CN115851346A - Color lubricating grease with layered borophosphate as solid additive and preparation method thereof - Google Patents

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

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CN115851346A
CN115851346A CN202211721218.7A CN202211721218A CN115851346A CN 115851346 A CN115851346 A CN 115851346A CN 202211721218 A CN202211721218 A CN 202211721218A CN 115851346 A CN115851346 A CN 115851346A
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layered
borophosphate
boron
grease
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CN115851346B (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 a color lubricating grease taking layered 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 to 99.0 parts of basic composite calcium-based lubricating grease and 1.0 to 10.0 parts of solid lubricating additive; wherein the solid lubricant additive is a layered borophosphate M (H) 2 O) 2 [B 2 P 2 O 8 (OH) 2 ]H 2 O, wherein M represents one of Cu, co, ni and Mn metals; namely: the layered borophosphate is Cu (H) 2 O) 2 [B 2 P 2 O 8 (OH) 2 ]H 2 O、Co(H 2 O) 2 [B 2 P 2 O 8 (OH) 2 ]H 2 O、Ni(H 2 O) 2 [B 2 P 2 O 8 (OH) 2 ]H 2 O or Mn (H) 2 O) 2 [B 2 P 2 O 8 (OH) 2 ]H 2 And O is one of the compounds. Layered borophosphate M (H) in the present invention 2 O) 2 [B 2 P 2 O 8 (OH) 2 ]H 2 The O material molecule contains lubricating elements such as boron, phosphorus and the like, and can effectively improve the extreme pressure, bearing, wear resistance and antifriction property of the lubricating grease; meanwhile, the material has rich and bright color, is added into lubricating grease as a solid additive, and plays roles of a lubricating improver and a dye.

Description

Color lubricating grease with layered borophosphate as solid additive and preparation method thereof
Technical Field
The invention relates to a composition of a color lubricating grease, in particular to a color lubricating grease with good lubricating property and using layered borophosphate as a solid additive and a preparation method thereof, belonging to the technical field of lubricating grease preparation.
Background
Greases are stable semi-solid or semi-fluid products formed by dispersing a thickener in a liquid lubricant, and have unique rheological properties. Because of the inherent good properties of the lubricating grease, besides the general lubricating action, the extreme pressure, wear resistance, sealing and protecting actions of the lubricating grease are far superior to those of the conventional lubricating oil, so the lubricating grease is widely applied to the moving parts of various industrial machinery such as gears, bearings and the like.
In order to facilitate maintenance when the work is not stopped, 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 lubricating grease is supplied to a required lubricating point through a pipeline by a lubricating grease supply source; meanwhile, the oil quantity of each lubricating point needs to be adjusted, so that the optimal protection effect is achieved. The colored lubricating grease is used, so that whether the lubricating grease is delivered in place or not can be conveniently observed; after the colored grease is used, the condition that oil leakage occurs to the equipment is easier to detect. In addition, in the maintenance of the large-sized motor, whether the lubrication is failed or not is judged by observing the color change degree of the grease discharged from the motor. Traditional color lotionThe grease is generally blended with a specific pigment to prepare a color. Pigment species generally include cadmium Red (CdS nCdS), iron Red (Fe) 2 O 3 ) Inorganic pigments represented by the following 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]. In general, the addition of these pigments only serves for toning in the grease and does not have a lubricating protection effect.
The solid lubricant is an important additive in the lubricating grease, and can play the roles of extreme pressure, bearing, wear resistance, friction reduction and cooperative reinforcement when subjected to harsh operating 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 the lubricating grease. Therefore, new solid lubricant additive materials are continuously developed to meet the requirements of different working conditions.
Disclosure of Invention
The invention aims to provide color lubricating grease with good lubricating performance and using layered borophosphate as a solid additive and a preparation method thereof.
The principle of the invention is as follows: the invention relates to a boron phosphate (M (H) containing layer 2 O) 2 [B 2 P 2 O 8 (OH) 2 ]H 2 O) color grease of, wherein M (H) 2 O) 2 [B 2 P 2 O 8 (OH) 2 ]H 2 O (wherein M represents Cu/Co/Ni/Mn) is a series of layered borophosphate materials, and the molecular composition contains lubricating elements such as boron, phosphorus and the like, so that the extreme pressure, bearing, wear resistance and antifriction properties can be effectively improved; meanwhile, the material has color and good dyeing effect. Layered borophosphate (M (H) 2 O) 2 [B 2 P 2 O 8 (OH) 2 ]H 2 O) is added into the lubricating grease as a solid additive, can simultaneously play the roles of a dye and a lubrication improver, and is added with a necessary antioxidant to prepare the lamellar borophosphate color lubricating grease with good lubricating performance. The invention is a series of layered borophosphate materials (Cu)(H 2 O) 2 [B 2 P 2 O 8 (OH) 2 ]H 2 O、Co(H 2 O) 2 [B 2 P 2 O 8 (OH) 2 ]H 2 O、Ni(H 2 O) 2 [B 2 P 2 O 8 (OH) 2 ]H 2 O and Mn (H) 2 O) 2 [B 2 P 2 O 8 (OH) 2 ]H 2 O) complex calcium based greases as additives were first reported.
The invention provides composite calcium-based lubricating grease taking different layered 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 to 10.0 parts of solid lubricating additive;
wherein the solid lubricant additive is a layered borophosphate M (H) 2 O) 2 [B 2 P 2 O 8 (OH) 2 ]H 2 O (wherein M represents one of Cu, co, ni and Mn metals); namely: cu (H) 2 O) 2 [B 2 P 2 O 8 (OH) 2 ]H 2 O、Co(H 2 O) 2 [B 2 P 2 O 8 (OH) 2 ]H 2 O、Ni(H 2 O) 2 [B 2 P 2 O 8 (OH) 2 ]H 2 O or Mn (H) 2 O) 2 [B 2 P 2 O 8 (OH) 2 ]H 2 And O is one of the compounds.
The preparation method of the layered borophosphate comprises the steps of reacting a metal source, a phosphorus source and a boron source corresponding to raw materials in a water solution according to a certain ratio, filtering, washing with distilled water, and drying at room temperature to obtain the layered borophosphate.
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 raw materials are as follows: the molar 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 to 250 ℃, and the reaction is carried out for 0.05 to 7 days.
Further, the metal is selected from 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 raw materials are proportioned as follows: the molar ratio of the phosphorus source to the boron source to the cobalt source to the water is (1 to 12) to (1 to 5 to 600); the specific reaction process is as follows: the reaction temperature is 50 to 350 ℃, and the reaction is carried out for 1 to 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 raw materials are proportioned as follows: the mol 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 to 300 ℃, and the reaction is carried out for 1 to 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 raw materials are proportioned as follows: the molar ratio of the phosphorus source to the boron source to the manganese source to the water is (1.5-12) to (1-500); the specific reaction process is as follows: the reaction temperature is 50 to 200 ℃, and the reaction is carried out for 0.05 to 10 days.
The invention provides a preparation method of the composite calcium-based lubricating grease with layered borophosphate as a solid additive, which comprises the following steps: mixing the basic composite calcium-based lubricating grease and the layered borophosphate at room temperature to 280 ℃ for 0.5 to 36 hours by stirring according to the mass ratio, and grinding and homogenizing for 0.1 to 5 hours by using a three-roll machine or a high-pressure homogenizer to obtain a composite calcium-based lubricating grease product.
In the preparation method, the basic composite calcium-based lubricating grease is prepared by mixing and reacting raw materials including fatty acid, low-molecular-weight acid, calcium source, base oil and antioxidant, wherein the fatty acid accounts for 2.0 to 25.0 parts, the low-molecular-weight acid accounts for 1.0 to 6.0 parts, the calcium source accounts for 1.0 to 9.0 parts, the base oil accounts for 60.0 to 96.0 parts, and the antioxidant accounts for 0.5 to 6.0 parts;
in the preparation method, the preparation method of the basic composite calcium-based lubricating grease comprises the following steps: adding metered fatty acid, low-molecular acid and 1/3-1/2 base oil into a fat-making kettle for mixing, adding 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 grease making kettle for thickening; heating to 200-220 deg.C, and refining for 5-10min; after the reaction is finished, quenching to 80-95 ℃; grinding by a three-roller machine or uniformly grinding by a high-pressure homogenizer to obtain the basic composite calcium-based lubricating grease.
In the above 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 one or a mixture of a plurality of hydrocarbon base oil, ester base oil and silicone base oil in any ratio.
Further, the hydrocarbon base oil is one of synthetic oils of PAO series, paraffin-based mineral oil, naphthenic-based mineral oil and intermediate-based mineral oil.
Further, the ester base oil refers to one of diester oil, polyol ester oil, complex ester oil, or 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 a series of layered borophosphates M (H) for the first time 2 O) 2 [B 2 P 2 O 8 (OH) 2 ]H 2 Preparation of grease in which O (where M represents Cu/Co/Ni/Mn) was used as a solid additive, a novel colored grease was developed.
(2) The series layered borophosphate M (H) in the invention 2 O) 2 [B 2 P 2 O 8 (OH) 2 ]H 2 The molecular composition of O (wherein M represents Cu/Co/Ni/Mn) material contains lubricating elements such as boron, phosphorus and the like, so that the extreme pressure, bearing, wear resistance and friction reduction are effectively improved; meanwhile, the material has rich and bright color, is added into lubricating grease as a solid additive, and plays roles of a lubricating improver and a dye.
(3) The series layered borophosphate M (H) in the invention 2 O) 2 [B 2 P 2 O 8 (OH) 2 ]H 2 The O (wherein M represents Cu/Co/Ni/Mn) material has good compatibility and compatibility with the traditional grease antioxidant.
(4) The invention contains series of layered boron phosphate M (H) 2 O) 2 [B 2 P 2 O 8 (OH) 2 ]H 2 The preparation method of the lubricating grease with O (wherein M represents Cu/Co/Ni/Mn) as the solid additive is simple, can realize automatic control, and has low energy consumption and wide industrialization prospect.
Drawings
FIG. 1 is a diagram showing the appearance effect of grease samples in examples 1 to 4 of the present invention.
Detailed Description
The present invention is further illustrated by, but is not limited to, the following examples.
The lubricating performance in the examples of the present invention was measured by a four-ball method. According to standard SH/T0204-92, the obtained lubricating grease sample is subjected to antifriction and wear resistance tests by adopting a Xiamen celestial machine MS-10A four-ball friction and wear testing machine and electricityThe rotation speed of the machine is 1200 +/-50 r/min, the temperature is 75 ℃, the load is 392N, and the time is 60 min. The smaller the Wear Scar Diameter (WSD), the better the wear resistance; the smaller the friction coefficient (mu) is, the more effective the energy loss caused by friction can be reduced. And (3) testing the extreme pressure and bearing performance of the obtained lubricating grease sample according to the standard SH/T0202-92, and adopting a Xiamen Tianji MS-10J four-ball friction wear testing machine, wherein the rotating speed of a motor is 1770 +/-50 r/min, the temperature is room temperature, and the time is 10 s. Sintering load (P D ) The larger the size, the better the extreme pressure performance; maximum no bite load: (P B ) Larger indicates better load bearing performance.
Example 1
Adding 2.0 g of 12-hydroxystearic acid, 1.0 g of acetic acid and 32.0 g of PAO10 into a fat making kettle for mixing, adding 1.0 g of calcium hydroxide into the mixed material, heating the mixed material to 100 ℃ at the speed of 15 ℃/min, and carrying out saponification reaction for about 1 h; adding the remaining 64.0 g of PAO10 into a grease making kettle for thickening; heating to 200 deg.C, and refining for 5 min; after the reaction is finished, when the temperature is rapidly cooled to 80 ℃, 0.01 g of diphenylamine is added, the stirring is stopped, and the basic composite calcium-based lubricating grease A is obtained after the mixture is uniformly ground by a three-roller grinder.
A30 mL polytetrafluoroethylene stainless steel vessel was charged with 0.34 g of copper chloride, 0.5 g of phosphoric acid and 0.3 g of boric acid as raw materials, and reacted in 15 mL of an aqueous solution. Reacting at 250 deg.C for 0.05 day, filtering, washing with distilled water, and drying at room temperature to obtain layered copper borophosphate Cu (H) 2 O) 2 [B 2 P 2 O 8 (OH) 2 ]H 2 O。
Selecting layered copper borophosphate Cu (H) 2 O) 2 [B 2 P 2 O 8 (OH) 2 ]H 2 Stirring 1.0 g of O and 99.0 g of basic composite calcium-based lubricating grease A for 36 hours at room temperature, and grinding and homogenizing for 0.1 hour by using a three-roll machine to obtain a finished product composite calcium-based lubricating grease; the appearance is shown in FIG. 1 (a). Naphthol green B is added into the basic composite calcium-based lubricating grease A in equal proportion as a reference sample. The lubrication test results data are shown in the table below.
Figure 274563DEST_PATH_IMAGE002
From the table, the lubricating grease using the layered copper borophosphate as the additive has better extreme pressure, bearing, wear resistance and antifriction properties.
Example 2
Adding 25.0 g of stearic acid, 6.0 g of formic acid and 30.0 g of naphthenic base oil N4010 into a fat making kettle for mixing, adding 9.0 g of calcium oxide into the mixed material, heating the mixed material to 140 ℃ at the speed of 30 ℃/min, and carrying out saponification reaction for about 4 hours; adding the rest 30.0 g of naphthenic base oil N4010 into a grease making kettle for thickening; heating to 220 deg.C, and refining for 10min; 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 using a high-pressure homogenizer to obtain the basic composite calcium-based lubricating grease B.
A30 mL polytetrafluoroethylene stainless steel vessel was charged with 0.35 g of cobalt acetate, 3.32 g of trimethyl phosphate, and 0.14 g of boron oxide as raw materials, and reacted in 15 mL of an aqueous solution. Reacting at 50 deg.C for 11 days, filtering, washing with distilled water, and drying at room temperature to obtain layered cobalt borophosphate Co (H) 2 O) 2 [B 2 P 2 O 8 (OH) 2 ]H 2 O。
Selecting layered cobalt borophosphate Co (H) 2 O) 2 [B 2 P 2 O 8 (OH) 2 ]H 2 Stirring 10.0 g of O and 90.0 g of basic composite calcium-based lubricating grease B for 0.5 h at 280 ℃, and grinding and homogenizing for 5 h by using a three-roller machine to obtain a finished product of composite calcium-based lubricating grease; the appearance is shown in FIG. 1 (b). Sudan III is added into the basic composite calcium-based lubricating grease B in a medium proportion as a reference sample. The lubrication test results are shown in the table below.
Figure 237709DEST_PATH_IMAGE004
As can be seen from the table above, the lubricating grease using the layered cobalt borophosphate as the additive has better extreme pressure, bearing, wear resistance and antifriction properties.
Example 3
Adding 5.0 g of 12-hydroxystearic acid, 2.0 g of propionic acid and 45.0 g of dimethyl silicone oil into a fat making kettle for mixing, adding 3.0 g of calcium hydroxide into the mixed material, heating the mixed material to 110 ℃ at the speed of 25 ℃/min, and performing saponification for about 2 hours; adding the remaining 45.0 g of dimethyl silicone oil into a grease making kettle for thickening; heating to 210 deg.C, and refining for 8 min; after the reaction is finished, when the temperature is rapidly cooled to 90 ℃, 1.0 g of phenothiazine is added, the stirring is stopped, and the basic composite calcium-based lubricating grease C is obtained after the mixture is uniformly ground by a three-roller grinder.
A30 mL polytetrafluoroethylene stainless steel pot was charged with 0.53 g of nickel sulfate, 0.91 g of tributyl phosphate, and 2.56 g of boric acid as starting materials, and reacted in 5 mL of an aqueous solution. Reacting at 25 deg.C for 8 days, filtering, washing with distilled water, and drying at room temperature to obtain layered nickel borophosphate Ni (H) 2 O) 2 [B 2 P 2 O 8 (OH) 2 ]H 2 O。
Selecting layered nickel borophosphate Ni (H) 2 O) 2 [B 2 P 2 O 8 (OH) 2 ]H 2 Stirring 3.0 g of O and 97.0 g of basic composite calcium-based lubricating grease C for 10 hours at the temperature of 100 ℃, and grinding and homogenizing for 1.5 hours by using a homogenizer to obtain a finished product of composite calcium-based lubricating grease; the appearance is shown in FIG. 1 (c). Pigment yellow G is added into the basic composite calcium-based lubricating grease C in a medium proportion to serve as a reference sample. The lubrication test results are shown in the table below.
Figure 361654DEST_PATH_IMAGE006
From the above table, the grease using the layered nickel borophosphate as the additive has better extreme pressure, bearing, wear resistance and antifriction properties.
Example 4
Adding 15.0 g of stearic acid, 3.0 g of acetic acid and 25.0 g of pentaerythritol ester into a fat making kettle for mixing, adding 7.0 g of calcium oxide into the organic acid-base oil mixed material, heating the material to 130 ℃ at the speed of 20 ℃/min, and performing saponification for about 3 hours; adding 50.0 g of pentaerythritol ester into a grease making kettle for thickening; heating to 205 deg.C, and refining for 9 min; after the reaction is finished, quenching to 90 ℃, adding 2.0 g of phenothiazine, stopping stirring, and uniformly grinding by using a high-pressure homogenizer to obtain the basic composite calcium-based lubricating grease D.
A30 mL polytetrafluoroethylene stainless steel kettle was charged with the starting materials 3.38 g manganese sulfate, 0.78 g boron phosphate and 3.12 g boron oxide, and reacted in 0.5 mL water. Reacting at 50 deg.C for 10 days, filtering, washing with distilled water, and drying at room temperature to obtain layered manganese borophosphate (Mn) (H) 2 O) 2 [B 2 P 2 O 8 (OH) 2 ]H 2 O。
Selecting layered manganese borophosphate Mn (H) 2 O) 2 [B 2 P 2 O 8 (OH) 2 ]H 2 Stirring and mixing 2.0 g of O and 98.0 g of basic composite calcium-based lubricating grease D for 24 hours at the temperature of 50 ℃, and homogenizing for 2 hours by using a three-roller machine to obtain finished composite calcium-based lubricating grease; the appearance is shown in FIG. 1 (d). Cadmium red pigment red 108 was added to the basic composite calcium grease D in a medium proportion as a reference. The lubrication test results are shown in the table below.
Figure DEST_PATH_IMAGE008
From the table, the lubricating grease using the layered manganese borophosphate as the additive has better extreme pressure, bearing, wear resistance and antifriction properties.
Example 5
Adding 5.0 g of stearic acid, 2.0 g of formic acid and 30.0 g of PAO8 into a fat making kettle for mixing, adding 1.5g of calcium hydroxide into the mixed material, heating the mixed material to 110 ℃ at the speed of 20 ℃/min, and carrying out saponification for about 2 hours; adding the remaining 60.0 g of PAO8 into a grease making kettle for thickening; heating to 205 deg.C, and refining for 6 min; after the reaction is finished, when the temperature is rapidly cooled to 85 ℃, 0.5 g of diphenylamine is added, the stirring is stopped, and the basic composite calcium-based lubricating grease E is obtained after the mixture is uniformly ground by a three-roller grinder.
At 30A mL polytetrafluoroethylene stainless steel vessel was charged with raw materials of 0.36 g of copper acetate, 1.0 g of phosphoric acid and 0.6 g of boric acid, and reacted in 5 mL of an aqueous solution. Reacting at 25 deg.C for 7 days, filtering, washing with distilled water, and drying at room temperature to obtain layered copper borophosphate Cu (H) 2 O) 2 [B 2 P 2 O 8 (OH) 2 ]H 2 O。
Selecting layered copper borophosphate Cu (H) 2 O) 2 [B 2 P 2 O 8 (OH) 2 ]H 2 Stirring 6.0 g of O and 94.0 g of basic composite calcium-based lubricating grease E for 24 hours at room temperature, and grinding and homogenizing for 2 hours by using a three-roller machine to obtain the finished product composite calcium-based lubricating grease. Naphthol green B is added into the basic composite calcium-based lubricating grease E in a medium proportion to serve as a reference sample. The lubrication test results are shown in the table below.
Figure DEST_PATH_IMAGE010
From the table, the lubricating grease using the layered copper borophosphate as the additive has better extreme pressure, bearing, wear resistance and antifriction properties.
Example 6
Adding 10.0 g of 12-hydroxystearic acid, 3.0 g of acetic acid and 25.0 g of mineral base oil 100SN into a grease making kettle for mixing, adding 9.0 g of calcium oxide into the mixed material, heating the material to 140 ℃ at the speed of 10 ℃/min, and carrying out saponification for about 2 hours; adding the rest 50.0 g of mineral base oil 100SN into a grease making kettle for thickening; heating to 210 deg.C, and refining for 6 min; after the reaction is finished, quenching to 90 ℃, adding 3 g of 2, 6-di-tert-butyl-p-cresol, stopping stirring, and grinding uniformly by using a high-pressure homogenizer to obtain the basic composite calcium-based lubricating grease F.
A30 mL polytetrafluoroethylene stainless steel vessel was charged with 0.31 g of cobalt sulfate, 3.32 g of trimethyl phosphate, and 0.3 g of boric acid as raw materials, and reacted in 10 mL of an aqueous solution. Reacting at 350 deg.C for 1 day, filtering, washing with distilled water, and drying at room temperature to obtain layered cobalt borophosphate Co (H) 2 O) 2 [B 2 P 2 O 8 (OH) 2 ]H 2 O。
Selecting layered cobalt borophosphate Co (H) 2 O) 2 [B 2 P 2 O 8 (OH) 2 ]H 2 Stirring 7.0 g of O and 93.0 g of basic composite calcium-based lubricating grease F for 2.5 hours at the temperature of 80 ℃, and grinding and homogenizing for 3 hours by using a three-roll machine to obtain the finished product composite calcium-based lubricating grease. Adding iron oxide red Fe into basic composite calcium-based lubricating grease F in a medium proportion 2 O 3 As a reference. The lubrication test results are shown in the table below.
Figure DEST_PATH_IMAGE012
From the above table, the grease using the layered cobalt borophosphate as the additive has better extreme pressure, bearing, wear resistance and antifriction properties.
Example 7
Adding 5.0 g of 12-hydroxystearic acid, 2.0 g of propionic acid, 21.0 g of diethyl silicone oil and 21.0 g of mineral base oil 100SN into a grease making kettle for mixing, adding 6.0 g of calcium hydroxide into the mixed material, heating the material to 125 ℃ at the speed of 20 ℃/min, and carrying out saponification for about 2.5 hours; adding the rest 21.0 g of diethyl silicone oil and 21.0 g of mineral base oil 100SN into a grease making kettle for thickening; heating to 215 deg.C, and refining for 7 min; after the reaction is finished, when the temperature is rapidly cooled to 88 ℃, 3.0G of phenothiazine is added, the stirring is stopped, and the basic composite calcium-based lubricating grease G is obtained after the mixture is uniformly ground by a three-roller grinder.
A30 mL polytetrafluoroethylene stainless steel vessel was charged with 0.48 g of nickel chloride, 0.91 g of tributyl phosphate and 3.12 g of boron oxide, and reacted in 20 mL of an aqueous solution. Reacting at 300 deg.C for 1 day, filtering, washing with distilled water, and drying at room temperature to obtain layered nickel borophosphate Ni (H) 2 O) 2 [B 2 P 2 O 8 (OH) 2 ]H 2 O。
Selecting layered nickel borophosphate Ni (H) 2 O) 2 [B 2 P 2 O 8 (OH) 2 ]H 2 OH 1.0G and basic composite calcium base grease G98.5GStirring for 12 h at 100 ℃, and grinding and homogenizing for 1.5 h by a homogenizer to obtain the finished product of the composite calcium-based lubricating grease. Oil-soluble orange 60 was added to the basic composite calcium-based grease G in a moderate proportion as a reference. The lubrication test results data are shown in the table below.
Figure DEST_PATH_IMAGE014
From the above table, the grease using the layered nickel borophosphate as the additive has better extreme pressure, bearing, wear resistance and antifriction properties.
Example 8
Adding 16.0 g 12-hydroxystearic acid, 3.0 g acetic acid and 24.0 g phthalic acid ester into a grease kettle, mixing, adding 5.0 g calcium oxide into the above organic acid-base oil mixture, heating to 135 deg.C at a rate of 25 deg.C/min, and performing saponification for about 1.5 h; adding 48.0 g of phthalic acid ester into a grease making kettle for thickening; heating to 215 deg.C, and refining for 6 min; after the reaction is finished, quenching to 85 ℃, adding 4.0 g of diphenylamine, stopping stirring, and uniformly grinding by using a high-pressure homogenizer to obtain the basic composite calcium-based lubricating grease H.
A30 mL polytetrafluoroethylene stainless steel kettle was charged with 2.7 g of manganese acetate, 2.34 g of boron phosphate, and 1.92 g of boric acid as starting materials, and reacted in 15 mL of water. Reacting at 200 deg.C for 0.05 days, filtering, washing with distilled water, and drying at room temperature to obtain layered manganese borophosphate Mn (H) 2 O) 2 [B 2 P 2 O 8 (OH) 2 ]H 2 O。
Selecting layered manganese borophosphate Mn (H) 2 O) 2 [B 2 P 2 O 8 (OH) 2 ]H 2 Stirring and mixing 3.0 g of O and 97.0 g of basic composite calcium-based lubricating grease H for 8 hours at the temperature of 50 ℃, and homogenizing for 3 hours by using a three-roller machine to obtain the finished product composite calcium-based lubricating grease. Cadmium red pigment red 108 was added to the basic composite calcium grease H in a moderate proportion as a reference. The lubrication test results are shown in the table below.
Figure DEST_PATH_IMAGE016
From the table, the lubricating grease using the layered manganese borophosphate as the additive has better extreme pressure, bearing, wear resistance and antifriction properties.

Claims (10)

1. The color lubricating grease taking layered borophosphate as a 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 to 10.0 parts of solid lubricating additive;
wherein the solid lubricant additive is a layered borophosphate M (H) 2 O) 2 [B 2 P 2 O 8 (OH) 2 ]H 2 O, wherein M represents one of Cu, co, ni and Mn metals; namely: the layered borophosphate is Cu (H) 2 O) 2 [B 2 P 2 O 8 (OH) 2 ]H 2 O、Co(H 2 O) 2 [B 2 P 2 O 8 (OH) 2 ]H 2 O、Ni(H 2 O) 2 [B 2 P 2 O 8 (OH) 2 ]H 2 O or Mn (H) 2 O) 2 [B 2 P 2 O 8 (OH) 2 ]H 2 And O is one of the compounds.
2. A colored grease with layered borophosphate as a solid additive according to claim 1, characterized in that: the preparation method of the layered borophosphate comprises the steps of reacting a metal source, a phosphorus source and a boron source corresponding to raw materials in a water solution according to a ratio, filtering, washing with distilled water, and drying at room temperature to obtain the layered borophosphate.
3. A colored grease with layered borophosphate as a solid additive according to claim 2, characterized in that: 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 raw materials are proportioned as follows: the molar 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 to 250 ℃, and the reaction is carried out for 0.05 to 7 days.
4. A colour grease with layered borophosphate as solid additive according to claim 2, characterised in that: the metal is selected from 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 raw materials are proportioned as follows: the mol ratio of the phosphorus source to the boron source to the cobalt source to the water is (1 to 12) to (1 to 1) to (5 to 600); the specific reaction process conditions are as follows: the reaction temperature is 50 to 350 ℃, and the reaction is carried out for 1 to 11 days.
5. A colored grease with layered borophosphate as a solid additive according to claim 2, characterized in that: the metal is selected from 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 raw materials are proportioned as follows: the molar ratio of the phosphorus source to the boron source to the nickel source to the water is (0.5-8) to (1-300); the specific reaction process conditions are as follows: the reaction temperature is 25 to 300 ℃, and the reaction is carried out for 1 to 8 days.
6. A colored grease with layered borophosphate as a solid additive according to claim 2, characterized in that: 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 raw materials are proportioned as follows: the molar ratio of the phosphorus source to the boron source to the manganese source to the water is (1.5-12) to (1-500); the specific reaction process conditions are as follows: the reaction temperature is 50 to 200 ℃, and the reaction is carried out for 0.05 to 10 days.
7. A method for preparing the color grease with the layered borophosphate as the solid additive according to any one of claims 1 to 6, which is characterized by comprising the following steps: stirring and mixing the basic composite calcium-based lubricating grease and the layered boron phosphate at room temperature to 280 ℃ for 0.5 to 36 hours according to the mass ratio, and grinding and homogenizing for 0.1 to 5 hours by using a three-roll machine or a high-pressure homogenizer to obtain a color lubricating grease product.
8. The method for preparing a color grease with layered borophosphate as solid additive according to claim 7, characterized in that: the basic composite calcium-based lubricating grease is formed by mixing and reacting 2.0 to 25.0 parts of fatty acid, 1.0 to 6.0 parts of low molecular acid, 1.0 to 9.0 parts of calcium source, 60.0 to 96.0 parts of base oil and 0.5 to 6.0 parts of antioxidant;
the preparation method of the basic composite calcium-based lubricating grease comprises the following steps: adding metered fatty acid, low-molecular acid and 1/3-1/2 base oil into a fat-making kettle for mixing, adding 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 grease making kettle for thickening; heating to 200-220 deg.C, and refining for 5-10min; after the reaction is finished, quenching to 80-95 ℃; grinding by a three-roller machine or uniformly grinding by a high-pressure homogenizer to obtain the basic composite calcium-based lubricating grease.
9. The method for preparing a color grease with layered borophosphate as solid additive according to claim 8, wherein the method comprises the following steps: 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 one or a mixture of a plurality of hydrocarbon base oil, ester base oil and silicone base oil in any ratio.
10. The method for preparing a color grease with layered borophosphate as a solid additive according to claim 9, 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 is one of diester oil, polyol ester oil, double ester oil or trimellitate oil; the silicone oil base oil is one of methyl silicone oil, ethyl silicone oil, tolyl silicone oil or diphenyl silicone oil.
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