Interlayer modified zirconium phosphate lubricating grease and preparation method thereof

By introducing zirconium phosphate material modified by decylamine, the problem of insufficient stability and lipophilicity of solid lubricant additives in the grease under high temperature and high load was solved, and a zirconium phosphate grease with excellent anti-wear and friction reduction performance was prepared. It is suitable for Various working conditions.

CN119264967AInactive Publication Date: 2025-01-07SHANDONG HAIHUA GRP CO LTD +1
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Patent Information

Application Number
CN202411788830.5
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2024-12-06
Publication Date
2025-01-07
Estimated Expiration
Not applicable · inactive patent

AI Technical Summary

Technical Problem

Commonly used solid lubricating additives in existing greases such as molybdenum disulfide and graphite are prone to oxidation or electrical corrosion under high temperature and high loads, and the layered zirconium phosphate is poorly lipophilic, resulting in uneven dispersion in greases and local lubricating properties. insufficient.

Method used

Using n-decylamine interlayer modified zirconium phosphate as solid lubricant additive, the lipophilicity of zirconium phosphate is improved by combining with base lithium-based grease and N,N-dise-sec-butyl-p-phenylenediamine, and by hydrothermal The synthesis simplifies the operation steps and prepares interlayer modified zirconium phosphate grease with excellent anti-wear and friction reduction properties.

Benefits of technology

Improve the lipophilicity of zirconium phosphate material, making it evenly dispersed in the grease, significantly enhancing the anti-wear and friction reduction performance of the grease, is suitable for harsh working conditions such as high-speed heavy loads, and is good in different base oils. adaptability.

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Abstract

The invention discloses interlayer modified zirconium phosphate lubricating grease and a preparation method thereof. The lubricating grease is prepared from the following components in percentage by weight: 88 to 92 percent of basic lithium-based lubricating grease, 6 to 10 percent of n-decylamine interlayer modified zirconium phosphate and 2 percent of N, N-di-sec-butyl-p-phenylenediamine. According to the technical scheme, phosphoric acid, zirconium oxychloride octahydrate, distilled water and n-decylamine are stirred and mixed and heated for a hydrothermal synthesis reaction, and the n-decylamine interlayer modified zirconium phosphate material is prepared. The lipophilic n-decylamine is introduced between zirconium phosphate layers, so that the lipophilicity of the zirconium phosphate material is improved. The n-decylamine interlayer modified zirconium phosphate material is used as a solid lubricating additive to prepare the lubricating grease, so that the anti-wear and anti-friction properties of the lubricating grease can be remarkably improved.
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Description

Technical Field

[0001] The invention relates to an interlayer modified zirconium phosphate grease and a preparation method thereof, belonging to the technical field of grease. Background Art

[0002] Grease is a semi-solid substance. Due to its easy addition, long life, strong adhesion and good sealing effect, it is widely used in industrial machinery, transportation, aviation and aerospace, etc., which can effectively reduce the friction and wear between mechanical moving parts. Adding solid lubricant additives to grease can significantly enhance its lubrication performance, protect friction pairs, reduce friction and save energy. Molybdenum disulfide and graphite additives, which are widely used in research and application, have their own defects. For example, molybdenum disulfide is easily oxidized and decomposed under high temperature and high load, and graphite is easy to aggravate the electrical corrosion between friction pairs. In order to adapt to the ever-changing industrial needs, new solid lubricant additives need to be developed to meet the application requirements of various working conditions.

[0003] The structure of layered zirconium phosphate materials consists of horizontally arranged zirconium atoms and PO3(OH) molecular layers on both sides. This layered crystal structure is similar to traditional solid lubricating materials such as molybdenum disulfide and graphite. Layered zirconium phosphate materials have good high temperature stability and chemical stability. Therefore, they have been widely used as solid lubricating additives in recent years. However, layered zirconium phosphate has poor lipophilicity and is unevenly dispersed in grease, which can easily cause insufficient local lubrication performance. Summary of the invention

[0004] The purpose of the present invention is to provide an interlayer modified zirconium phosphate grease and a preparation method thereof. The interlayer modified zirconium phosphate grease prepared by the method has excellent anti-wear and friction-reducing properties.

[0005] In order to achieve the above object, the present invention adopts the following technical solutions: In one aspect, the present invention provides an interlayer modified zirconium phosphate grease, characterized in that it comprises the following components in weight percentage: Basic lithium grease: 88-92%, n-Decylamine interlayer modified zirconium phosphate: 6-10%, N,N-di-sec-butyl-p-phenylenediamine: 2%.

[0006] On the other hand, the present invention provides a method for preparing an interlayer modified zirconium phosphate grease, comprising the following steps: stirring and mixing a basic lithium-based grease and N,N-di-sec-butyl-p-phenylenediamine evenly, and grinding to obtain a lithium-based grease; then adding n-decylamine interlayer modified zirconium phosphate to the lithium-based grease, stirring and mixing evenly, and grinding to obtain an interlayer modified zirconium phosphate grease.

[0007] In the above preparation method, the weight ratio of the basic lithium-based grease, the zirconium phosphate modified by n-decylamine interlayer, and N,N-di-sec-butyl-p-phenylenediamine is 88-92:6-10:2.

[0008] In the above preparation method, the stirring and mixing time of the basic lithium-based grease and N,N-di-sec-butyl-p-phenylenediamine is 3-5 minutes; the stirring and mixing time of the lithium-based grease and the n-decylamine interlayer-modified zirconium phosphate is 5-10 minutes.

[0009] In the above preparation method, the preparation method of the basic lithium-based grease is as follows: pour 1 / 5-2 / 5 of the total amount of the base lubricating oil into a reaction container with a stirrer, start the stirrer, the stirring speed is 100-110rmp, heat to 75-85°C, then add fatty acid, wait for it to be completely dissolved, then add lithium hydroxide solution, control the heating rate to 2-5°C / min to heat to 125-135°C, and carry out saponification reaction for 2-3h; then add 1 / 5-2 / 5 of the base lubricating oil, control the heating rate to 2-5°C / min to heat to 210-220°C, continue for 10-15min, and then stop heating; when the temperature drops to 175-185°C, add the remaining base lubricating oil, when the temperature drops to 90-110°C, stop stirring to obtain a semi-solid fluid, when the temperature drops to room temperature, pour the semi-solid fluid out of the reaction container, and grind to obtain the basic lithium-based grease.

[0010] In the preparation method of the above-mentioned basic lithium-based grease, the base lubricating oil is any one of mineral oil 150BS, polyalphaolefin, cycloalkyl mineral oil or alkyl naphthalene; the fatty acid is 12-hydroxystearic acid; the mass fraction of the lithium hydroxide solution is 40-45wt%; the weight ratio of the base lubricating oil, fatty acid and lithium hydroxide solution is 18-20:2-4:1.

[0011] In the above preparation method, the preparation method of the n-decylamine interlayer modified zirconium phosphate is: phosphoric acid, zirconium oxychloride octahydrate, distilled water, and n-decylamine are stirred and mixed, heated for hydrothermal synthesis reaction to generate a precipitate, and then centrifuged, washed, and dried to obtain the n-decylamine interlayer modified zirconium phosphate.

[0012] In the preparation method of the above-mentioned n-decylamine interlayer modified zirconium phosphate, the molar ratio of the phosphoric acid, zirconium oxychloride octahydrate, distilled water and n-decylamine is 5-10:1-5:90-300:1; the hydrothermal synthesis reaction temperature is 100-300°C, and the reaction time is 12-72h.

[0013] Compared with the prior art, the present invention has the following beneficial effects: (1) The technical solution of the present invention is to prepare a zirconium phosphate material modified by n-decylamine interlayer by stirring and mixing phosphoric acid, zirconium oxychloride octahydrate, distilled water and n-decylamine, and heating to carry out a hydrothermal synthesis reaction. Compared with the prior art, this solution does not require pre-intercalation and simplifies the operation steps.

[0014] (2) The technical solution of the present invention improves the lipophilicity of the zirconium phosphate material by introducing lipophilic n-decylamine into the interlayer of zirconium phosphate. Compared with the prior art, the zirconium phosphate pillared by n-decylamine interlayer is used as a solid lubricant additive to prepare grease. The solid lubricant additive is more evenly dispersed in the grease, and the anti-wear and friction-reducing properties of the grease product are stronger. The material is suitable for harsh working conditions such as high speed and heavy load.

[0015] (3) The n-decylamine interlayer modified zirconium phosphate solid lubricant additive provided by the present invention exhibits good anti-wear and friction-reducing properties in greases with different base oils, has good compatibility with the grease base oil, and can meet different application conditions. DETAILED DESCRIPTION

[0016] The present invention is further illustrated by the following examples, but is not limited to the following examples. Example 1

[0017] Phosphoric acid, zirconium oxychloride octahydrate, distilled water and n-decylamine are added to a polytetrafluoroethylene liner at a molar ratio of 6:2:150:1, and the mixture is stirred and evenly mixed. The polytetrafluoroethylene liner is placed in a reaction kettle and tightened, and then the reaction kettle is placed in an oven for hydrothermal synthesis reaction. The hydrothermal synthesis reaction temperature is controlled to be 180° C. and the reaction is carried out for 36 hours to obtain a precipitate. The precipitate is taken out, centrifuged, washed and dried in sequence to obtain n-decylamine interlayer modified zirconium phosphate, abbreviated as ND-ZrP. Weigh 120g of mineral oil 150BS, first pour 40g of mineral oil 150BS into the fat-making kettle, start the stirrer, stir at a speed of 105rmp, heat to 80°C, add 18.95g of 12-hydroxystearic acid, and after it is completely dissolved, add 6.32g of lithium hydroxide solution (mass fraction is 42wt%), control the heating rate to 2°C / min and heat to 130°C, and carry out saponification reaction for 2.5h; add 40g of mineral oil 150BS, control the heating rate to 2°C / min and heat to 215°C, continue for 12min, and then stop heating; when the temperature drops to 180°C, add 40g of mineral oil 150BS, when the temperature drops to 100°C, stop stirring to obtain a semi-solid fluid, after the temperature drops to room temperature, pour the semi-solid fluid out of the fat-making kettle, roll and grind it 5 times using a three-roll grinder to obtain a basic lithium-based grease; 2 g of N,N-di-sec-butyl-p-phenylenediamine was added to 92 g of basic lithium-based grease, the mixture was mixed and stirred for 4 minutes, and the mixture was rolled and ground for 5 times using a three-roll mill to obtain a lithium-based grease; then 6 g of zirconium phosphate modified with n-decylamine was added to the lithium-based grease, the mixture was mixed and stirred for 8 minutes, and the mixture was rolled and ground for 5 times using a three-roll mill to obtain an interlayer-modified zirconium phosphate grease, which was named 6% ND-ZrP grease (the weight ratio of zirconium phosphate modified with n-decylamine in the product was 6%). Example 2

[0018] Using the n-decylamine interlayer modified zirconium phosphate material prepared in Example 1; The preparation method of basic lithium-based grease is the same as that of Example 1; Add 2g of N,N-di-sec-butyl-p-phenylenediamine to 90g of basic lithium-based grease, mix and stir for 4 minutes, and roll and grind 5 times using a three-roll mill to obtain lithium-based grease; then add 8g of n-decylamine interlayer-modified zirconium phosphate to the lithium-based grease, mix and stir for 8min, and roll and grind 5 times using a three-roll mill to obtain interlayer-modified zirconium phosphate grease, named 8% ND-ZrP grease. Example 3

[0019] Using the n-decylamine interlayer modified zirconium phosphate material prepared in Example 1; The preparation method of basic lithium-based grease is the same as that of Example 1; 2g of N,N-di-sec-butyl-p-phenylenediamine was added to 88g of basic lithium-based grease, the mixture was stirred for 4 minutes, and the mixture was rolled and ground for 5 times using a three-roll mill to obtain a lithium-based grease; then 10g of zirconium phosphate modified by n-decylamine was added to the lithium-based grease, the mixture was stirred for 8 minutes, and the mixture was rolled and ground for 5 times using a three-roll mill to obtain an interlayer-modified zirconium phosphate grease, which was named 10% ND-ZrP grease. Example 4

[0020] Phosphoric acid, zirconium oxychloride octahydrate, distilled water and n-decylamine are added to a polytetrafluoroethylene liner in a molar ratio of 7:2:120:1, and the mixture is stirred and evenly mixed. The polytetrafluoroethylene liner is placed in a reaction kettle and tightened, and then the reaction kettle is placed in an oven for hydrothermal synthesis reaction. The hydrothermal synthesis reaction temperature is controlled to be 150° C. and the reaction is carried out for 24 hours to obtain a precipitate. The precipitate is taken out, centrifuged, washed and dried in sequence to obtain n-decylamine interlayer modified zirconium phosphate; Weigh 120g of polyalphaolefin, first pour 40g of polyalphaolefin into the grease-making kettle, start the agitator, stir at a speed of 105rmp, heat to 80°C, add 18.95g of 12-hydroxystearic acid, and after it is completely dissolved, add 6.32g of lithium hydroxide solution (mass fraction is 41wt%), control the heating rate to 2°C / min and heat to 130°C, and carry out saponification reaction for 2.5h; add 40g of polyalphaolefin, control the heating rate to 2°C / min and heat to 215°C, continue for 12min, and then stop heating; when the temperature drops to 180°C, add 40g of polyalphaolefin, and when the temperature drops to 100°C, stop stirring to obtain a semi-solid fluid. After the temperature drops to room temperature, pour the semi-solid fluid out of the grease-making kettle, roll and grind it 5 times using a three-roll grinder to obtain a basic lithium-based grease; 2 g of N, N-di-sec-butyl-p-phenylenediamine was added to 92 g of basic lithium-based grease, the mixture was stirred for 4 minutes, and the mixture was rolled and ground for 5 times using a three-roll mill to obtain a lithium-based grease; then 6 g of zirconium phosphate modified with n-decylamine was added to the lithium-based grease, the mixture was stirred for 7 minutes, and the mixture was rolled and ground for 5 times using a three-roll mill to obtain an interlayer-modified zirconium phosphate grease, which was named 6% ND-ZrP-4 grease. Example 5

[0021] Phosphoric acid, zirconium oxychloride octahydrate, distilled water and n-decylamine are added to a polytetrafluoroethylene liner at a molar ratio of 8:3:200:1, and the mixture is stirred and evenly mixed. The polytetrafluoroethylene liner is placed in a reaction kettle and tightened, and then the reaction kettle is placed in an oven for hydrothermal synthesis reaction. The hydrothermal synthesis reaction temperature is controlled to be 200° C. and the reaction is carried out for 36 hours to obtain a precipitate. The precipitate is taken out, centrifuged, washed and dried in sequence to obtain n-decylamine interlayer modified zirconium phosphate; Weigh 120g of cycloalkyl mineral oil, first pour 40g of cycloalkyl mineral oil into the fat making kettle, start the agitator, the stirring speed is 105rmp, heat to 80°C, add 18.95g of 12-hydroxystearic acid, and after it is completely dissolved, add 6.32g of lithium hydroxide solution (mass fraction is 43wt%), control the heating rate to 2°C / min and heat to 130°C, and carry out saponification reaction for 2.5h; add 40g of cycloalkyl mineral oil, control the heating rate to 2°C / min and heat to 215°C, after 12min, stop heating; when the temperature drops to 180°C, add 40g of cycloalkyl mineral oil, when the temperature drops to 100°C, stop stirring, and obtain a semi-solid fluid. After the temperature drops to room temperature, pour the semi-solid fluid out of the fat making kettle, roll and grind it 5 times using a three-roll grinder to obtain a basic lithium-based grease; Add 2g of N,N-di-sec-butyl-p-phenylenediamine to 92g of basic lithium-based grease, mix and stir for 4min, and roll and grind 5 times on a three-roll mill to obtain lithium-based grease; then add 6g of n-decylamine interlayer-modified zirconium phosphate to the lithium-based grease, mix and stir for 8min, and roll and grind 5 times on a three-roll mill to obtain interlayer-modified zirconium phosphate grease, named 6% ND-ZrP-5 grease. Example 6

[0022] Phosphoric acid, zirconium oxychloride octahydrate, distilled water and n-decylamine are added to a polytetrafluoroethylene liner in a molar ratio of 9:4:280:1, and the mixture is stirred and evenly mixed. The polytetrafluoroethylene liner is placed in a reaction kettle and tightened, and then the reaction kettle is placed in an oven for hydrothermal synthesis reaction. The hydrothermal synthesis reaction temperature is controlled to be 250° C. and the reaction is carried out for 48 hours to obtain a precipitate. The precipitate is taken out, centrifuged, washed and dried in sequence to obtain n-decylamine interlayer modified zirconium phosphate; Weigh 120g of alkyl naphthalene, first pour 40g of alkyl naphthalene into the fat-making kettle, start the agitator, the stirring speed is 105rmp, heat to 80°C, add 18.95g of 12-hydroxystearic acid, and after it is completely dissolved, add 6.32g of lithium hydroxide solution (mass fraction is 44wt%), control the heating rate to 2°C / min and heat to 130°C, and carry out saponification reaction for 2.5h; add 40g of alkyl naphthalene, control the heating rate to 2°C / min and heat to 215°C, after 12min, stop heating; when the temperature drops to 180°C, add 40g of alkyl naphthalene, when the temperature drops to 100°C, stop stirring, and obtain a semi-solid fluid. After the temperature drops to room temperature, pour the semi-solid fluid out of the fat-making kettle, roll and grind it 5 times using a three-roll grinder to obtain a basic lithium-based grease; Add 2g of N,N-di-sec-butyl-p-phenylenediamine to 92g of basic lithium-based grease, mix and stir for 4min, and roll and grind 5 times using a three-roll mill to obtain lithium-based grease; then add 6g of n-decylamine interlayer-modified zirconium phosphate to the lithium-based grease, mix and stir for 9min, and roll and grind 5 times using a three-roll mill to obtain interlayer-modified zirconium phosphate grease, named 6% ND-ZrP-6 grease. Example 7

[0023] Phosphoric acid, zirconium oxychloride octahydrate, distilled water and n-decylamine are added to a polytetrafluoroethylene liner at a molar ratio of 5:1:90:1, and the mixture is stirred and evenly mixed. The polytetrafluoroethylene liner is placed in a reaction kettle and tightened, and then the reaction kettle is placed in an oven for hydrothermal synthesis reaction. The hydrothermal synthesis reaction temperature is controlled to be 100° C. and the reaction is carried out for 12 hours to obtain a precipitate. The precipitate is taken out, and centrifuged, washed and dried in sequence to obtain n-decylamine interlayer modified zirconium phosphate. Weigh 120g of mineral oil 150BS, first pour 24g of mineral oil 150BS into the fat-making kettle, start the agitator, stir at a speed of 100rmp, heat to 75°C, add 13.33g of 12-hydroxystearic acid, and after it is completely dissolved, add 6.67g of lithium hydroxide solution (mass fraction is 40wt%), control the heating rate to 5°C / min and heat to 125°C, and carry out saponification reaction for 2h; add 24g of mineral oil 150BS, control the heating rate to 5°C / min and heat to 210°C, continue for 10min, and then stop heating; when the temperature drops to 175°C, add 72g of mineral oil 150BS, when the temperature drops to 90°C, stop stirring to obtain a semi-solid fluid, after the temperature drops to room temperature, pour the semi-solid fluid out of the fat-making kettle, roll and grind it 5 times using a three-roll grinder to obtain a basic lithium-based grease; Add 2g of N,N-di-sec-butyl-p-phenylenediamine to 92g of basic lithium-based grease, mix and stir for 3min, and roll and grind 5 times using a three-roll mill to obtain lithium-based grease; then add 6g of n-decylamine interlayer-modified zirconium phosphate to the lithium-based grease, mix and stir for 5min, and roll and grind 5 times using a three-roll mill to obtain an interlayer-modified zirconium phosphate grease, named 6% ND-ZrP-7 grease. Example 8

[0024] Phosphoric acid, zirconium oxychloride octahydrate, distilled water and n-decylamine are added to a polytetrafluoroethylene liner at a molar ratio of 10:5:300:1, and the mixture is stirred and evenly mixed. The polytetrafluoroethylene liner is placed in a reaction kettle and tightened, and the reaction kettle is placed in an oven for hydrothermal synthesis reaction. The hydrothermal synthesis reaction temperature is controlled to be 300° C. and the reaction is carried out for 72 hours to obtain a precipitate. The precipitate is taken out, and centrifuged, washed and dried in sequence to obtain n-decylamine interlayer modified zirconium phosphate. Weigh 120g of mineral oil 150BS, first pour 48g of mineral oil 150BS into the grease making kettle, start the stirrer, stir at a speed of 110rmp, heat to 85°C, add 24g of 12-hydroxystearic acid, and after it is completely dissolved, add 6g of lithium hydroxide solution (mass fraction is 45wt%), control the heating rate to 3°C / min and heat to 135°C, and carry out saponification reaction for 3h; add 48g of mineral oil 150BS, control the heating rate to 3°C / min and heat to 220°C, continue for 15min, and then stop heating; when the temperature drops to 185°C, add 24g of mineral oil 150BS, when the temperature drops to 110°C, stop stirring to obtain a semi-solid fluid, after the temperature drops to room temperature, pour the semi-solid fluid out of the grease making kettle, roll and grind it 5 times using a three-roll grinder to obtain a basic lithium-based grease; 2 g of N, N-di-sec-butyl-p-phenylenediamine was added to 92 g of basic lithium-based grease, the mixture was mixed and stirred for 5 minutes, and the mixture was rolled and ground 5 times using a three-roll mill to obtain a lithium-based grease; then 6 g of zirconium phosphate modified by n-decylamine was added to the lithium-based grease, the mixture was mixed and stirred for 10 minutes, and the mixture was rolled and ground 5 times using a three-roll mill to obtain an interlayer-modified zirconium phosphate grease, which was named 6% ND-ZrP-8 grease.

[0025] Comparative Example 1 (Using Layered Zirconium Phosphate as Solid Lubricant Additive) The preparation method of basic lithium-based grease is the same as that of Example 1; Add 2g of N,N-di-sec-butyl-p-phenylenediamine to 92g of basic lithium-based grease, mix and stir for 4min, and roll and grind 5 times on a three-roll mill to obtain lithium-based grease; then add 6g of layered zirconium phosphate to the lithium-based grease, mix and stir for 8min, and roll and grind 5 times on a three-roll mill to obtain zirconium phosphate grease, named 6% α-ZrP grease.

[0026] This embodiment provides a 6% α-ZrP grease, whose base oil is mineral oil 150BS, for comparison with Example 1.

[0027] Comparative Example 2 (using molybdenum disulfide as a solid lubricant additive) The preparation method of basic lithium-based grease is the same as that of Example 1; Add 2g of N,N-di-sec-butyl-p-phenylenediamine to 92g of basic lithium-based grease, mix and stir for 4min, and roll and grind 5 times on a three-roll mill to obtain lithium-based grease; then add 6g of molybdenum disulfide to the lithium-based grease, mix and stir for 8min, and roll and grind 5 times on a three-roll mill to obtain molybdenum disulfide grease, named 6% MoS2 grease.

[0028] This embodiment provides a 6% MoS2 grease, whose base oil is mineral oil 150BS, in contrast to Example 1. Test example

[0029] The greases prepared in the above embodiments and comparative examples were tested for extreme pressure performance using a four-ball friction and wear tester, and the test method was based on GB / T3142-2019 standard. At the same time, the anti-wear and friction reduction performance of the greases prepared in the above embodiments and comparative examples was tested in accordance with SH / T0204-92 standard. Maximum no-seizure load (P B ), sintering load (P D ) value, the better the extreme pressure bearing performance; the smaller the wear spot diameter (WSD) value, the better the anti-wear performance; the smaller the friction coefficient (μ) value, the better the friction reduction performance. The test results are shown in Table 1 (Table 1 P B , P DThe value is determined by using a step-by-step load level, that is, if the test requirements are not met under a certain load, the test value is a lower level load).

[0030]

[0031] From the lubricating grease lubrication data of Example 1, Comparative Example 1 and Comparative Example 2, it can be seen that after adding ND-ZrP, α-ZrP and MoS2 to the lithium-based grease, the maximum no-seizure load (P B ) is significantly higher than that of 6%α-ZrP grease and 6%MoS2 grease; the sintering load (P D ) is significantly higher than 6% MoS2 grease and comparable to 6% α-ZrP grease. In addition, the wear spot diameter (WSD) and friction coefficient (μ) of 6% ND-ZrP grease are significantly lower than those of 6% α-ZrP grease and 6% MoS2 grease. Compared with the prior art, the technical scheme of the present invention improves the lipophilicity of zirconium phosphate material by introducing lipophilic n-decylamine into the interlayer of zirconium phosphate, and uses the zirconium phosphate material modified by n-decylamine interlayer as a solid lubricating additive to prepare grease, and the obtained grease product has stronger anti-wear and friction reduction properties.

[0032] From the data in Table 1, it can be seen that after adding n-decylamine interlayer modified zirconium phosphate material to lithium grease, the maximum non-seizure load (P B ) and sintering load (P D ) have achieved significant improvements, indicating that the material can significantly enhance the load-bearing capacity of grease; the wear spot diameter (WSD) and friction coefficient (μ) have also been significantly reduced, further confirming the effect of this material in improving anti-wear and friction reduction properties.

[0033] In Example 1 (the base oil is mineral oil 150BS), Example 4 (the base oil is poly-α-olefin), Example 5 (the base oil is cycloalkyl mineral oil), and Example 6 (the base oil is alkyl naphthalene), although the base oils are different, the same amount of zirconium phosphate modified by n-decylamine interlayer is added to the four, and the improvement trend of lubrication performance is basically the same. This shows that the zirconium phosphate solid lubricating additive modified by n-decylamine interlayer exhibits good anti-wear and friction reduction performance in greases with different base oils, has good compatibility with grease base oils, and can meet different application conditions.

[0034] The above embodiments are only used to illustrate the technical solutions of the present invention and do not constitute a limitation thereto. Although these embodiments have been described in detail, it should be understood by those skilled in the art that the technical solutions can still be modified or some or all of the technical features thereof can be replaced by equivalents without departing from the scope of the technical solutions of the present invention. These modifications or replacements do not change the essence of the corresponding technical solutions and still fall within the scope of protection of the present invention.

Claims

1. An interlayer modified zirconium phosphate grease, characterized in that: The composition includes the following weight percentages: Basic lithium grease: 88-92%, n-Decylamine interlayer modified zirconium phosphate: 6-10%, N,N-di-sec-butyl-p-phenylenediamine: 2%.

2. A method for preparing the interlayer modified zirconium phosphate grease according to claim 1, characterized in that: The following steps are involved: The basic lithium-based grease and N,N-di-sec-butyl-p-phenylenediamine are stirred and mixed evenly, and then ground to obtain the lithium-based grease; then the zirconium phosphate modified by n-decylamine is added to the lithium-based grease, stirred and mixed evenly, and then ground to obtain the interlayer-modified zirconium phosphate grease.

3. The preparation method according to claim 2, characterized in that: The weight ratio of the basic lithium-based grease, the zirconium phosphate modified by n-decylamine interlayer, and N,N-di-sec-butyl-p-phenylenediamine is 88-92:6-10:

2.

4. The preparation method according to claim 2, characterized in that: The stirring and mixing time of the basic lithium-based grease and N,N-di-sec-butyl-p-phenylenediamine is 3-5 minutes; the stirring and mixing time of the lithium-based grease and the n-decylamine interlayer-modified zirconium phosphate is 5-10 minutes.

5. The preparation method according to claim 2, characterized in that: The preparation method of the basic lithium-based grease is as follows: pouring 1 / 5-2 / 5 of the total amount of the basic lubricating oil into a reaction container with a stirrer, starting the stirrer at a stirring speed of 100-110 rpm, heating to 75-85° C., adding fatty acid, and waiting for the fatty acid to be completely dissolved, then adding lithium hydroxide solution, controlling the heating rate to 2-5° C. / min, heating to 125-135° C., and performing saponification reaction for 2-3 hours; then adding 1 / 5-2 / 5 of the basic lubricating oil, controlling the heating rate to 2-5° C. / min, heating to 210-220° C., and stopping heating after 10-15 minutes; when the temperature drops to 175-185° C., adding the remaining basic lubricating oil, and when the temperature drops to 90-110° C., stopping stirring to obtain a semi-solid fluid, and when the temperature drops to room temperature, pouring the semi-solid fluid out of the reaction container and grinding it to obtain the basic lithium-based grease.

6. The preparation method according to claim 5, characterized in that: The base lubricant is any one of mineral oil 150BS, polyalphaolefin, cycloalkyl mineral oil and alkyl naphthalene; the fatty acid is 12-hydroxystearic acid; the mass fraction of the lithium hydroxide solution is 40-45wt%; the weight ratio of the base lubricant, fatty acid and lithium hydroxide solution is 18-20:2-4:

1.

7. The preparation method according to claim 2, characterized in that: The preparation method of the n-decylamine interlayer modified zirconium phosphate is as follows: phosphoric acid, zirconium oxychloride octahydrate, distilled water and n-decylamine are stirred and mixed, heated for hydrothermal synthesis reaction to generate a precipitate, and the precipitate is centrifuged, washed and dried to obtain the n-decylamine interlayer modified zirconium phosphate.

8. The preparation method according to claim 7, characterized in that: The molar ratio of phosphoric acid, zirconium oxychloride octahydrate, distilled water and n-decylamine is 5-10:1-5:90-300:1; the hydrothermal synthesis reaction temperature is 100-300° C., and the reaction time is 12-72 hours.

Citation Information

Patent Citations

  • Method for simultaneously and stably dispersing laminated nanosheets and spherical nanoparticles in oily medium and application thereof

    CN104178249A

  • Interlayer pillared N, N'-dimethylpiperazine zirconium phosphate lubricating grease and preparation method thereof

    CN107129851A

  • Lubricating oil antiwear agent, lubricating oil composite agent, lubricating oil and use

    CN107532101A

  • Lubricating grease compound additive and lubricating grease composition prepared from lubricating grease compound additive

    CN114426898A

  • Wear-resistant lubricant and preparation method thereof

    CN118360101A