CN107502417B - layered potassium calcium sodium phosphate grease composition and preparation method thereof - Google Patents

layered potassium calcium sodium phosphate grease composition and preparation method thereof Download PDF

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CN107502417B
CN107502417B CN201710645502.3A CN201710645502A CN107502417B CN 107502417 B CN107502417 B CN 107502417B CN 201710645502 A CN201710645502 A CN 201710645502A CN 107502417 B CN107502417 B CN 107502417B
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calcium
sodium
potassium
phosphate
layered
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CN107502417A (en
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张效胜
董晋湘
牛文星
代莹静
徐红
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Taiyuan University of Technology
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    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M169/00—Lubricating compositions characterised by containing as components a mixture of at least two types of ingredient selected from base-materials, thickeners or additives, covered by the preceding groups, each of these compounds being essential
    • C—CHEMISTRY; METALLURGY
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    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M125/00—Lubricating compositions characterised by the additive being an inorganic material
    • C10M125/24—Compounds containing phosphorus, arsenic or antimony
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    • C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/085—Phosphorus oxides, acids or salts
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    • 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
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    • C10M2205/00—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions
    • C10M2205/18—Natural waxes, e.g. ceresin, ozocerite, bees wax, carnauba; Degras
    • C10M2205/183—Natural waxes, e.g. ceresin, ozocerite, bees wax, carnauba; Degras used as base material
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    • C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/02—Hydroxy compounds
    • C10M2207/023—Hydroxy compounds having hydroxy groups bound to carbon atoms of six-membered aromatic rings
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    • C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/02—Hydroxy compounds
    • C10M2207/023—Hydroxy compounds having hydroxy groups bound to carbon atoms of six-membered aromatic rings
    • C10M2207/026—Hydroxy compounds having hydroxy groups bound to carbon atoms of six-membered aromatic rings with tertiary alkyl groups
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    • 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
    • C10M2207/121—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of seven or less carbon atoms
    • C10M2207/123—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of seven or less carbon atoms polycarboxylic
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    • C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/10—Carboxylix acids; Neutral salts thereof
    • C10M2207/12—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms
    • C10M2207/125—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids
    • C10M2207/126—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids monocarboxylic
    • C10M2207/1265—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids monocarboxylic used as thickening agent
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    • 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
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    • C10M2215/00—Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
    • C10M2215/02—Amines, e.g. polyalkylene polyamines; Quaternary amines
    • C10M2215/04—Amines, e.g. polyalkylene polyamines; Quaternary amines having amino groups bound to acyclic or cycloaliphatic carbon atoms
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    • 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
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    • C10M2215/00—Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
    • C10M2215/22—Heterocyclic nitrogen compounds
    • C10M2215/223—Five-membered rings containing nitrogen and carbon only
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    • C10M2219/00—Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions
    • C10M2219/02—Sulfur-containing compounds obtained by sulfurisation with sulfur or sulfur-containing compounds
    • C10M2219/022—Sulfur-containing compounds obtained by sulfurisation with sulfur or sulfur-containing compounds of hydrocarbons, e.g. olefines
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    • C10M2219/00—Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions
    • C10M2219/10—Heterocyclic compounds containing sulfur, selenium or tellurium compounds in the ring
    • C10M2219/104—Heterocyclic compounds containing sulfur, selenium or tellurium compounds in the ring containing sulfur and carbon with nitrogen or oxygen in the ring
    • C10M2219/108—Phenothiazine
    • C—CHEMISTRY; METALLURGY
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    • C10M2223/00—Organic non-macromolecular compounds containing phosphorus as ingredients in lubricant compositions
    • C10M2223/02—Organic non-macromolecular compounds containing phosphorus as ingredients in lubricant compositions having no phosphorus-to-carbon bonds
    • C10M2223/04—Phosphate esters
    • C10M2223/045—Metal containing thio derivatives
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    • C10M2229/00—Organic macromolecular compounds containing atoms of elements not provided for in groups C10M2205/00, C10M2209/00, C10M2213/00, C10M2217/00, C10M2221/00 or C10M2225/00 as ingredients in lubricant compositions
    • C10M2229/04—Siloxanes with specific structure
    • C10M2229/041—Siloxanes with specific structure containing aliphatic substituents
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    • C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
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    • C10N2050/00—Form in which the lubricant is applied to the material being lubricated
    • C10N2050/10—Semi-solids; greasy

Abstract

The invention discloses layered potassium calcium sodium phosphate grease composition and a preparation method thereof, wherein the composition comprises the following components, by weight, 90.0-99.0 parts of basic sodium grease, 1.0-10.0 parts of solid anti-wear additive, and the solid anti-wear additive is layered potassium calcium phosphate CaKPO4·H2And O. The preparation method comprises the following steps: mixing basic sodium-based lubricating grease and layered potassium calcium phosphate (CaKPO)4·H2Stirring and mixing the O at room temperature to 200 ℃ for 1-24 h, and grinding and homogenizing for 0.5-6 h by using a triple roller or a quintuplet roller to obtain a sodium-based lubricating grease product.

Description

layered potassium calcium sodium phosphate grease composition and preparation method thereof
Technical Field
The invention discloses sodium-based lubricating greases with excellent wear resistance and a preparation method thereof, and particularly relates to sodium-based lubricating greases containing layered potassium calcium phosphate as a wear resistance additive and a preparation method thereof, belonging to the technical field of lubrication.
Background
With the modernization of industrial machinery, high-temperature lubricating grease is increasingly applied to , sodium-based lubricating grease has a moderate price and excellent performance (good thermal stability, colloid stability and shear stability) and plays a role in a plurality of important lubricating places (textile machinery, paper making machinery and the like).
Of solid antiwear agents during actual machine operationThe material which needs to consider economic cost, rich resources and low price is selected to be worth noting, calcium is which is the most -ubiquitous element in the crust of the earth, accounts for the fifth place, and the mass percentage content reaches 3.64 percent4·H2In the practical application process, the physical and chemical properties (such as purity, particle size and distribution, morphology and the like) of the solid lubricating material are required, the problem of impurity symbiosis existing in the mineral can bring negative effects, the problem can be effectively solved by utilizing a manual synthesis method, and the report of manual synthesis of the layered calcium potassium phosphate mineral material does not exist.
Disclosure of Invention
The invention aims to provide sodium-based lubricating greases with excellent wear resistance and a preparation method thereof, wherein the solid wear resistance additive is layered potassium calcium phosphate CaKPO4·H2O。
The sodium-based lubricating grease comprises the following components in parts by weight: 90.0-99.0 parts of basic sodium-based lubricating grease and 1.0-10.0 parts of solid anti-wear additive; wherein the solid antiwear additive is layered potassium calcium phosphate CaKPO4·H2O。
The preparation method of the sodium-based lubricating grease comprises the following steps: according to proper mass parts, basic sodium-based lubricating grease and layered potassium calcium phosphate CaKPO4·H2Stirring and mixing the O at room temperature to 200 ℃ for 1-24 h, and grinding and homogenizing for 0.5-6 h by using a triple roll machine or a five-roll machine to obtain a sodium-based lubricating grease product.
The basic sodium-based lubricating grease comprises fatty acid, antioxidant, antirust agent, extreme pressure agent and oxyhydrogen
Sodium chloride and base oil, wherein the raw materials comprise 5.0-35.0 parts of fatty acid, 65.0-95.0 parts of base oil, 0.5-5.0 parts of sodium hydroxide, 0.05-5.0 parts of antioxidant, 0-6.0 parts of antirust agent and 0-6.0 parts of extreme pressure agent.
The preparation method of the basic sodium-based lubricating grease comprises the following steps: 1/3 base oil and fatty acid are added into a grease making kettle, the temperature is raised to melt, and sodium hydroxide aqueous solution (the concentration is 20-35%) is slowly added at the temperature of 80-90 ℃. After the sodium hydroxide solution is added, controlling the temperature at 110 ℃ of 100 ℃ and saponifying for about 3-4 h; the temperature is increased to 150-; measuring the content of free acid and alkali at 160 deg.C to control it within 0.15-0.2%; slowly adding the rest base oil, continuously heating to 190-. The mixture is quenched to about 100 ℃ and homogenized by using a triple roll or a quintuplet roll.
The fatty acid is 12-hydroxystearic acid or stearic acid.
The antioxidant comprises of 2, 6-di-tert-butyl-p-cresol, β -naphthol, diphenylamine and phenothiazine.
The rust inhibitor comprises of alkenyl succinic acid, dodecenyl butanediamine and benzotriazole.
The extreme pressure agent is zinc dialkyl dithiophosphate ZDDP or sulfurized isobutylene T321.
The base oil is selected from or more of hydrocarbon mineral base oil, PAO series synthetic base oil and silicone oil series base oil, and is mixed in any ratio.
Layered potassium calcium phosphate CaKPO as described above4·H2The preparation method adopts a hydrothermal synthesis method, and specifically comprises the steps of reacting raw materials of a calcium source, a phosphorus source and inorganic potassium salt in an aqueous solution; reacting at 25-300 deg.C for 0.1-7 days, filtering, washing with distilled water, and drying at room temperature; the raw material ratio is the mol ratio of phosphorus to calcium (1-10): 1, the mol ratio of potassium to calcium (1-10): 1 and the mol ratio of water to calcium (5-100): 1.
The calcium source is selected from calcium chloride, calcium acetate, calcium hydroxide, calcium sulfate and calcium carbonate.
The phosphorus source is selected from phosphoric acid, potassium dihydrogen phosphate and dipotassium hydrogen phosphate.
The inorganic potassium salt is kinds selected from potassium chloride, potassium sulfate, potassium acetate and potassium hydroxide.
The invention has the following advantages and beneficial effects:
(1) the sodium-based lubricating grease added with layered calcium potassium phosphate as a solid lubricating additive has good bearing and wear-resisting capabilities and is suitable for various harsh working conditions.
(2) The invention reports the preparation of the sodium-based lubricating grease added with the layered calcium potassium phosphate as the solid lubricating additive, has rich raw material sources, and can effectively reduce the cost of industrial application.
(3) The invention reports sodium-based lubricating grease added with layered calcium potassium phosphate as a solid lubricating additive, the layered calcium potassium phosphate has good compatibility with various traditional lubricating grease additives, the preparation method is simple and easy to implement, and industrialization is easy to realize.
Drawings
FIG. 1 is an XRD pattern of layered potassium calcium phosphate obtained in example 1.
Detailed Description
The following are specific embodiments of the present invention, and the examples are merely illustrative and are not intended to limit the scope of the present invention.
Example 1
30.0 g of 100SN and 10.0 g of 12-hydroxystearic acid were added to a fat-making kettle, the mixture was melted by heating, and 25.0g of an aqueous sodium hydroxide solution (concentration: 20%) was slowly added thereto at 80 ℃. After the sodium hydroxide solution is added, controlling the temperature at 110 ℃ and saponifying for about 3 hours; the temperature is increased to 170 ℃ for dehydration, the materials in the kettle are observed to gradually become thick, and when the materials are in a thick wiredrawing shape, the water is basically completely removed; measuring the content of free acid and alkali at 160 ℃ to control the content to be 0.2%; then slowly adding 60.0 g of 100SN, continuously heating to 200 ℃ for thickening, adding 0.05 g of 2, 6-di-tert-butyl-p-cresol, 6.0 g of alkenyl succinic acid and 6.0 g T321, continuously heating to the maximum refining temperature, and keeping the temperature for 5 min after the materials in the kettle are in a true solution state. And (3) quenching to 100 ℃ and homogenizing by using a triple roller machine to obtain the basic sodium-based lubricating grease A.
A30 mL polytetrafluoroethylene stainless steel kettle was charged with 1.11 g of calcium chloride and 1.74 g of dipotassium hydrogen phosphate as raw materials, and reacted in 0.9 mL of an aqueous solution. Reacting for 7 days at the temperature of 25 ℃, filtering, washing by distilled water, and drying at room temperature to obtain the layered calcium potassium phosphate CaKPO4·H2And O. Fig. 1 is the XRD pattern of the product.
Selecting layered calcium potassium phosphate CaKPO4·H2Stirring O1.0 g and the basic sodium-based lubricating grease 99.0 g for 24 h at room temperature, and grinding and homogenizing by a triple roller machine for 0.5 h to obtain the finished product sodium-based lubricating grease.
The bearing wear resistance of the prepared sodium-based lubricating grease is evaluated by using a four-ball friction wear testing machine, the experimental parameters refer to GB/T3142-82 and SH/T0204-92, and the experimental result shows that after the layered potassium calcium phosphate is added, the bearing capacity is improvedP BThe values are significantly improved and the Wear Scar Diameter (WSD) is significantly reduced.
Figure DEST_PATH_IMAGE001
Example 2
Adding 31.7 g of PAO10 and 5.0g of stearic acid into a grease making kettle, heating to melt, slowly adding 2.5 g of sodium hydroxide aqueous solution (the concentration is 20%), controlling the temperature at 90 ℃, after the sodium hydroxide solution is completely added, controlling the temperature at 100 ℃, saponifying for about 4 hours, heating to 170 ℃ for dehydration, observing that the material in the kettle gradually thickens and presents a viscous wirelike shape, indicating that water is basically removed, measuring the content of free acid and alkali at 160 ℃ to control the content at 0.15%, then slowly adding 63.3 g of PAO10, continuously heating to 190 ℃ for thickening, adding 5.0g of β -naphthol, 1.0g of dodecenyl butylene and 1.0g of ZDDP, continuously heating to the highest refining temperature, keeping the temperature for 10 min to be close to 100 ℃ after the material in the kettle is in a true solution state, and homogenizing by using a five-linked roll machine to prepare the basic lubricating grease sodium base B.
A30 mL polytetrafluoroethylene stainless steel kettle was charged with 0.16 g of calcium acetate, 1.74 g of dipotassium hydrogen phosphate, and 1.74 g of potassium sulfate as raw materials, and reacted in 1.8 mL of an aqueous solution. Temperature ofReacting for 0.1 day at 300 ℃, filtering, washing by distilled water, and drying at room temperature to obtain the layered calcium potassium phosphate CaKPO4·H2O。
Selecting layered calcium potassium phosphate CaKPO4·H2Stirring 10.0 g of O and 90.0 g of the basic sodium-based lubricating grease for 11 hours at the temperature of 200 ℃, and grinding and homogenizing for 0.5 hour by using a triple roller machine to obtain the finished product sodium-based lubricating grease.
The bearing wear resistance of the prepared sodium-based lubricating grease is evaluated by using a four-ball friction wear testing machine, the experimental parameters refer to GB/T3142-82 and SH/T0204-92, and the experimental result shows that after the layered potassium calcium phosphate is added, the bearing capacity is improvedP BThe values are significantly improved and the Wear Scar Diameter (WSD) is significantly reduced.
Figure 408199DEST_PATH_IMAGE002
Example 3
21.7 g of PAO8 and 35.0 g of 12-hydroxystearic acid were added to a fat-making kettle, the mixture was melted by heating, and 8.0 g of an aqueous solution of sodium hydroxide (35% concentration) was slowly added thereto at 85 ℃. After the sodium hydroxide solution is added, controlling the temperature at 105 ℃ and saponifying for about 3.5 hours; the temperature is increased to 155 ℃ for dehydration, the materials in the kettle are observed to gradually become thick, and when the materials are in a thick wiredrawing shape, the water is basically completely removed; measuring the content of free acid and alkali at 160 deg.C to control it within 0.19%; then 63.3 g of PAO8 is slowly added, the heating is continued to be carried out to the temperature of 195 ℃ for thickening, 4.0 g of phenothiazine, 2.0 g of benzotriazole and 1.0g of ZDDP are added, the temperature is continued to be increased to the highest refining temperature, and when the materials in the kettle are in a true solution state, the temperature is kept for 6 min. And (3) quenching to 100 ℃ and homogenizing by using a triple roller machine to obtain the basic sodium-based lubricating grease C.
A30 mL polytetrafluoroethylene stainless steel vessel was charged with 0.37 g of calcium hydroxide, 1.36 g of potassium dihydrogen phosphate, and 1.4 g of potassium hydroxide as starting materials, and reacted in 4.5 mL of an aqueous solution. Reacting for 3 days at 180 ℃, filtering, washing by distilled water, and drying at room temperature to obtain the layered calcium potassium phosphate CaKPO4·H2O。
Selecting layered calcium potassium phosphate CaKPO4·H2Stirring O1.0 g and the basic sodium-based lubricating grease 99.0 g for 24 h at room temperature, and grinding and homogenizing by a five-roller machine for 6 h to obtain the finished product sodium-based lubricating grease.
The bearing wear resistance of the prepared sodium-based lubricating grease is evaluated by using a four-ball friction wear testing machine, the experimental parameters refer to GB/T3142-82 and SH/T0204-92, and the experimental result shows that after the layered potassium calcium phosphate is added, the bearing capacity is improvedP BThe values are significantly improved and the Wear Scar Diameter (WSD) is significantly reduced.
Figure DEST_PATH_IMAGE003
Example 4
27.0 g of 500SN and 20.0 g of stearic acid were added to a fat-making kettle, and the mixture was melted by heating, and 10.0 g of an aqueous solution of sodium hydroxide (35% concentration) was slowly added thereto at 88 ℃. After the sodium hydroxide solution is added, controlling the temperature at 108 ℃ and saponifying for about 3 hours; the temperature is increased to 165 ℃ for dehydration, the materials in the kettle are observed to gradually become thick, and when the materials are thick and threadlike, the water is basically completely removed; measuring the content of free acid and alkali at 160 deg.C to control it within 0.16%; then, 54.0 g of 500SN is slowly added, the heating is continuously carried out to 196 ℃ for thickening, 3.0 g of 2, 6-di-tert-butyl-p-cresol and 3.0 g of dodecenyl butanediamine are added, the heating is continuously carried out to the maximum refining temperature, and when the materials in the kettle are in a true solution state, the temperature is kept for 8 min. And (3) carrying out rapid cooling to the temperature of 100 ℃ and homogenizing by using a five-roller machine to obtain the basic sodium-based lubricating grease D.
A30 mL polytetrafluoroethylene stainless steel kettle was charged with the starting materials 1.36 g of calcium sulfate, 2.72 g of potassium dihydrogen phosphate and 2.94 g of phosphoric acid, and reacted in 15 mL of water. Reacting at 250 deg.C for 2 days, filtering, washing with distilled water, and drying at room temperature to obtain layered calcium potassium phosphate CaKPO4·H2O。
Selecting layered calcium potassium phosphate CaKPO4·H2Stirring and mixing O4.0 g and the basic sodium-based lubricating grease 96.0 g for 6 h at 150 ℃, homogenizing for 5 h by using a five-roller machine to ensure uniformity,and obtaining the finished product of the sodium-based lubricating grease.
The bearing wear resistance of the prepared sodium-based lubricating grease is evaluated by using a four-ball friction wear testing machine, the experimental parameters refer to GB/T3142-82 and SH/T0204-92, and the experimental result shows that after the layered potassium calcium phosphate is added, the bearing capacity is improvedP BThe values are significantly improved and the Wear Scar Diameter (WSD) is significantly reduced.
Figure 841453DEST_PATH_IMAGE004
Example 5
Adding 29.0 g of simethicone and 13.0 g of 12-hydroxystearic acid into a grease making kettle, heating to melt, slowly adding 10.0 g of sodium hydroxide aqueous solution (the concentration is 25 percent), controlling the temperature to be 86 ℃, controlling the temperature to be 104 ℃ after the sodium hydroxide solution is added, saponifying for about 4 hours, heating to 160 ℃ for dehydration, observing that the material in the kettle gradually thickens to be in a viscous drawing shape, indicating that water is basically removed, measuring the content of free acid and alkali at 160 ℃ to be controlled within the range of 0.16 percent, then slowly adding 58.0 g of simethicone, continuously heating to 192 ℃ for thickening, adding 4.0 g of β -naphthol and 3.0 g T321, continuously heating to the highest refining temperature, keeping the temperature for 7min after the material in the kettle is in a true solution state, rapidly cooling to be close to 100 ℃, and homogenizing by using a triple roll mill to prepare the basic lubricating grease base E.
A30 mL polytetrafluoroethylene stainless steel vessel was charged with 1.0g of calcium carbonate, 3.73 g of potassium chloride and 4.9g of phosphoric acid as raw materials, and reacted in 8.0 mL of water. Reacting for 7 days at the temperature of 25 ℃, filtering, washing by distilled water, and drying at room temperature to obtain the layered calcium potassium phosphate CaKPO4·H2O。
Selecting layered calcium potassium phosphate CaKPO4·H2Stirring and mixing 6.0 g of O and 94.0 g of the basic sodium-based lubricating grease for 1 hour at 180 ℃, and homogenizing for 3 hours by using a triple roller machine to obtain the finished product sodium-based lubricating grease.
The bearing and wear resistance of the prepared sodium-based lubricating grease is evaluated by using a four-ball friction and wear testing machine, and the experimental parameters refer to GB/T3142-82 andSH/T0204-92, the experimental result shows that after the lamellar calcium potassium phosphate is added, the bearing capacity is improvedP BThe values are significantly improved and the Wear Scar Diameter (WSD) is significantly reduced.
Figure DEST_PATH_IMAGE005
Example 6
22.0 g of liquid paraffin and 34.0 g of stearic acid were added to a grease kettle, the mixture was heated to melt, and 15.0 g of an aqueous sodium hydroxide solution (32% concentration) was slowly added thereto at 83 ℃. After the sodium hydroxide solution is added, controlling the temperature at 103 ℃ and saponifying for about 3.8 hours; the temperature is increased to 165 ℃ for dehydration, the materials in the kettle are observed to gradually become thick, and when the materials are thick and threadlike, the water is basically completely removed; measuring the content of free acid and alkali at 160 ℃ to control the content to be 0.19%; then slowly adding 66.0 g of liquid paraffin, continuously heating to 199 ℃ for thickening, adding 5.0g of diphenylamine, continuously heating to the highest refining temperature, and keeping the temperature for 9 min when the materials in the kettle are in a true solution state. And (3) carrying out rapid cooling to the temperature of 100 ℃ and homogenizing by using a five-roller machine to obtain the basic sodium-based lubricating grease F.
A30 mL polytetrafluoroethylene stainless steel kettle was charged with raw materials of 0.74 g calcium hydroxide, 0.98 g potassium acetate and 4.9g phosphoric acid, and reacted in 5 mL water. Reacting for 5 days at 180 ℃, filtering, washing by distilled water, and drying at room temperature to obtain the layered calcium potassium phosphate CaKPO4·H2O。
Selecting layered calcium potassium phosphate CaKPO4·H2Mixing O2.0 g and the basic sodium-based lubricating grease 98.0 g at 100 ℃ for 16 h, and homogenizing by a five-roller machine for 2 h to obtain the finished product sodium-based lubricating grease.
The bearing wear resistance of the prepared sodium-based lubricating grease is evaluated by using a four-ball friction wear testing machine, the experimental parameters refer to GB/T3142-82 and SH/T0204-92, and the experimental result shows that after the layered potassium calcium phosphate is added, the bearing capacity is improvedP BThe values are significantly improved and the Wear Scar Diameter (WSD) is significantly reduced.
Figure 745824DEST_PATH_IMAGE006
Example 7
30.0 g of 500SN and 57.0 g of liquid paraffin are mixed uniformly, 29.0 g of mixed oil sample and stearic acid are added into a grease making kettle, the temperature is raised to melt, and 15.0 g of sodium hydroxide aqueous solution (the concentration is 30 percent) is slowly added, and the temperature is 86 ℃. After the sodium hydroxide solution is added, controlling the temperature at 103 ℃ and saponifying for about 3.5 hours; the temperature is increased to 163 ℃ for dehydration, and when the materials in the kettle gradually become thick and are in a thick wiredrawing shape, the water is basically completely removed; measuring the content of free acid and alkali at 160 ℃ to control the content to be within 0.17%; then slowly adding 58.0 g of mixed oil sample, continuously heating to 194 ℃ for thickening, adding 2.0 g of 2, 6-di-tert-butyl-p-cresol and 3.0 g of dodecenyl butanediamine, continuously heating to the maximum refining temperature, and keeping the temperature for 7min when the materials in the kettle are in a true solution state. And (3) rapidly cooling to 100 ℃ and homogenizing by using a five-roller machine to obtain the basic sodium-based lubricating grease G.
A30 mL polytetrafluoroethylene stainless steel kettle was charged with the starting materials 0.27 g of calcium sulfate, 1.36 g of potassium dihydrogen phosphate and 0.59 g of phosphoric acid, and reacted in 2 mL of water. Reacting at 250 deg.C for 2 days, filtering, washing with distilled water, and drying at room temperature to obtain layered calcium potassium phosphate CaKPO4·H2O。
Selecting layered calcium potassium phosphate CaKPO4·H2And stirring and mixing 4.0 g of O and 96.0 g of the basic sodium-based lubricating grease for 6 hours at the temperature of 150 ℃, and homogenizing for 5 hours by using a five-roller machine to obtain the finished product sodium-based lubricating grease.
The bearing wear resistance of the prepared sodium-based lubricating grease is evaluated by using a four-ball friction wear testing machine, the experimental parameters refer to GB/T3142-82 and SH/T0204-92, and the experimental result shows that after the layered potassium calcium phosphate is added, the bearing capacity is improvedP BThe values are significantly improved and the Wear Scar Diameter (WSD) is significantly reduced.
Figure DEST_PATH_IMAGE007
From the above data it can be seen that: compared with the prior art, the invention adds the layered calcium potassium phosphate CaKPO4·H2Grease of O, bearing capacity thereofP BThe values are significantly improved and the Wear Scar Diameter (WSD) is significantly reduced. The method shows that after the potassium calcium phosphate material is added into the basic sodium-based grease, the bearing and wear resistance of the lubricating grease can be effectively improved.

Claims (6)

1, layered potassium calcium sodium phosphate grease composition, which is characterized by comprising the following components in parts by weight:
90.0-99.0 parts of basic sodium-based lubricating grease and 1.0-10.0 parts of solid anti-wear additive; wherein the solid antiwear additive is layered potassium calcium phosphate CaKPO4·H2O；
The layered calcium potassium phosphate CaKPO4·H2The preparation method adopts a hydrothermal synthesis method, and specifically comprises the steps of reacting raw materials of calcium source, phosphorus source and inorganic sylvite in an aqueous solution at the temperature of 25-300 ℃ for 0.1-7 days, filtering, washing with distilled water, and drying at room temperature to obtain the layered calcium potassium phosphate CaKPO4·H2O；
The raw materials are in the molar ratio of phosphorus to calcium (1-10): 1, the molar ratio of potassium to calcium (1-10): 1 and the molar ratio of water to calcium (5-100): 1.
2. The layered potassium calcium phosphate sodium-based lubricating grease composition according to claim 1, characterized in that the calcium source is of calcium chloride, calcium acetate, calcium hydroxide, calcium sulfate and calcium carbonate, the phosphorus source is of phosphoric acid, monopotassium phosphate and dipotassium phosphate, and the inorganic potassium salt is of potassium chloride, potassium sulfate and potassium hydroxide.
3, A method for preparing the layered potassium calcium phosphate sodium grease composition as claimed in any of claims 1-2, which comprises the steps of mixing basic sodium grease and layered potassium calcium phosphate CaKPO4·H2Stirring and mixing O at room temperature to 200 ℃ for 1-24 h, and grinding and homogenizing by using a triple roller or a five-roller machine for 0.5Homogenizing for 6 h to obtain the sodium-based lubricating grease product.
4. The method for preparing a layered potassium calcium sodium phosphate grease composition according to claim 3, wherein: the basic sodium-based lubricating grease is prepared by reacting and mixing raw materials including fatty acid, antioxidant, antirust agent, extreme pressure agent, sodium hydroxide and base oil, wherein the raw materials include 5.0-35.0 parts of fatty acid, 65.0-95.0 parts of base oil, 0.5-5.0 parts of sodium hydroxide, 0.05-5.0 parts of antioxidant, 0-6.0 parts of antirust agent and 0-6.0 parts of extreme pressure agent.
5. The method for preparing a layered potassium calcium sodium phosphate grease composition according to claim 3, wherein: the preparation method of the basic sodium-based lubricating grease comprises the following steps: adding 1/3 base oil and fatty acid into a fat making kettle, heating to melt, and slowly adding 20-35% sodium hydroxide aqueous solution at 80-90 deg.C; after the sodium hydroxide aqueous solution is added, controlling the temperature at 110 ℃ and saponifying for 3-4 h; the temperature is increased to 150-; measuring the content of free acid and alkali at 160 deg.C to control it within 0.15-0.2%; slowly adding the rest base oil, continuously heating to 190-; the mixture is quenched to about 100 ℃ and homogenized by using a triple roll or a quintuplet roll.
6. The preparation method of the layered potassium calcium phosphate sodium-based lubricating grease composition according to claim 5, wherein the fatty acid is 12-hydroxystearic acid or stearic acid, the antioxidant comprises of 2, 6-di-tert-butyl-p-cresol, β -naphthol, diphenylamine and phenothiazine, the antirust agent comprises of alkenyl succinic acid, dodecenyl butanediamine and benzotriazole, the extreme pressure agent is zinc dialkyl dithiophosphate ZDDP or sulfurized isobutylene T321, the base oil is selected from or more of hydrocarbon mineral base oil, PAO series synthetic base oil and silicone oil series base oil, and the selected base oil is mixed in any ratio.
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