CN115851346B - Color lubricating grease with lamellar borophosphate as solid additive and preparation method thereof - Google Patents

Color lubricating grease with lamellar borophosphate as solid additive and preparation method thereof Download PDF

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CN115851346B
CN115851346B CN202211721218.7A CN202211721218A CN115851346B CN 115851346 B CN115851346 B CN 115851346B CN 202211721218 A CN202211721218 A CN 202211721218A CN 115851346 B CN115851346 B CN 115851346B
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boron
borophosphate
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CN115851346A (en
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张效胜
孔晓伟
徐小奇
贺雪雪
马冲
刘雷
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Taiyuan University of Technology
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Abstract

The invention discloses color lubricating grease taking lamellar borophosphate as a solid additive and a preparation method thereof, wherein the color lubricating grease comprises the following raw materials in parts by weight: 90.0-99.0 parts of basic composite calcium-based lubricating grease and 1.0-10.0 parts of solid lubricating additive; the solid lubricating additive is lamellar borophosphate M (H 2O)2[B2P2O8(OH)2]H2 O, wherein M represents one of Cu, co, ni, mn metals), namely, the lamellar borophosphate is Cu(H2O)2[B2P2O8(OH)2]H2O、Co(H2O)2[B2P2O8(OH)2]H2O、Ni(H2O)2[B2P2O8(OH)2]H2O or Mn (one of H 2O)2[B2P2O8(OH)2]H2 O), the lamellar borophosphate M (H 2O)2[B2P2O8(OH)2]H2 O material molecules contain lubricating elements such as boron, phosphorus and the like, so that extreme pressure, bearing, wear resistance and antifriction of lubricating grease can be effectively improved, and meanwhile, the material has rich and bright color and luster, and can be added into the lubricating grease as a solid additive to play roles of a lubricating improver and a dye.

Description

Color lubricating grease with lamellar borophosphate as solid additive and preparation method thereof
Technical Field
The invention relates to a composition of color grease, in particular to color grease with good lubricating property and using lamellar borophosphate as a solid additive and a preparation method thereof, and belongs to the technical field of grease preparation.
Background
Grease is a stable semi-solid or semi-fluid product formed from a thickener dispersed in a liquid lubricant and has unique rheological properties. Because of the inherent good properties of the lubricating grease, besides the general lubrication function, the functions of extreme pressure, wear resistance, sealing and protection of the lubricating grease are far superior to those of conventional lubricating grease, so that the lubricating grease is widely applied to the motion parts of gears, bearings and other machines of various industrial machines.
In order to facilitate maintenance when the machine does not stop working, a lubricating system of large-scale mechanical equipment such as a continuous casting machine, a wind motor, a blast furnace top machine and the like mostly adopts double-line centralized lubrication, and is sent to a needed lubricating point through a pipeline by a lubricating grease supply source; meanwhile, oil quantity adjustment is needed to be carried out on each lubrication point, so that the best protection effect is achieved. The color lubricating grease is used, so that whether the lubricating grease is dispensed in place or not can be conveniently observed; after the color grease is used, the oil leakage condition of the equipment is more easily found. In addition, in maintenance of a large motor, it is judged whether lubrication is failed by observing the degree of color change of grease discharged from the motor. Conventional color greases are typically formulated by adding specific pigments. The pigment types generally include inorganic pigments represented by cadmium red (nCdS, cdSe), iron red (Fe 2O3), etc., and organic pigments represented by naphthol green B, sudan iii, oil-soluble orange, pigment yellow G, etc. (chinese patent CN 111748400a; chinese patent CN101886017a; chinese patent CN 101886018a ]. Usually, the addition of these pigments only plays a role in color mixing in grease, and has no lubricating protective effect.
The solid lubricant is an important additive in lubricating grease, and can play roles in extreme pressure, bearing, wear resistance, antifriction and collaborative reinforcement when being subjected to severe operation conditions such as high load, high temperature, strong radiation and the like. With the development of modern industrial technology, higher and higher requirements are put on the performance of lubricating grease. Accordingly, there is a continuing need to develop new solid lubricant additive materials to meet the needs of different operating conditions.
Disclosure of Invention
The invention aims to provide color lubricating grease with good lubricating property and taking lamellar borophosphate as a solid additive and a preparation method thereof.
The principle of the invention is as follows: the invention relates to a color grease containing lamellar borophosphate (M (H 2O)2[B2P2O8(OH)2]H2 O), wherein M (H 2O)2[B2P2O8(OH)2]H2 O) (wherein M stands for Cu/Co/Ni/Mn) is a series of lamellar borophosphate materials, lubricating elements such as boron, phosphorus and the like are contained in molecular composition, so that extreme pressure, bearing, wear resistance and antifriction properties can be effectively improved, meanwhile, the material is self-colored and has good dyeing effect.
The invention provides composite calcium-based lubricating grease with different lamellar borophosphates as solid additives, which comprises the following raw materials in parts by weight:
90.0 to 99.0 parts of basic composite calcium-based lubricating grease,
1.0-10.0 Parts of solid lubricating additive;
The solid lubricating additive is lamellar borophosphate M (H 2O)2[B2P2O8(OH)2]H2 O (wherein M represents one of Cu, co, ni, mn metals), namely :Cu(H2O)2[B2P2O8(OH)2]H2O、Co(H2O)2[B2P2O8(OH)2]H2O、Ni(H2O)2[B2P2O8(OH)2]H2O or Mn (H 2O)2[B2P2O8(OH)2]H2 O).
The preparation method of the lamellar borophosphate comprises the steps of reacting raw materials corresponding to a metal source, a phosphorus source and a boron source in a water solution according to a certain proportion, filtering, washing with distilled water, and drying at room temperature.
Further, the metal is copper, and the copper source is one of copper chloride, copper acetate or copper sulfate;
the phosphorus source is one of phosphoric acid, trimethyl phosphate, tributyl phosphate or boron phosphate;
the boron source is one of boric acid, boron oxide or boron phosphate;
The mixture ratio of the raw materials is as follows: the mole ratio of the phosphorus source to the boron source to the copper source to the water is (0.5-10) to 1 to (3-500); the specific reaction process is as follows: the reaction temperature is 25-250 ℃, and the reaction is carried out for 0.05-7 days.
Further, the metal is cobalt, and the cobalt source is one of cobalt chloride, cobalt acetate or cobalt sulfate;
the phosphorus source is one of phosphoric acid, trimethyl phosphate, tributyl phosphate or boron phosphate;
the boron source is one of boric acid, boron oxide or boron phosphate;
the mixture ratio of the raw materials is as follows: the mole ratio of the phosphorus source to the boron source to the cobalt source to the water is (1-12) to 1 to (5-600); the specific reaction process is as follows: the reaction temperature is 50-350 ℃, and the reaction is carried out for 1-11 days.
Further, the metal is nickel, and the nickel source is one of nickel chloride, nickel acetate or nickel sulfate;
the phosphorus source is one of phosphoric acid, trimethyl phosphate, tributyl phosphate or boron phosphate;
the boron source is one of boric acid, boron oxide or boron phosphate;
The mixture ratio of the raw materials is as follows: the mole ratio of the phosphorus source to the boron source to the nickel source to the water is (0.5-8) to 1 to (3-300); the specific reaction process is as follows: the reaction temperature is 25-300 ℃, and the reaction is carried out for 1-8 days.
Further, the metal is manganese, and the manganese source is one of manganese chloride, manganese acetate or manganese sulfate;
the phosphorus source is one of phosphoric acid, trimethyl phosphate, tributyl phosphate or boron phosphate;
the boron source is one of boric acid, boron oxide or boron phosphate;
The mixture ratio of the raw materials is as follows: the mole ratio of the phosphorus source to the boron source to the manganese source to the water is (1.5-12) to 1 to (10-500); the specific reaction process is as follows: the reaction temperature is 50-200 ℃, and the reaction is carried out for 0.05-10 days.
The invention provides a preparation method of the composite calcium-based lubricating grease with the layered borophosphate as a solid additive, which comprises the following steps: mixing the basic composite calcium-based lubricating grease and the layered borophosphate for 0.5-36 hours at the temperature of between room temperature and 280 ℃ according to the mass ratio, and grinding and homogenizing for 0.1-5 hours by using a three-roll machine or a high-pressure homogenizer to obtain the composite calcium-based lubricating grease product.
According to the preparation method, the basic composite calcium-based lubricating grease is prepared by mixing and reacting raw materials including fatty acid, low molecular acid, a calcium source, base oil and an antioxidant, wherein the fatty acid is 2.0-25.0 parts, the low molecular acid is 1.0-6.0 parts, the calcium source is 1.0-9.0 parts, the base oil is 60.0-96.0 parts, and the antioxidant is 0.5-6.0 parts;
in the preparation method, the preparation method of the basic composite calcium-based lubricating grease comprises the following steps: adding the metered fatty acid, the low molecular acid and the 1/3-1/2 base oil into a fat preparation kettle for mixing, adding the metered calcium source into the organic acid-base oil mixed material, heating the material to 100-140 ℃ at the speed of 15-30 ℃/min, and carrying out saponification reaction for 1-4 h; adding the rest base oil into a fat preparation kettle for thickening; heating to 200-220deg.C, and refining for 5-10min; quenching to 80-95 ℃ after the reaction is finished; grinding uniformly by a three-roll machine or a high-pressure homogenizer to obtain the basic composite calcium-based lubricating grease.
In the preparation method, the fatty acid comprises 12-hydroxystearic acid or stearic acid; the low molecular acid comprises formic acid, acetic acid or propionic acid; the calcium source comprises calcium hydroxide or calcium oxide; the antioxidant comprises diphenylamine or phenothiazine or 2, 6-di-tert-butyl-p-cresol.
In the preparation method, the base oil is selected from one or more of hydrocarbon base oil, ester base oil and silicone oil base oil.
Further, the hydrocarbon base oil refers to one of PAO series synthetic oil, paraffin base mineral oil, naphthenic base mineral oil and intermediate base mineral oil.
Further, the ester base oil refers to one of a diester oil, a polyol ester oil, a complex ester oil, or a trimellitate oil.
Further, the silicone oil base oil is one of methyl silicone oil, ethyl silicone oil, tolyl silicone oil, or diphenyl silicone oil.
The invention has the following advantages and beneficial effects:
(1) The invention reports the preparation of lubricating grease taking a series of lamellar borophosphate M (H 2O)2[B2P2O8(OH)2]H2 O (wherein M represents Cu/Co/Ni/Mn) as a solid additive for the first time, and develops novel color lubricating grease.
(2) The serial layered borophosphate M (H 2O)2[B2P2O8(OH)2]H2 O (where M stands for Cu/Co/Ni/Mn) material contains lubricating elements such as boron, phosphorus and the like in the molecular composition, so that extreme pressure, bearing, wear resistance and antifriction are effectively improved, and meanwhile, the material has rich and bright color and luster, is added into lubricating grease as a solid additive, and plays roles of a lubricating improver and a dye.
(3) The series of lamellar borophosphate M (H 2O)2[B2P2O8(OH)2]H2 O) (wherein M represents Cu/Co/Ni/Mn) materials in the invention have good compatibility and compatibility with the traditional grease antioxidant.
(4) In the invention, the preparation method of the lubricating grease containing the series of lamellar borophosphate M (H 2O)2[B2P2O8(OH)2]H2 O (wherein M represents Cu/Co/Ni/Mn) as the solid additive is simple, can realize automatic control, has low energy consumption and has wide industrial prospect.
Drawings
FIG. 1 is a graph showing the appearance effect of a grease sample according to examples 1 to 4 of the present invention.
Detailed Description
The present invention is further illustrated by, but not limited to, the following examples.
The lubricating performance in the embodiment of the invention is measured by adopting a four-ball method. According to standard SH/T0204-92, the antifriction and antiwear performance of the obtained lubricating grease sample is tested, and a Xiamen astronomical machine MS-10A four-ball friction and wear testing machine is adopted, wherein the motor rotation speed is 1200+/-50 r/min, the temperature is 75 ℃, the load is 392N, and the time is 60 min. The smaller the plaque diameter (WSD), the better the abrasion resistance; the smaller the coefficient of friction (mu) is, the more effective the reduction of the energy loss due to friction. And (3) testing extreme pressure and bearing performance of the obtained lubricating grease sample according to standard SH/T0202-92, wherein a Xiamen astronomical engine MS-10J four-ball friction and wear testing machine is adopted, the motor rotating speed is 1770+/-50 r/min, the temperature is room temperature, and the time is 10 s. The larger the sintering load (P D), the better the extreme pressure performance; the greater the maximum bite-free load (P B), the better the load-bearing performance.
Example 1
Adding 2.0 g of 12-hydroxystearic acid, 1.0 g g of acetic acid and 32.0 g of PAO10 into a fat preparation kettle, mixing, adding 1.0 g calcium hydroxide into the mixed material, heating the material to 100 ℃ at a speed of 15 ℃/min, and carrying out saponification reaction for about 1 h; adding the rest 64.0 g of PAO10 into a fat-making kettle for thickening; heating to 200deg.C, and refining to 5 min; after the reaction is finished, quenching to 80 ℃, adding 0.01g diphenylamine, stopping stirring, and grinding uniformly by a three-roll grinder to obtain the basic composite calcium-based lubricating grease A.
Raw materials of 0.34 g copper chloride, 0.5g phosphoric acid and 0.3 g boric acid are added into a 30 mL polytetrafluoroethylene stainless steel kettle and reacted in a 15 mL aqueous solution. The reaction is carried out for 0.05 days at the temperature of 250 ℃, and the layered copper borophosphate Cu (H 2O)2[B2P2O8(OH)2]H2 O) is obtained after filtration, washing with distilled water and drying at room temperature.
The layered copper boron phosphate Cu (H 2O)2[B2P2O8(OH)2]H2 O1.0 g and basic composite calcium-based grease A99.0 g are stirred at room temperature for 36. 36H, and are uniformly ground and homogenized by a three-roller mill for 0.1H to obtain the finished composite calcium-based grease, the appearance is shown in figure 1 (a), naphthol green B is added into the basic composite calcium-based grease A in equal proportion as a reference sample, and the lubrication test result data are shown in the following table.
As shown in the table, the lubricating grease taking the layered copper borophosphate as the additive has better extreme pressure, bearing, wear resistance and antifriction performance.
Example 2
Adding 25.0 g stearic acid, 6.0 g formic acid and 30.0 g naphthenic base oil N4010 into a fat-making kettle, mixing, adding 9.0 g calcium oxide into the mixed materials, heating the materials to 140 ℃ at a speed of 30 ℃/min, and carrying out saponification reaction for about 4 h; adding the rest 30.0 g cycloalkyl base oil N4010 into a fat making kettle for thickening; heating to 220 ℃, and refining for 10min; and after the reaction is finished, quenching to 95 ℃, adding 6 g of 2, 6-di-tert-butyl-p-cresol, stopping stirring, and uniformly grinding by a high-pressure homogenizer to obtain the basic composite calcium-based lubricating grease B.
Raw materials of 0.35 g cobalt acetate, 3.32 g trimethyl phosphate and 0.14 g boron oxide are added into a 30 mL polytetrafluoroethylene stainless steel kettle to react in 15 mL water solution. The mixture is reacted for 11 days at 50 ℃, filtered, washed by distilled water and dried at room temperature to obtain the layered cobalt borophosphate Co (H 2O)2[B2P2O8(OH)2]H2 O).
The layered cobalt borophosphate Co (H 2O)2[B2P2O8(OH)2]H2 O10.0 g) and basic composite calcium-based grease B90.0 g are stirred at 280 ℃ for 0.5H, and are uniformly ground and homogenized by a three-roller mill for 5H to obtain the finished composite calcium-based grease, the appearance is shown in the figure 1 (B), sudan III is added into the basic composite calcium-based grease B in a medium proportion as a reference sample, and the lubrication test result data are shown in the following table.
As can be seen from the table, the lubricating grease taking the layered cobalt borophosphate as the additive has better extreme pressure, bearing, wear resistance and antifriction performance.
Example 3
Adding 5.0 g of 12-hydroxystearic acid, 2.0 g propionic acid and 45.0 g dimethyl silicone oil into a fat preparation kettle, mixing, adding 3.0 g calcium hydroxide into the mixed materials, heating the materials to 110 ℃ at a speed of 25 ℃/min, and carrying out saponification reaction for about 2 h; adding the rest 45.0 g dimethyl silicone oil into a fat-making kettle for thickening; heating to 210 ℃, and refining 8 min; after the reaction is finished, quenching to 90 ℃, adding 1.0 g phenothiazine, stopping stirring, and grinding uniformly by a three-roll grinder to obtain the basic composite calcium-based lubricating grease C.
Raw materials of 0.53 g nickel sulfate, 0.91 g tributyl phosphate and 2.56 g boric acid are added into a 30 mL polytetrafluoroethylene stainless steel kettle to react in a5 mL aqueous solution. The reaction is carried out for 8 days at 25 ℃, and the layered nickel boron phosphate Ni (H 2O)2[B2P2O8(OH)2]H2 O) is obtained after filtration, distilled water washing and room temperature drying.
The layered nickel boron phosphate Ni (H 2O)2[B2P2O8(OH)2]H2 O3.0G and basic composite calcium-based grease C97.0G are stirred at 100 ℃ for 10H, and are uniformly ground and homogenized by a homogenizer for 1.5H to obtain the finished composite calcium-based grease, the appearance is shown in the figure 1 (C), pigment yellow G is added into the basic composite calcium-based grease C in a medium proportion as a reference sample, and the lubrication test result data are shown in the following table.
As shown in the table, the lubricating grease taking the layered nickel borophosphate as the additive has better extreme pressure, bearing, wear resistance and antifriction performance.
Example 4
15.0 G stearic acid, 3.0 g acetic acid and 25.0 g pentaerythritol ester are added into a fat manufacturing kettle for mixing, 7.0 g calcium oxide is added into the organic acid-base oil mixed material, the material is heated to 130 ℃ at the speed of 20 ℃/min, and saponification reaction is carried out for about 3 h; adding 50.0 g pentaerythritol ester into a fat manufacturing kettle for thickening; raising the temperature to 205 ℃ and refining 9 min; and after the reaction is finished, quenching to 90 ℃, adding 2.0 g phenothiazine, stopping stirring, and uniformly grinding by a high-pressure homogenizer to obtain the basic composite calcium-based lubricating grease D.
Raw materials of 3.38 g manganese sulfate, 0.78 g boron phosphate and 3.12 g boron oxide are added into a 30 mL polytetrafluoroethylene stainless steel kettle to react in 0.5 mL water. The mixture is reacted for 10 days at 50 ℃, filtered, washed by distilled water and dried at room temperature to obtain the layered manganese borophosphate Mn (H 2O)2[B2P2O8(OH)2]H2 O).
The layered manganese borophosphate Mn (H 2O)2[B2P2O8(OH)2]H2 O2.0 g and basic composite calcium-based grease D98.0 g are stirred and mixed at 50 ℃ for 24H, and homogenized by a three-roll machine for 2H to be uniform, so that the finished composite calcium-based grease is prepared, the appearance is shown in figure 1 (D), cadmium red pigment red 108 is added into the basic composite calcium-based grease D in a medium proportion as a reference sample, and the lubrication test result data are shown in the following table.
As can be seen from the table, the lubricating grease taking the layered manganese borophosphate as the additive has better extreme pressure, bearing, wear resistance and antifriction performance.
Example 5
Adding 5.0 g stearic acid, 2.0 g formic acid and 30.0 g PAO8 into a fat preparation kettle, mixing, adding 1.5g calcium hydroxide into the mixed materials, heating the materials to 110 ℃ at the speed of 20 ℃/min, and carrying out saponification reaction for about 2 h; adding the rest 60.0 g of PAO8 into a fat-making kettle for thickening; raising the temperature to 205 ℃ and refining 6 min; after the reaction is finished, quenching to 85 ℃, adding 0.5 g diphenylamine, stopping stirring, and grinding uniformly by a three-roll grinder to obtain the basic composite calcium-based lubricating grease E.
Raw materials of 0.36 g copper acetate, 1.0 g phosphoric acid and 0.6 g boric acid are added into a 30 mL polytetrafluoroethylene stainless steel kettle to react in a 5 mL aqueous solution. The reaction is carried out for 7 days at 25 ℃, and the layered copper borophosphate Cu (H 2O)2[B2P2O8(OH)2]H2 O) is obtained after filtration, distilled water washing and room temperature drying.
The layered copper borophosphate Cu (H 2O)2[B2P2O8(OH)2]H2 O6.0 g and basic composite calcium-based grease E94.0 g) are stirred at room temperature for 24H, and are uniformly ground and homogenized by a three-roller mill for 2H, so that the finished composite calcium-based grease is prepared.
As shown in the table, the lubricating grease taking the layered copper borophosphate as the additive has better extreme pressure, bearing, wear resistance and antifriction performance.
Example 6
10.0 G of 12-hydroxystearic acid, 3.0 g acetic acid and 25.0 g mineral base oil 100SN are added into a fat-making kettle for mixing, 9.0 g calcium oxide is added into the mixed materials, the materials are heated to 140 ℃ at the speed of 10 ℃/min, and saponification reaction is carried out for about 2 h; adding the rest 50.0 g mineral base oil 100SN into a fat manufacturing kettle for thickening; heating to 210 ℃, and refining to 6 min; after the reaction is finished, quenching to 90 ℃, adding 3g of 2, 6-di-tert-butyl-p-cresol, stopping stirring, and grinding uniformly by a high-pressure homogenizer to obtain the basic composite calcium-based lubricating grease F.
Raw materials of 0.31 g cobalt sulfate, 3.32 g trimethyl phosphate and 0.3 g boric acid are added into a 30 mL polytetrafluoroethylene stainless steel kettle to react in a 10 mL aqueous solution. The mixture is reacted for 1 day at the temperature of 350 ℃, filtered, washed by distilled water and dried at room temperature to obtain the layered cobalt borophosphate Co (H 2O)2[B2P2O8(OH)2]H2 O).
The layered cobalt borophosphate Co (H 2O)2[B2P2O8(OH)2]H2 O7.0 g and the basic composite calcium-based grease F93.0 g are stirred at 80 ℃ for 2.5H and are uniformly ground and homogenized by a three-roll mill for 3H to prepare the finished composite calcium-based grease, iron oxide red Fe 2O3 is added into the basic composite calcium-based grease F in a medium proportion as a reference sample, and the lubrication test result data are shown in the following table.
As can be seen from the table, the lubricating grease taking the layered cobalt borophosphate as the additive has better extreme pressure, bearing, wear resistance and antifriction performance.
Example 7
Adding 5.0 g of 12-hydroxystearic acid, 2.0 g propionic acid, 21.0 g diethyl silicone oil and 21.0 g mineral base oil 100SN into a fat-making kettle, mixing, adding 6.0 g calcium hydroxide into the mixed materials, heating the materials to 125 ℃ at a speed of 20 ℃/min, and carrying out saponification reaction of about 2.5 h; adding the rest 21.0 g diethyl silicone oil and 21.0 g mineral base oil 100SN into a fat-making kettle for thickening; heating to 215 ℃, and refining to 7 min; after the reaction is finished, quenching to 88 ℃, adding 3.0G phenothiazine, stopping stirring, and grinding uniformly by a three-roll grinder to obtain the basic composite calcium-based lubricating grease G.
Raw materials of 0.48 g nickel chloride, 0.91 g tributyl phosphate and 3.12 g boron oxide are added into a 30 mL polytetrafluoroethylene stainless steel kettle to react in a 20mL aqueous solution. The mixture is reacted for 1 day at 300 ℃, filtered, washed by distilled water and dried at room temperature to obtain the layered nickel boron phosphate Ni (H 2O)2[B2P2O8(OH)2]H2 O).
The layered nickel boron phosphate Ni (H 2O)2[B2P2O8(OH)2]H2 OH 1.0G and basic composite calcium-based grease G98.5G are stirred at 100 ℃ for 12H, and are uniformly ground and homogenized by a homogenizer for 1.5H, so that the finished composite calcium-based grease is prepared.
As shown in the table, the lubricating grease taking the layered nickel borophosphate as the additive has better extreme pressure, bearing, wear resistance and antifriction performance.
Example 8
Adding 16.0 g of 12-hydroxystearic acid, 3.0 g acetic acid and 24.0 g phthalic acid ester into a lipid preparation kettle, mixing, adding 5.0 g calcium oxide into the organic acid-base oil mixture, heating the mixture to 135 ℃ at a speed of 25 ℃/min, and carrying out saponification reaction at about 1.5 h; adding 48.0 g phthalate into a fat manufacturing kettle for thickening; heating to 215 ℃, and refining to 6 min; and after the reaction is finished, quenching to 85 ℃, adding 4.0 g diphenylamine, stopping stirring, and uniformly grinding by a high-pressure homogenizer to obtain the basic composite calcium-based lubricating grease H.
Raw materials of 2.7 g manganese acetate, 2.34 g boron phosphate and 1.92 g boric acid are added into a 30 mL polytetrafluoroethylene stainless steel kettle and reacted in 15 mL water. The mixture is reacted for 0.05 days at the temperature of 200 ℃, filtered, washed by distilled water and dried at room temperature to obtain the layered manganese borophosphate Mn (H 2O)2[B2P2O8(OH)2]H2 O).
The layered manganese borophosphate Mn (H 2O)2[B2P2O8(OH)2]H2 O3.0 g) and the basic composite calcium-based grease H97.0 g are stirred and mixed at 50 ℃ for 8H, and homogenized by a three-roll machine for 3H to be uniform, so that the finished composite calcium-based grease is prepared.
As can be seen from the table, the lubricating grease taking the layered manganese borophosphate as the additive has better extreme pressure, bearing, wear resistance and antifriction performance.

Claims (5)

1. The color lubricating grease taking the lamellar borophosphate as the solid additive is characterized by comprising the following raw materials in parts by weight:
90.0 to 99.0 parts of basic composite calcium-based lubricating grease,
1.0-10.0 Parts of solid lubricating additive;
Wherein the solid lubricating additive is lamellar borophosphate M (H 2O)2[B2P2O8(OH)2]H2 O, wherein M represents one of Cu, co, ni, mn metals, namely, lamellar borophosphate is one of Cu(H2O)2[B2P2O8(OH)2]H2O、Co(H2O)2[B2P2O8(OH)2]H2O、Ni(H2O)2[B2P2O8(OH)2]H2O or Mn (H 2O)2[B2P2O8(OH)2]H2 O;
the preparation method of the lamellar borophosphate comprises the steps of reacting raw materials corresponding to a metal source, a phosphorus source and a boron source in an aqueous solution according to a proportion, filtering, washing with distilled water, and drying at room temperature to obtain the lamellar borophosphate;
the metal is copper, and the copper source is one of copper chloride, copper acetate or copper sulfate; the phosphorus source is one of phosphoric acid, trimethyl phosphate, tributyl phosphate or boron phosphate; the boron source is one of boric acid, boron oxide or boron phosphate; the mixture ratio of the raw materials is as follows: the mole ratio of the phosphorus source to the boron source to the copper source to the water is (0.5-10) to 1 to (3-500); the specific reaction process conditions are as follows: the reaction temperature is 25-250 ℃, and the reaction is carried out for 0.05-7 days;
The metal is cobalt, and the cobalt source is one of cobalt chloride, cobalt acetate or cobalt sulfate; the phosphorus source is one of phosphoric acid, trimethyl phosphate, tributyl phosphate or boron phosphate; the boron source is one of boric acid, boron oxide or boron phosphate; the mixture ratio of the raw materials is as follows: the mole ratio of the phosphorus source to the boron source to the cobalt source to the water is (1-12) to 1 to (5-600); the specific reaction process conditions are as follows: the reaction temperature is 50-350 ℃, and the reaction is carried out for 1-11 days;
the metal is nickel, and the nickel source is one of nickel chloride, nickel acetate or nickel sulfate; the phosphorus source is one of phosphoric acid, trimethyl phosphate, tributyl phosphate or boron phosphate; the boron source is one of boric acid, boron oxide or boron phosphate; the mixture ratio of the raw materials is as follows: the mole ratio of the phosphorus source to the boron source to the nickel source to the water is (0.5-8) to 1 to (3-300); the specific reaction process conditions are as follows: the reaction temperature is 25-300 ℃, and the reaction is carried out for 1-8 days;
The metal is manganese, and the manganese source is one of manganese chloride, manganese acetate or manganese sulfate; the phosphorus source is one of phosphoric acid, trimethyl phosphate, tributyl phosphate or boron phosphate; the boron source is one of boric acid, boron oxide or boron phosphate; the mixture ratio of the raw materials is as follows: the mole ratio of the phosphorus source to the boron source to the manganese source to the water is (1.5-12) to 1 to (10-500); the specific reaction process conditions are as follows: the reaction temperature is 50-200 ℃, and the reaction is carried out for 0.05-10 days.
2. A method for preparing a color grease according to claim 1 with a layered borophosphate as a solid additive, characterized by comprising the steps of: mixing the basic composite calcium-based lubricating grease and the lamellar borophosphate for 0.5-36 hours at the temperature of between room temperature and 280 ℃ according to the mass ratio, and grinding and homogenizing for 0.1-5 hours by using a three-roller machine or a high-pressure homogenizer to obtain the color lubricating grease product.
3. The method for preparing the color grease with the layered borophosphate as the solid additive according to claim 2, wherein the method comprises the following steps: the basic composite calcium-based lubricating grease is prepared by mixing and reacting fatty acid, low molecular acid, a calcium source, base oil and an antioxidant raw material, wherein the fatty acid is 2.0-25.0 parts, the low molecular acid is 1.0-6.0 parts, the calcium source is 1.0-9.0 parts, the base oil is 60.0-96.0 parts, and the antioxidant is 0.5-6.0 parts;
The preparation method of the basic composite calcium-based lubricating grease comprises the following steps: adding the metered fatty acid, the low molecular acid and the 1/3-1/2 base oil into a fat preparation kettle for mixing, adding the metered calcium source into the organic acid-base oil mixed material, heating the material to 100-140 ℃ at the speed of 15-30 ℃/min, and carrying out saponification reaction for 1-4 h; adding the rest base oil into a fat preparation kettle for thickening; heating to 200-220deg.C, and refining for 5-10min; quenching to 80-95 ℃ after the reaction is finished; grinding uniformly by a three-roll machine or a high-pressure homogenizer to obtain the basic composite calcium-based lubricating grease.
4. The method for preparing a color grease using a layered borophosphate as a solid additive according to claim 3, wherein: the fatty acid comprises 12-hydroxystearic acid or stearic acid; the low molecular acid comprises formic acid, acetic acid or propionic acid; the calcium source comprises calcium hydroxide or calcium oxide; the antioxidant comprises diphenylamine or phenothiazine or 2, 6-di-tert-butyl-p-cresol; the base oil is selected from one or more of hydrocarbon base oil, ester base oil and silicone oil base oil.
5. The method for preparing the color grease with the layered borophosphate as the solid additive according to claim 4, wherein the method comprises the following steps: the hydrocarbon base oil is one of PAO series synthetic oil, paraffin base mineral oil, naphthenic base mineral oil and intermediate base mineral oil; the ester base oil refers to one of diester oil, polyol ester oil, complex ester oil or trimellitate oil; the silicone oil base oil is one of methyl silicone oil, ethyl silicone oil, toluene silicone oil or diphenyl silicone oil.
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