CN107502418B - Environment-friendly layered potassium magnesium calcium phosphate grease and preparation method thereof - Google Patents
Environment-friendly layered potassium magnesium calcium phosphate grease and preparation method thereof Download PDFInfo
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- 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
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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
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- C10M2201/08—Inorganic acids or salts thereof
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- C10M2203/00—Organic non-macromolecular hydrocarbon compounds and hydrocarbon fractions as ingredients in lubricant compositions
- C10M2203/10—Petroleum or coal fractions, e.g. tars, solvents, bitumen
- C10M2203/1006—Petroleum or coal fractions, e.g. tars, solvents, bitumen 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
- C10M2205/02—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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- 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
- C10M2207/04—Ethers; Acetals; Ortho-esters; Ortho-carbonates
- C10M2207/046—Hydroxy ethers
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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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- C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
- C10M2207/40—Fatty vegetable or animal oils
- C10M2207/401—Fatty vegetable or animal oils used as base material
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- C10M2219/00—Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions
- C10M2219/08—Thiols; Sulfides; Polysulfides; Mercaptals
- C10M2219/082—Thiols; Sulfides; Polysulfides; Mercaptals containing sulfur atoms bound to acyclic or cycloaliphatic carbon atoms
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- 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
- C10M2219/08—Thiols; Sulfides; Polysulfides; Mercaptals
- C10M2219/082—Thiols; Sulfides; Polysulfides; Mercaptals containing sulfur atoms bound to acyclic or cycloaliphatic carbon atoms
- C10M2219/085—Thiols; Sulfides; Polysulfides; Mercaptals containing sulfur atoms bound to acyclic or cycloaliphatic carbon atoms containing carboxyl groups; Derivatives thereof
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- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
- C10N2030/06—Oiliness; Film-strength; Anti-wear; Resistance to extreme pressure
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- C10N2050/00—Form in which the lubricant is applied to the material being lubricated
- C10N2050/10—Semi-solids; greasy
Abstract
The invention discloses an ringA shape-preserving layered potassium magnesium calcium phosphate grease and a preparation method thereof. The lubricating grease comprises the following components in parts by weight: 80.0-99.0 parts of basic calcium-based lubricating grease and 1.0-20.0 parts of antiwear additive; wherein the antiwear additive is layered potassium magnesium phosphate MgKPO4·H2And O. The preparation method comprises the following steps: basic calcium-based lubricating grease and layered potassium magnesium phosphate MgKPO4·H2Stirring and mixing the O at room temperature to 200 ℃ for 1-16 h, and grinding and homogenizing for 0.5-5 h by using a three-roller machine or a high-pressure homogenizer to obtain a calcium-based lubricating grease product. The calcium-based lubricating grease using the layered potassium magnesium phosphate as the solid lubricating additive provided by the invention has excellent bearing and wear-resisting capabilities, green and environment-friendly raw materials and rich sources, and effectively reduces the cost.
Description
Technical Field
The invention discloses environment-friendly calcium-based lubricating greases with excellent wear resistance, in particular to environment-friendly calcium-based lubricating greases containing layered potassium magnesium phosphate as a wear-resistant additive and a preparation method thereof, belonging to the technical field of lubrication.
Background
The calcium-based lubricating grease has the characteristics of excellent water resistance, shear stability, thixotropic stability and pumping property, and is applied to times in the running occasions of rolling and sliding bearings with medium rotation speed and medium load in medium and small motors, water pumps, tractors, automobiles, metallurgy, textile machinery and the like at present, the calcium-based lubricating grease is a traditional classical lubricating grease type, the development direction is to improve the quality so as to adapt to increasingly rich and harsh working environments, and meanwhile, the increasingly strict energy-saving and environment-friendly requirements can be met.
The layered magnesium phosphate material (non-toxic and environment-friendly, and related materials reported in food additive application) is formed by mixing main body laminates with MgO6Octahedron, PO4The tetrahedron-formed inorganic compound has a layered crystal structure similar to that of molybdenum disulfide and graphite which are traditional solid lubricating additives on a microscopic scale, and is expected to show good lubricating performance, magnesium is high in abundance in earth crust, the mass percentage content reaches 2.4%, and the development of the magnesium industry is vigorous, so that the resource advantages are obvious, and the early stage of the subject group reports magnesium ion exchange type layered magnesium phosphates (Mg 103264999) in patent CN1032649994P4H14O21) As a lubricating oil additive, the lubricating property can be effectively improved, but the problems of high material synthesis cost and easy residue of ionic liquid exist, and the lubricating oil additive is not beneficial to large-scale industrial production. Lamellar potassium magnesium phosphate MgKPO4·H2O is made of MgO6Octahedron, PO4 kinds of inorganic layered magnesium phosphate compounds consisting of tetrahedral laminates and potassium ions and water molecules existing between the laminates [ G Jovanovski, S Pocev, BKaitner. Bulletin of the Chemists and technologies of Macedonia, 1997, 16(1): 59-63]And the hydrothermal synthesis is easy. At present, no layered potassium magnesium phosphate MgKPO exists4·H2O is reported as a solid lubricant additive for use in calcium-based greases.
Disclosure of Invention
The invention aims to provide environment-friendly calcium-based lubricating greases with excellent wear resistance and a preparation method thereof, wherein the wear resistance additive is layered potassium magnesium phosphate MgKPO4·H2O。
The calcium-based lubricating grease comprises the following components in parts by weight: basic calcium-based lubricating grease80.0-99.0 parts of antiwear additive, 1.0-20.0 parts of antiwear additive; wherein the antiwear additive is layered potassium magnesium phosphate MgKPO4·H2O。
The preparation method of the calcium-based lubricating grease comprises the following steps: according to proper mass parts, basic calcium-based lubricating grease and layered potassium magnesium phosphate MgKPO4·H2Stirring and mixing the O at room temperature to 200 ℃ for 1-16 h, and grinding and homogenizing for 0.5-5 h by using a three-roller machine or a high-pressure homogenizer to obtain a calcium-based lubricating grease product. The lubrication properties were evaluated using a four-ball friction and wear tester.
The basic calcium-based lubricating grease is prepared by reacting and mixing the following raw materials including fatty acid, base oil, calcium hydroxide and an antioxidant: wherein, 5.0 to 20.0 portions of fatty acid, 80.0 to 95.0 portions of base oil, 0.5 to 6.0 portions of calcium hydroxide and 0.05 to 5.0 portions of antioxidant. The specific preparation method of the basic calcium-based lubricating grease comprises the following steps: firstly, part of base oil, fatty acid and calcium hydroxide emulsifiable paste are put into a kettle, heated to 130-140 ℃ for saponification for 30-40 min, free acid and alkali are regulated and controlled to be qualified, water is introduced for cooling, the stirring speed is increased for hydration until the material is obviously thickened into grease, an antioxidant is added, the mixture is stirred for 10-20 min after phase change, the rest base oil is added for adjusting the penetration degree, and the mixture is ground uniformly by a three-roller machine to obtain the base calcium-based lubricating grease.
The fatty acids include or both of 12-hydroxystearic acid and stearic acid, and when selected, the two are mixed in any ratio.
The antioxidant includes kinds of methyl propyl disulfide, dilauryl thiodipropionate, tert-butyl hydroxy anisol or 2, 6-di-tert-butyl p-cresol.
The base oil is selected from or more of vegetable oil, environment-friendly synthetic base oil or mineral oil, and the selected oils can be mixed at any ratio.
The animal and vegetable oil refers to kinds or more of lard oil, beef tallow, epoxidized soybean oil or coconut oil, and the selected several kinds are mixed in any ratio.
The environment-friendly synthetic oil is PAO series synthetic oil.
The mineral oil is refined white oil.
Layered potassium magnesium phosphate MgKPO as described above4·H2The preparation method of the O-magnesium alloy material comprises the steps of reacting raw materials of a magnesium source, a phosphorus source and inorganic potassium salt in an aqueous solution at the temperature of 25-300 ℃ for 0.1-10 days, filtering, washing with distilled water, and drying at room temperature, wherein the raw materials comprise phosphorus and magnesium in a molar ratio of (1-10): 1, potassium and magnesium in a molar ratio of (1-10): 1 and water and magnesium in a molar ratio of (5-100): 1.
The magnesium source is selected from magnesium chloride, magnesium acetate, magnesium sulfate or amorphous magnesium phosphate.
The phosphorus source is selected from phosphoric acid, potassium dihydrogen phosphate or dipotassium hydrogen phosphate.
The inorganic potassium salt is kinds selected from potassium chloride, potassium acetate, potassium sulfate or potassium hydroxide.
All other components are not mentioned to adopt environment-friendly components specified by pharmacopoeia.
The invention has the following advantages and beneficial effects:
(1) the calcium-based lubricating grease added with layered potassium magnesium phosphate as the solid lubricating additive has good bearing and wear resistance, is suitable for various harsh working conditions, particularly the application field with high environmental protection requirements, has simple and easy preparation method, and is easy to realize industrialization.
(2) The invention reports the preparation of the calcium-based lubricating grease added with the layered potassium magnesium phosphate as the solid lubricating additive, has rich raw material sources, and can effectively reduce the cost of industrial application.
Drawings
FIG. 1 is an XRD pattern of layered potassium magnesium phosphate obtained in example 1.
Detailed Description
Example 1
Firstly, 40.0 g of refined white oil, 20.0 g of 12-hydroxystearic acid and 0.5 g of calcium hydroxide cream are put into a kettle, heated to 130 ℃ for saponification for 30 min, free acid and alkali are regulated and controlled to be qualified, water is introduced for cooling, the stirring speed is increased for hydration until the material is obviously thickened into grease, 0.1 g of 2, 6-di-tert-butyl-p-cresol is added, phase change is carried out, stirring is carried out for 10 min, 40.0 g of refined white oil is added for adjusting cone penetration, and the base calcium-based lubricating grease is obtained after the materials are uniformly ground by a three-roll machine.
A30 mL polytetrafluoroethylene stainless steel kettle was charged with 0.75 g of magnesium chloride, 1.36 g of potassium dihydrogen phosphate, and 4.9 g of potassium acetate, and reacted in 10 mL of an aqueous solution. Reacting for 5 days at the temperature of 150 ℃, filtering, washing by distilled water, and drying at room temperature to obtain the layered potassium magnesium phosphate MgKPO4·H2And O. Fig. 1 is the XRD pattern of the product.
Selecting layered potassium magnesium phosphate MgKPO4·H2O1.0 g and the above basic calcium grease 99.0 g were stirred at room temperature for 16 hours, and homogenized by grinding with a three-roll mill for 0.5 hour to obtain calcium grease A.
Example 2
Firstly, 47.5 g of PAO8, 5.0 g of stearic acid and 6.0 g of calcium hydroxide cream are put into a kettle, heated to 140 ℃ for saponification for 40 min, free acid and alkali are regulated to be qualified, water is introduced for cooling, the stirring speed is increased for hydration until the materials are obviously thickened into grease, 0.05 g of methyl propyl disulfide is added, the materials are stirred for 20min after phase change, PAO8 is added for adjusting the cone penetration, and the basic calcium-based lubricating grease is obtained after the materials are uniformly ground by a three-roller machine.
A30 mL polytetrafluoroethylene stainless steel kettle was charged with 0.21 g of magnesium acetate, 2.28 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. Reacting at 300 deg.C for 0.1 day, filtering, washing with distilled water, and drying at room temperature to obtain layered potassium magnesium phosphate MgKPO4·H2O。
Selecting layered potassium magnesium phosphate MgKPO4·H220.0 g of O and 80.0g of the basic calcium grease are stirred for 1 hour at the temperature of 200 ℃, and are ground and homogenized for 5 hours by a three-roller machine to prepare the calcium grease B.
Example 3
Firstly, putting 45.0 g of epoxidized soybean oil, 10.0 g of 12-hydroxystearic acid and 2.0 g of calcium hydroxide cream into a kettle, heating to 135 ℃ for saponification for 35 min, regulating and controlling free acid and alkali to be qualified, introducing water for cooling, increasing stirring speed for hydration until the material is obviously thickened into grease, adding 5.0 g of dilauryl thiodipropionate, stirring for 15min after phase change, adding 45.0 g of epoxidized soybean oil for adjusting cone penetration, and uniformly grinding by a three-roller machine to obtain the basic calcium-based lubricating grease.
A30 mL polytetrafluoroethylene stainless steel vessel was charged with the starting materials 0.3 g magnesium sulfate, 3.4 g potassium dihydrogen phosphate and 0.7g potassium hydroxide, and reacted in 15 mL of an aqueous solution. Reacting at 25 deg.C for 10 days, filtering, washing with distilled water, and drying at room temperature to obtain layered potassium magnesium phosphate MgKPO4·H2O。
Selecting layered potassium magnesium phosphate MgKPO4·H2O3.0 g and the basic calcium grease 97.0 g are stirred for 10 h at 100 ℃, and are ground and homogenized for 1.5 h by a high-pressure homogenizer to prepare the calcium grease C.
Example 4
Firstly, 42.5 g of beef tallow, 15.0 g of stearic acid and 3.0 g of calcium hydroxide cream are put into a kettle, the temperature is raised to 134 ℃ for saponification for 34 min, the free acid and alkali are regulated and controlled to be qualified, the water is introduced for cooling, the stirring speed is increased for hydration until the materials are obviously thickened into grease, 3.0 g of tert-butyl hydroxy anisole is added, the materials are stirred for 14 min after phase change, 42.5 g of beef tallow is added for adjusting the cone penetration, and the basic calcium-based lubricating grease is obtained after the materials are uniformly ground by a three-roller machine.
A30 mL polytetrafluoroethylene stainless steel vessel was charged with 2.14 g of magnesium acetate, 6.8 g of potassium dihydrogen phosphate, and 4.9 g of phosphoric acid as starting materials, and reacted in 5 mL of water. Reacting for 3 days at 180 ℃, filtering, washing by distilled water, and drying at room temperature to obtain the layered potassium magnesium phosphate MgKPO4·H2O。
Selecting layered potassium magnesium phosphate MgKPO4·H25.0 g of O and 95.0 g of the basic calcium grease are stirred and mixed for 12 hours at the temperature of 50 ℃, and homogenized by a three-roller machine for 3 hours to prepare the calcium grease D.
Example 5
42.0 g of lard, 16.0 g of 12-hydroxystearic acid and 4.0 g of calcium hydroxide cream are firstly put into a kettle, heated to 136 ℃ for saponification for 36 min, free acid and alkali are regulated and controlled to be qualified, water is introduced for cooling, the stirring speed is increased for hydration until the material is obviously thickened into grease, 2.0 g of methyl propyl disulfide is added, the mixture is stirred for 16 min after phase change, 42.0 g of lard is added for adjusting the cone penetration, and the basic calcium-based lubricating grease is obtained after the mixture is uniformly ground by a three-roller machine.
A30 mL polytetrafluoroethylene stainless steel kettle was charged with 2.09 g of amorphous magnesium phosphate, 2.98 g of potassium chloride and 5.88 g of phosphoric acid as raw materials, and reacted in 15 mL of water. Reacting for 6 days at the temperature of 100 ℃, filtering, washing by distilled water, and drying at room temperature to obtain the layered potassium magnesium phosphate MgKPO4·H2O。
Selecting layered potassium magnesium phosphate MgKPO4·H2O9.0 g and the above basic calcium grease 91.0 g were stirred and mixed at 180 ℃ for 1 hour, and homogenized by a three-roll mill for 3 hours to obtain calcium grease E.
Example 6
Firstly, uniformly mixing 16.0 g of coconut oil and 80.0g of refined white oil, putting 48.0 g of mixed oil sample, 14.0 g of stearic acid and 5.0 g of calcium hydroxide cream into a kettle, heating to 132 ℃, saponifying for 38 min, regulating and controlling free acid and alkali to be qualified, introducing water, cooling, increasing stirring speed for hydration until the material is obviously thickened into grease, adding 4.0 g of tert-butyl hydroxy anisole, stirring for 18 min after phase change, adding 48.0 g of mixed oil sample, adjusting cone penetration, and uniformly grinding by using a three-roller machine to obtain the basic calcium-based lubricating grease.
A30 mL polytetrafluoroethylene stainless steel kettle was charged with raw materials of 0.42 g amorphous magnesium phosphate, 0.59 g potassium acetate and 0.59 g phosphoric acid, and reacted in 20 mL water. Reacting for 5 days at the temperature of 150 ℃, filtering, washing by distilled water, and drying at room temperature to obtain the layered potassium magnesium phosphate MgKPO4·H2O。
Selecting layered potassium magnesium phosphate MgKPO4·H215.0 g of O and 85.0 g of the basic calcium grease are stirred and mixed for 3 hours at the temperature of 180 ℃, and homogenized for 1.5 hours by a high-pressure homogenizer to prepare the calcium grease F.
Example 7
Firstly, uniformly mixing 30.0 g of epoxidized soybean oil and 60.0 g of beef tallow, putting 45.0 g of mixed oil sample, 15.0 g of 12-hydroxystearic acid and 5.0 g of calcium hydroxide cream into a kettle, heating to 132 ℃, saponifying for 38 min, regulating free acid and alkali to be qualified, introducing water, cooling, increasing stirring speed for hydration until the material is obviously thickened into grease, adding 5.0 g of dilauryl thiodipropionate, stirring for 15min after phase change, adding 45.0 g of mixed oil sample, adjusting conicity, and uniformly grinding by a three-roller machine to obtain the basic calcium-based lubricating grease.
A30 mL polytetrafluoroethylene stainless steel kettle was charged with 0.6 g of magnesium sulfate and 6.8 g of potassium dihydrogen phosphate as raw materials, and reacted in 6mL of an aqueous solution. Reacting at 25 deg.C for 10 days, filtering, washing with distilled water, and drying at room temperature to obtain layered potassium magnesium phosphate MgKPO4·H2O。
Selecting layered potassium magnesium phosphate MgKPO4·H2Stirring O10.0G and the basic calcium grease 90.0G at 100 deg.C for 8.0 h, and grinding with high pressure homogenizer for 1.0 h to homogenize to obtain calcium grease G.
Example 8
Firstly, uniformly mixing 42.5 g of lard oil and 42.5 g of coconut oil, putting 42.5 g of mixed oil, 8.0 g of 12-hydroxystearic acid, 8.0 g of stearic acid and 4.0 g of calcium hydroxide cream into a kettle, heating to 135 ℃, saponifying for 35 min, regulating and controlling free acid and alkali to be qualified, introducing water for cooling, increasing the stirring speed for hydration until the material is obviously thickened into grease, adding 2.0 g of methyl propyl disulfide, stirring for 16 min after phase change, adding 42.5 g of mixed oil sample for adjusting the cone penetration, and uniformly grinding by a three-roller machine to obtain the basic calcium-based lubricating grease.
A30 mL polytetrafluoroethylene stainless steel kettle was charged with 2.09 g of amorphous magnesium phosphate, 0.75 g of potassium chloride and 4.9 g of phosphoric acid as raw materials, and reacted in 10 mL of water. Reacting for 1 day at the temperature of 100 ℃, filtering, washing by distilled water, and drying at room temperature to obtain the layered potassium magnesium phosphate MgKPO4·H2O。
Selecting layered potassium magnesium phosphate MgKPO4·H28.0 g of O and 92.0 g of the basic calcium grease are stirred and mixed for 5.0H at the temperature of 150 ℃, and are homogenized for 3.0H by a three-roller machine to prepare the calcium grease H.
The lubricating property and the bearing capacity of the calcium-based lubricating grease are evaluated according to GB/T3142-82 and SH/T0204-92 by using a mansion sky machine MS-10A type four-ball friction wear testing machineP BSignificant value improvement, abrasion mark diameter WSDThe reduction is obvious, which shows that after the potassium magnesium phosphate material is added into the basic calcium-based grease, the bearing and anti-wear capacity of the lubricating grease can be effectively improved. The specific four-ball frictional wear test results data are shown in table 1.
TABLE 1
The above embodiments are merely illustrative, and the scope of the present invention should not be limited thereto, and modifications and changes made without departing from the scope of the present invention should be made within the scope of the present invention.
Claims (9)
1, parts of environment-friendly layered potassium magnesium phosphate calcium-based lubricating grease, which is characterized by comprising 80.0-99.0 parts of basic calcium-based lubricating grease and 1.0-20.0 parts of anti-wear additive, wherein the anti-wear additive is layered potassium magnesium phosphate MgKPO4·H2O;
The layered potassium magnesium phosphate MgKPO4·H2O, the preparation method comprises the steps of reacting raw materials of a magnesium source, a phosphorus source and inorganic potassium salt in an aqueous solution at the temperature of 25-300 ℃ for 0.1-10 days, filtering, washing with distilled water, and drying at room temperature to obtain the magnesium-containing organic silicon-based organic;
the raw material ratio is the mol ratio of phosphorus to magnesium (1-10): 1, the mol ratio of potassium to magnesium (1-10): 1 and the mol ratio of water to magnesium (5-100): 1.
2. The environment-friendly layered calcium magnesium potassium phosphate grease as claimed in claim 1, wherein the magnesium source is of magnesium chloride, magnesium acetate, magnesium sulfate and amorphous magnesium phosphate, 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 environment-friendly layered calcium magnesium potassium phosphate grease of any one of claims 1-2 to , comprising the step of adding basic calcium greaseLamellar potassium magnesium phosphate MgKPO4·H2Stirring and mixing the O at room temperature to 200 ℃ for 1-16 h, and grinding and homogenizing for 0.5-5 h by using a three-roller machine or a high-pressure homogenizer to obtain a calcium-based lubricating grease product.
4. The preparation method of the environment-friendly layered potassium magnesium calcium phosphate grease as claimed in claim 3, wherein the preparation method comprises the following steps: the basic calcium-based lubricating grease is prepared by reacting and mixing raw materials including fatty acid, base oil, calcium hydroxide and an antioxidant: wherein, 5.0 to 20.0 portions of fatty acid, 80.0 to 95.0 portions of base oil, 0.5 to 6.0 portions of calcium hydroxide and 0.05 to 5.0 portions of antioxidant;
the specific preparation method of the basic calcium-based lubricating grease comprises the following steps: firstly, part of base oil, fatty acid and calcium hydroxide emulsifiable paste are put into a kettle, heated to 130-140 ℃ for saponification for 30-40 min, free acid and alkali are regulated and controlled to be qualified, water is introduced for cooling, the stirring speed is increased for hydration until the material is obviously thickened into grease, an antioxidant is added, the mixture is stirred for 10-20 min after phase change, the rest base oil is added for adjusting the penetration degree, and the mixture is ground uniformly by a three-roller machine to obtain the base calcium-based lubricating grease.
5. The method for preparing environment-friendly layered potassium magnesium calcium phosphate grease as claimed in claim 4, wherein the fatty acid comprises kinds or two kinds of 12-hydroxystearic acid and stearic acid, and the two kinds of fatty acid are mixed at any ratio.
6. The method for preparing environment-friendly layered potassium magnesium calcium phosphate grease as claimed in claim 4, wherein the antioxidant comprises kinds of methyl propyl disulfide, dilauryl thiodipropionate, tert-butyl hydroxy anisol, and 2, 6-di-tert-butyl-p-cresol.
7. The method for preparing environment-friendly layered calcium magnesium potassium phosphate grease as claimed in claim 4, wherein the base oil is selected from kinds or more of vegetable oil, environment-friendly synthetic oil or mineral oil, and the selected kinds are mixed at any ratio.
8. The method for preparing the environment-friendly layered potassium magnesium calcium phosphate-based lubricating grease as claimed in claim 7, wherein the animal and vegetable oil is kinds or more of lard, beef tallow, epoxidized soybean oil and coconut oil, and the selected several kinds are mixed in any ratio.
9. The preparation method of the environment-friendly layered potassium magnesium calcium phosphate grease as claimed in claim 7, wherein the preparation method comprises the following steps: the environment-friendly synthetic oil is PAO series synthetic oil; the mineral oil is refined white oil.
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US3421877A (en) * | 1965-04-19 | 1969-01-14 | Grace W R & Co | Method of precipitating potash from a phosphate mixture |
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