鹏
李少伟
陶大帅
贾文鹏
孟永钢
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Tsinghua University
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Tsinghua University
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    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M125/00Lubricating compositions characterised by the additive being an inorganic material
    • C10M125/04Metals; Alloys
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M169/00Lubricating 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
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M169/00Lubricating 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
    • C10M169/06Mixtures of thickeners and additives
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2201/00Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/04Elements
    • C10M2201/05Metals; Alloys
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2203/00Organic non-macromolecular hydrocarbon compounds and hydrocarbon fractions as ingredients in lubricant compositions
    • C10M2203/10Petroleum or coal fractions, e.g. tars, solvents, bitumen
    • C10M2203/1006Petroleum or coal fractions, e.g. tars, solvents, bitumen used as base material
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2207/00Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/10Carboxylix acids; Neutral salts thereof
    • C10M2207/12Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms
    • C10M2207/121Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of seven or less carbon atoms
    • C10M2207/123Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of seven or less carbon atoms polycarboxylic
    • C10M2207/1236Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of seven or less carbon atoms polycarboxylic used as thickening agent
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2207/00Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/10Carboxylix acids; Neutral salts thereof
    • C10M2207/12Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms
    • C10M2207/125Carboxylix 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
    • C10M2207/128Carboxylix 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
    • C10M2207/1285Carboxylix 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
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10NINDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2030/00Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
    • C10N2030/06Oiliness; Film-strength; Anti-wear; Resistance to extreme pressure
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10NINDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2050/00Form in which the lubricant is applied to the material being lubricated
    • C10N2050/10Semi-solids; greasy

Abstract

The invention provides lubricating grease and a preparation method thereof. The lubricating grease is non-toxic, non-irritant and non-corrosive, can achieve excellent extreme pressure performance equivalent to gallium-based liquid metal under a high load condition, can reduce the cost to less than one tenth of that of the gallium-based liquid metal, has obviously better abrasion resistance under a low load condition than the gallium-based liquid metal, and is suitable for various working conditions from low load to high load.

Description

Lubricating grease and preparation method thereof
Technical Field
The invention relates to the technical field of lubrication, in particular to lubricating grease and a preparation method thereof.
Background
At present, the extreme pressure agent of the grease is generally substances such as sulfur-containing compounds (such as sulfurized olefin, sulfurized lard, sulfurized oleic acid, polysulfide), phosphorus-containing compounds (such as phosphate, phosphite, phosphate) and nano materials, and the sulfur-containing compounds and the phosphorus-containing compounds have the defects of strong irritation and strong corrosivity when being used as the extreme pressure agent of the grease; in addition, the direct use of liquid metal as a lubricant is costly and has poor wear resistance under low load conditions.
Therefore, the related art of the existing grease is still to be improved.
Disclosure of Invention
The present invention is directed to solving, at least to some extent, one of the technical problems in the related art. Therefore, one objective of the present invention is to provide a non-toxic, non-irritant, non-corrosive grease which can achieve excellent extreme pressure performance equivalent to gallium-based liquid metal under high load condition, can reduce the cost to less than one tenth of gallium-based liquid metal, has abrasion resistance obviously superior to gallium-based liquid metal under low load condition, or is suitable for various working conditions from low load to high load.
In one aspect of the present invention, the present invention provides a grease. According to an embodiment of the present invention, the grease comprises a grease matrix and a gallium-based liquid metal. The inventor finds that the lubricating grease is non-toxic, non-irritant and non-corrosive, can achieve excellent extreme pressure performance equivalent to gallium-based liquid metal under the condition of high load, can reduce the cost to less than one tenth of the gallium-based liquid metal, has obviously better abrasion resistance under the condition of low load than the gallium-based liquid metal, and is suitable for various working conditions from low load to high load.
According to an embodiment of the present invention, the gallium-based liquid metal is present in an amount of 0.1 to 50% by mass, based on the total mass of the grease.
According to an embodiment of the invention, the gallium-based liquid metal is pure gallium or a mixture of gallium and at least one selected from indium, tin and zinc.
According to an embodiment of the present invention, the mixture of gallium and at least one selected from the group consisting of indium, tin and zinc contains one of the following: 28-95 parts of gallium and 5-72 parts of indium; 34-70 parts of gallium, 1-40 parts of indium and 1-26 parts of tin; 30-80 parts of gallium, 1-40 parts of indium, 1-30 parts of tin and 0.1-10 parts of zinc.
According to an embodiment of the invention, the grease matrix comprises: base oil and thickener.
According to an embodiment of the present invention, the base oil is one selected from 150BS base oil, 150SN base oil, 500SN base oil; the thickener comprises 12-hydroxystearic acid, sebacic acid and LiOH.
According to an embodiment of the present invention, the grease further comprises at least one of an antioxidant and an antiwear agent.
According to an embodiment of the invention, the grease matrix is a complex grease.
In another aspect of the invention, the invention provides a method of preparing a grease as described above. According to an embodiment of the invention, the method comprises mixing a gallium-based liquid metal and a grease base, and stirring and milling the resulting mixture. The inventor finds that the method is simple and convenient to operate, easy to realize and easy for industrial production, the lubricating grease prepared by the method is non-toxic, non-irritant and non-corrosive, the excellent extreme pressure performance equivalent to that of gallium-based liquid metal can be achieved under the condition of high load, the cost can be reduced to less than one tenth of that of the gallium-based liquid metal, the wear resistance under the condition of low load is obviously superior to that of the gallium-based liquid metal, and the method is suitable for various working conditions from low load to high load.
According to the embodiment of the invention, the stirring temperature is 50-130 ℃, the stirring time is 20-60 minutes, and the grinding time is 1-6 hours.
Detailed Description
The following describes embodiments of the present invention in detail. The following examples are illustrative only and are not to be construed as limiting the invention. The examples, where specific techniques or conditions are not indicated, are to be construed according to the techniques or conditions described in the literature in the art or according to the product specifications. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products commercially available.
In one aspect of the present invention, the present invention provides a grease. According to an embodiment of the present invention, the grease comprises a grease matrix and a gallium-based liquid metal. The inventor finds that the lubricating grease is non-toxic, non-irritant and non-corrosive, can achieve excellent extreme pressure performance equivalent to gallium-based liquid metal under the condition of high load, can reduce the cost to less than one tenth of the gallium-based liquid metal, has obviously better abrasion resistance under the condition of low load than the gallium-based liquid metal, and is suitable for various working conditions from low load to high load.
According to the embodiment of the present invention, the specific kind of the gallium-based liquid metal is not particularly limited, and may be flexibly selected by those skilled in the art as long as the requirement is satisfied, for example, including but not limited to pure gallium or a mixture of gallium and at least one selected from indium, tin and zinc. Thereby, the grease can be further made to have excellent extreme pressure properties.
According to the embodiment of the present invention, the ratio of each component in the mixture is not particularly limited, and one skilled in the art can flexibly select the mixture according to the requirement as long as the requirement is met. In some embodiments of the present invention, the mixture of gallium and at least one selected from the group consisting of indium, tin, and zinc contains 28 to 95 parts by weight of gallium and 5 to 72 parts by weight of indium. In other embodiments of the present invention, the mixture of gallium and at least one selected from the group consisting of indium, tin, and zinc contains 34 to 70 parts by weight of gallium, 1 to 40 parts by weight of indium, and 1 to 26 parts by weight of tin. In still other embodiments of the present invention, the mixture of gallium and at least one selected from the group consisting of indium, tin, and zinc contains 30 to 80 parts by weight of gallium, 1 to 40 parts by weight of indium, 1 to 30 parts by weight of tin, and 0.1 to 10 parts by weight of zinc. Therefore, the lubricating grease has excellent extreme pressure performance under high load conditions, good abrasion resistance under low load conditions and lower melting point.
According to embodiments of the present invention, the specific kind of the grease base is not particularly limited, and may be flexibly selected by those skilled in the art as needed as long as the requirements are satisfied, and may include, but is not limited to, a base grease or a complex grease, for example. In some embodiments of the present invention, the grease matrix is a complex grease, the specific type of which is not particularly limited and may be any known commercially available complex grease, including, for example, but not limited to, the KLUBER ISOFLEX LDS 18 SPECIAL A complex grease. Therefore, the lubricating grease has excellent extreme pressure performance, and meanwhile, as the compound lubricating grease already contains the antioxidant and the antiwear agent, the lubricating grease has excellent oxidation stability and abrasion resistance.
In other embodiments of the present invention, the grease matrix is a base grease comprising a base oil and a thickener. According to the embodiment of the present invention, the specific kind of the base oil is not particularly limited, and one skilled in the art may flexibly select according to the need as long as the requirement is satisfied, for example, including but not limited to 150BS base oil, 150SN base oil, 500SN base oil, and the like. In some embodiments of the invention, the base oil may be a 150BS base oil. Therefore, after the lubricating grease is compounded with gallium-based liquid metal, the extreme pressure performance of the lubricating grease can be greatly improved, and the lubricating grease has high viscosity, high flash point and good compound sensitivity with an antioxidant and an antiwear agent.
According to the embodiment of the present invention, the specific kind of the thickener is not particularly limited, and one skilled in the art can flexibly select the thickener according to the requirement as long as the requirement is satisfied, for example, the thickener includes, but is not limited to, soap-based thickener, non-soap-based thickener, hydrocarbon-based thickener, etc. In some embodiments of the invention, the specific type of thickener may be a soap-based thickener. Therefore, the grease is more easily industrially produced and is suitable for various greases.
According to the embodiment of the present invention, the specific kind of the soap-based thickener is not particularly limited, and one skilled in the art can flexibly select the soap-based thickener according to the requirement, such as but not limited to a complex lithium-based thickener, a complex calcium sulfonate thickener, a complex titanium thickener, etc. In some embodiments of the present invention, the specific type of soap-based thickener may be a complex lithium-based thickener. Therefore, the lubricating grease has higher use temperature, good colloid stability and oxidation stability, excellent waterproofness and corrosion resistance, no toxicity and no pollution to the environment.
According to the embodiment of the present invention, the specific kind of the complex lithium-based thickener is not particularly limited, and one skilled in the art can flexibly select the complex lithium-based thickener according to the requirement, such as but not limited to a complex lithium-based thickener of 12-hydroxystearic acid and fatty dibasic acid, or a complex lithium-based thickener of 12-hydroxystearic acid and inorganic acid, etc. In some embodiments of the present invention, the complex lithium-based thickener includes 12-hydroxystearic acid, sebacic acid, and LiOH. Therefore, the lubricating grease has the advantages of high use temperature, excellent colloid stability and oxidation stability, excellent waterproofness and corrosion resistance, no toxicity and no pollution to the environment.
According to the embodiment of the present invention, the grease further comprises an antioxidant, and the specific kind of the antioxidant is not particularly limited, and one skilled in the art can flexibly select the antioxidant according to the requirement, such as but not limited to phenolic antioxidants, or amine antioxidants, etc. In some embodiments of the invention, a particular class of the antioxidant may be a phenolic antioxidant. Therefore, the grease can have more excellent oxidation stability.
According to the embodiment of the present invention, the specific kind of the phenolic antioxidant is not particularly limited, and may be flexibly selected by those skilled in the art as needed as long as the requirement is satisfied, for example, including but not limited to 2, 6-di-tert-butyl-p-cresol, 2, 6-di-tert-butylphenol, etc. In some embodiments of the present invention, a specific class of the phenolic antioxidant may be 2, 6-di-tert-butyl-p-cresol. Therefore, the lubricating grease has more excellent oxidation stability, no pollution to the environment and higher efficiency.
According to the embodiment of the present invention, the grease further includes an anti-wear agent, and the specific kind of the anti-wear agent is not particularly limited, and one skilled in the art can flexibly select the anti-wear agent according to the requirement, for example, the anti-wear agent includes, but is not limited to, an organic chloride anti-wear agent, an organic metal salt anti-wear agent, a borate anti-wear agent, or a borate anti-wear agent. In some embodiments of the present invention, a specific type of the antiwear agent may be an organometallic salt antiwear agent. Therefore, the lubricating grease has better abrasion resistance, oxidation stability and rust resistance.
According to the embodiment of the present invention, the specific kind of the organic metal salt antiwear agent is not particularly limited as long as the requirement is satisfied, and those skilled in the art can flexibly select it as needed, for example, including but not limited to dialkyl dithiocarbamate, dialkyl dithiophosphate, diethyl phosphate amine salt, lead naphthenate, etc. In some embodiments of the present invention, the specific type of the organic metal salt antiwear agent may be diethyl phosphate amine salt, and specifically, may be molybdenum salt, antimony salt, or lead salt of diethyl phosphate amine. Therefore, the lubricating grease can further have excellent abrasion resistance, oxidation stability and rust resistance.
According to the embodiment of the present invention, the content of each component in the grease is not particularly limited, and one skilled in the art can flexibly select the components as needed as long as the requirements are met. In some embodiments of the present invention, the gallium-based liquid metal is present in an amount of 0.1 to 50 parts by weight, the grease base is present in an amount of 44 to 99.7 parts by weight, the antioxidant is present in an amount of 0 to 5 parts by weight, and the antiwear agent is present in an amount of 0 to 5 parts by weight. Therefore, the lubricating grease can achieve excellent extreme pressure performance under a high load condition, meanwhile, the cost of the lubricating grease is low, and the lubricating grease can also ensure good abrasion resistance under a low load condition, so that the abrasion resistance of a workpiece is not obviously affected in the using process, and the lubricating grease is suitable for various working conditions from low load to high load.
In another aspect of the invention, the invention provides a method of preparing a grease as described above. According to an embodiment of the invention, the method comprises mixing a gallium-based liquid metal and a grease base, and stirring and milling the resulting mixture. The inventor finds that the method is simple and convenient to operate, easy to realize and easy for industrial production, the lubricating grease prepared by the method is non-toxic, non-irritant and non-corrosive, the excellent extreme pressure performance equivalent to that of liquid metal can be achieved under the condition of high load, the cost can be reduced to less than one tenth of that of the liquid metal, the wear resistance under the condition of low load is obviously superior to that of the liquid metal, and the lubricating grease is suitable for various working conditions from low load to high load.
In the prior art, since the gallium-based liquid metal has good fluidity, and the lubricating grease matrix is a thick greasy semisolid which has the characteristics of high consistency, high dropping point, low penetration degree and the like, the gallium-based liquid metal and the lubricating grease matrix cannot be fully and uniformly mixed by a common dispersion method, so that the gallium-based liquid metal is generally considered to be incapable of being added into the lubricating grease as an extreme pressure agent of the lubricating grease in the prior art. In order to provide good extreme pressure performance to the grease, substances such as sulfur-containing compounds (such as sulfurized olefin, sulfurized lard, sulfurized oleic acid, polysulfide), phosphorus-containing compounds (such as phosphate, phosphite, phosphate) and the like are generally used as extreme pressure agents of the grease to be added into the grease, and the sulfur-containing compounds and the phosphorus-containing compounds have the defects of strong irritation and strong corrosiveness when being used as extreme pressure agents of the grease; in addition, the liquid metal can be directly used as the lubricant, and when the liquid metal is directly used as the lubricant, the cost is high, and the wear resistance under the low load condition is poor.
In the invention, the inventor has conducted a great deal of intensive investigation and experimental verification on the method for adding gallium-based liquid metal into the lubricating grease matrix, and found that the gallium-based liquid metal and the lubricating grease matrix can be fully and uniformly mixed by mixing the gallium-based liquid metal with the lubricating grease matrix and stirring and grinding the obtained mixture, the prepared mixture has good stability, and the gallium-based liquid metal and the lubricating grease matrix still do not have a layering phenomenon after being placed for a period of time, so that the gallium-based liquid metal is successfully added into the lubricating grease matrix as an extreme pressure agent of the lubricating grease, and the method is simple and convenient to operate, easy to implement and easy for industrial production.
The specific manner of mixing is not particularly limited according to the embodiments of the present invention, and one skilled in the art can flexibly select the mixing according to the requirements as long as the requirements are met, for example, but not limited to, adding the gallium-based liquid metal into the container in which the grease matrix is located, adding the grease matrix into the container in which the gallium-based liquid metal is located, or adding the gallium-based liquid metal and the grease matrix into the same container at the same time. In some embodiments of the present invention, the gallium-based liquid metal may be added into the grease matrix, and the grease matrix may be more easily and uniformly mixed due to the high consistency of the grease matrix.
According to the embodiment of the present invention, the mixing speed is not particularly limited, and one skilled in the art can flexibly select the mixing speed as needed, such as but not limited to slow dropwise addition or fast addition, as long as the requirement is met. In some embodiments of the invention, the rate of mixing may be a slow dropwise addition. Therefore, the gallium-based liquid metal and the lubricating grease matrix can be more easily and fully mixed uniformly.
According to the embodiment of the present invention, specific conditions of the stirring, such as temperature, time, etc., are not particularly limited, and those skilled in the art can flexibly select according to needs as long as the requirements are satisfied. In some embodiments of the invention, the temperature of the agitation may be 50-130 degrees celsius and the time of the agitation may be 20-60 minutes. In some more preferred embodiments of the present invention, the temperature of the stirring is 90 degrees celsius and the stirring time is 30 minutes. Therefore, the temperature is close to the dropping point of the grease matrix but not more than the dropping point, so that the consistency of the grease matrix can be reduced to the maximum extent on the premise of ensuring that the grease matrix is not deteriorated, the gallium-based liquid metal is fully mixed with the grease matrix, and the production efficiency is further improved.
According to the embodiment of the present invention, the specific manner of the stirring is not particularly limited, and those skilled in the art can flexibly select the stirring as needed as long as the requirement is satisfied. In some embodiments of the present invention, the stirring is performed by using a mechanical stirrer, and the stirring rate is 200-400 rpm. In some more preferred embodiments of the invention, the stirring rate is 300 rpm. Therefore, the operation is simple and convenient, the industrial production is easy, and the stirring efficiency is higher.
According to the embodiment of the present invention, the grinding tool is not particularly limited, and one skilled in the art can flexibly select the grinding tool as needed as long as the requirement is met. In some embodiments of the invention, the grinding tool may be a three-roll grinder. Therefore, the gallium-based liquid metal and the lubricating grease matrix can be fully and uniformly mixed, and the method is simple and convenient to operate and easy for industrial production.
According to the embodiment of the invention, the inventors have conducted a great deal of intensive investigation and experimental verification on the grinding time, and found that when the grinding time is 1-6 hours, the gallium-based liquid metal and the grease matrix can be well mixed and uniformly mixed. In some more preferred embodiments of the present invention, when the grinding time is 3 to 5 hours, the gallium-based liquid metal and the grease base are further mixed uniformly, and on the premise that the gallium-based liquid metal and the grease base are mixed uniformly, the preparation time is shortened to the greatest extent, and the production efficiency is improved.
According to the embodiment of the invention, as heat is generated in the grinding process, the gallium-based liquid metal and the grease matrix have certain temperature, so that the consistency of the grease matrix is reduced, and the gallium-based liquid metal and the grease matrix can be further fully and uniformly mixed.
The following describes embodiments of the present invention in detail.
Adding 92g of 15OBS base oil, 8g of thickening agent consisting of 12-hydroxystearic acid, sebacic acid and LiOH and 10g of water into a 250mL three-neck flask, heating to 90 ℃, reacting for 3 hours by mechanical stirring, then heating to 150 ℃, stirring for 2 hours, dehydrating, heating to 200 ℃, reacting for 30 minutes, cooling to 90 ℃, transferring to a three-roll grinder, and grinding to obtain the lubricating grease matrix.
Example 1
Taking 98g of lubricating grease matrix, adding 0.5g of antioxidant 2, 6-di-tert-butyl-p-cresol, 1g of antiwear agent diethyl phosphate amine salt and 0.5g of pure gallium, heating to 90 ℃, stirring for 30min to be uniform, cooling to room temperature, transferring to a three-roll grinder, and grinding for 3-5h to be uniform to obtain a sample 1.
Example 2
Taking 98g of a lubricating grease matrix, adding 0.5g of antioxidant 2, 6-di-tert-butyl-p-cresol, 1g of antiwear agent diethyl phosphate amine salt and 0.5g of a mixture containing 75 parts by weight of gallium and 25 parts by weight of indium, heating to 90 ℃, stirring for 30min to be uniform, transferring to a three-roll grinder, grinding for 3-5h to be uniform, and cooling to room temperature to obtain a sample 2.
Example 3
Taking 98g of a lubricating grease matrix, adding 0.5g of antioxidant 2, 6-di-tert-butyl-p-cresol, 1g of antiwear agent diethyl phosphate amine salt and 0.5g of a mixture containing 64 parts by weight of gallium, 24 parts by weight of indium and 12 parts by weight of tin, heating to 90 ℃, stirring for 30min to be uniform, cooling to room temperature, transferring to a three-roll grinder, and grinding for 3-5h to be uniform to obtain a sample 3.
Example 4
Taking 98g of lubricating grease matrix, adding 0.5g of antioxidant 2, 6-di-tert-butyl-p-cresol, 1g of antiwear agent diethyl phosphate amine salt and 0.5g of mixture containing 62 parts by weight of gallium, 24 parts by weight of indium, 12 parts by weight of tin and 2 parts by weight of zinc, heating to 90 ℃, stirring for 30min to be uniform, cooling to room temperature, transferring to a three-roll grinder, and grinding for 3-5h to be uniform to obtain a sample 4.
Example 5
Taking 97g of lubricating grease matrix, adding 0.5g of antioxidant 2, 6-di-tert-butyl-p-cresol, 1g of antiwear agent diethyl phosphate amine salt and 1.5g of mixture containing 75 parts by weight of gallium and 25 parts by weight of indium, heating to 90 ℃, stirring for 30min to be uniform, cooling to room temperature, transferring to a three-roll grinder, and grinding for 3-5h to be uniform to obtain a sample 5.
Example 6
Taking 93.5g of lubricating grease matrix, adding 0.5g of antioxidant 2, 6-di-tert-butyl-p-cresol, 1g of antiwear agent diethyl phosphate amine salt and 5g of mixture containing 75 parts by weight of gallium and 25 parts by weight of indium, heating to 90 ℃, stirring for 30min to be uniform, cooling to room temperature, transferring to a three-roll grinder, and grinding for 3-5h to be uniform to obtain a sample 6.
Example 7
Taking 88.5g of lubricating grease matrix, adding 0.5g of antioxidant 2, 6-di-tert-butyl-p-cresol, 1g of antiwear agent diethyl phosphate amine salt and 10g of mixture containing 75 parts by weight of gallium and 25 parts by weight of indium, heating to 90 ℃, stirring for 30min to be uniform, cooling to room temperature, transferring to a three-roll grinder, and grinding for 3-5h to be uniform to obtain a sample 7.
Example 8
Taking 90g of composite grease (KLUBER ISOFLEX LDS 18 SPECIAL A) and 10g of a mixture containing 75 parts by weight of gallium and 25 parts by weight of indium, stirring for 30min until the mixture is uniform, transferring the mixture to a three-roll grinder, and grinding for 3-5h to be uniform to obtain a sample 8.
Example 9
80g of composite grease (KLUBER ISOFLEX LDS 18 SPECIAL A) and 20g of a mixture containing 75 parts by weight of gallium and 25 parts by weight of indium are taken, stirred for 30min until the mixture is uniform, and transferred to a three-roll grinder to be ground for 3-5h to be uniform, so that a sample 9 is obtained.
Example 10
Taking 80g of composite lubricating grease (KLUBER ISOFLEX LDS 18 SPECIAL A) and 20g of pure gallium, stirring for 30min till uniformity, transferring to a three-roll grinder, and grinding for 3-5h till uniformity to obtain a sample 10.
Example 11
80g of composite grease (KLUBER ISOFLEX LDS 18 SPECIAL A) and 20g of a mixture containing 64 parts by weight of gallium, 24 parts by weight of indium and 12 parts by weight of tin are stirred for 30min until the mixture is uniform, and the mixture is transferred to a three-roll grinder to be ground for 3-5h to be uniform, so that a sample 11 is obtained.
Example 12
80g of composite grease (KLUBER ISOFLEX LDS 18 SPECIAL A) and 20g of a mixture containing 64 parts by weight of gallium, 24 parts by weight of indium and 12 parts by weight of tin are stirred for 30min until the mixture is uniform, and the mixture is transferred to a three-roll grinder to be ground for 3-5h to be uniform, so that a sample 12 is obtained.
Example 13
Taking 70g of composite grease (KLUBER ISOFLEX LDS 18 SPECIAL A) and 30g of a mixture containing 75 parts by weight of gallium and 25 parts by weight of indium, stirring for 30min till uniformity, transferring to a three-roll grinder, and grinding for 3-5h till uniformity to obtain a sample 13.
Example 14
Taking 50g of composite grease (KLUBER ISOFLEX LDS 18 SPECIAL A) and 50g of a mixture containing 75 parts by weight of gallium and 25 parts by weight of indium, stirring for 30min till uniformity, transferring to a three-roll grinder, and grinding for 3-5h till uniformity to obtain a sample 14.
Comparative example 1
50g of a mixture containing 75 parts by weight of gallium and 25 parts by weight of indium was taken and called EGaIn.
The sintering loads of the grease base, sample 1 to sample 14, and EGaIn were determined according to the national standard GB/T12583-1998 extreme pressure testing method for lubricants, and the results are shown in Table 1.
TABLE 1 sintering loads for grease base, samples 1-14, and EGaIn
Figure BDA0001469152310000131
The experimental data show that the sintering load of the grease of the present invention is higher than that of the grease base without the gallium-based liquid metal, and the grease prepared in example 14 can achieve excellent extreme pressure performance equivalent to that of the gallium-based liquid metal.
The wear-spot diameters of the grease base, the compound grease, sample 1 and sample 14, and EGaIn at low loads (40Kg) as measured by the "lubricating oil antiwear Performance test method (four ball machine method)" method of petrochemical industry Standard SH/T0189-92 are shown in Table 2.
TABLE 2 grease base, complex grease, sample 1 and sample 14, and wear scar diameter of EGaIn
Sample (I) Grease base Compound grease EGaIn 7 14
Abrasion Spot diameter (mm) 0.5 0.4 1.9 0.48 0.49
The experimental data show that the wear resistance of the lubricating grease is obviously superior to that of gallium-based liquid metal under the condition of low load, so that the lubricating grease has no obvious influence on the wear resistance of a workpiece and is suitable for various working conditions from low load to high load.
In the description herein, references to the description of the term "one embodiment," "some embodiments," "an example," "a specific example," or "some examples," etc., mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above are not necessarily intended to refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Furthermore, various embodiments or examples and features of different embodiments or examples described in this specification can be combined and combined by one skilled in the art without contradiction.
Although embodiments of the present invention have been shown and described above, it is understood that the above embodiments are exemplary and should not be construed as limiting the present invention, and that variations, modifications, substitutions and alterations can be made to the above embodiments by those of ordinary skill in the art within the scope of the present invention.

Claims (8)

1. A grease, characterized in that the grease has a sintering load of greater than 1000 kg, the grease comprising:
a grease base which is a thick grease-like semisolid; and
a gallium-based liquid metal, the gallium-based liquid metal being present in an amount of 50% by mass based on the total mass of the grease,
and the grease is prepared by the following steps:
slowly adding a gallium-based liquid metal dropwise into a container in which a grease base is present, and stirring and grinding the resulting mixture, wherein,
the stirring temperature is 50-130 ℃, the stirring time is 20-60 minutes, the stirring is carried out by utilizing a mechanical stirrer, and the stirring speed is 200-400 rpm;
the grinding is carried out by a three-roll grinder, and the grinding time is 3-5 hours.
2. The grease of claim 1, wherein the gallium-based liquid metal is pure gallium or a mixture of gallium and at least one selected from indium, tin, and zinc.
3. The grease of claim 2, wherein the mixture of gallium and at least one selected from indium, tin, and zinc contains one of the following:
28-95 parts of gallium and 5-72 parts of indium;
34-70 parts of gallium, 1-40 parts of indium and 1-26 parts of tin;
30-80 parts of gallium, 1-40 parts of indium, 1-30 parts of tin and 0.1-10 parts of zinc.
4. The grease of claim 1, wherein the grease matrix comprises:
a base oil; and
a thickening agent.
5. The grease of claim 4, wherein the base oil is one selected from 150BS base oil, 150SN base oil, 500SN base oil;
the thickener includes 12-hydroxystearic acid, sebacic acid, and LiOH.
6. The grease of claim 4, further comprising at least one of an antioxidant and an antiwear agent.
7. The grease of claim 1, wherein the grease matrix is a complex grease.
8. A method of preparing the grease of any one of claims 1-7, comprising:
slowly adding a gallium-based liquid metal dropwise into a container in which a grease base is present, and stirring and grinding the resulting mixture, wherein,
the stirring temperature is 50-130 ℃, the stirring time is 20-60 minutes, the stirring is carried out by utilizing a mechanical stirrer, and the stirring speed is 200-400 rpm;
the grinding is carried out by a three-roll grinder, and the grinding time is 3-5 hours.
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CN102977979A (en) * 2012-12-17 2013-03-20 江苏龙蟠石化有限公司 Composite lithium-calcium base lubricating grease and preparation method thereof
CN105062613A (en) * 2015-08-03 2015-11-18 清华大学 Lubricant as well as preparation method and application thereof
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Publication number Priority date Publication date Assignee Title
WO2004031328A2 (en) * 2002-10-01 2004-04-15 The Lubrizol Corporation Organic acid salts as thickeners
CN102977979A (en) * 2012-12-17 2013-03-20 江苏龙蟠石化有限公司 Composite lithium-calcium base lubricating grease and preparation method thereof
CN105062613A (en) * 2015-08-03 2015-11-18 清华大学 Lubricant as well as preparation method and application thereof
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