Composite calcium-based lubricating grease and preparation method thereof

Abstract

The invention discloses composite calcium-based lubricating grease and a preparation method thereof. The lubricating grease comprises the following components in percentage by weight: 90-94% of basic composite calcium-based lubricating grease, 5-9% of decyltrimethylammonium chloride modified zirconium phosphate and 1% of dinonyl diphenylamine. The preparation method comprises the following steps: mixing and heating phosphoric acid, zirconium oxychloride octahydrate, methanol and decyltrimethylammonium chloride, carrying out a synthetic reaction to prepare decyltrimethylammonium chloride modified zirconium phosphate, and preparing the composite calcium-based lubricating grease by taking the modified zirconium phosphate as a solid additive. The lubricating grease disclosed by the invention is simple and convenient in preparation method and good in stability, and due to the fact that the lubricating grease contains the decyltrimethylammonium chloride modified zirconium phosphate material, the extreme pressure and anti-wear and anti-friction properties of the lubricating grease are remarkably enhanced.

Description

Technical Field

[0001] The invention relates to a composite calcium-based grease and a preparation method thereof, belonging to the technical field of grease. Background Art

[0002] Complex calcium-based grease is a grease with complex calcium soap as thickener, which is generated by the reaction of low molecular weight acid and high molecular weight acid with calcium hydroxide. Its lubrication performance is closely related to the uniform dispersion of internal soap fibers in the base oil. This grease has good water washing resistance and mechanical stability, and is widely used in various mechanical equipment and industrial fields. However, with the development of industrial technology and the complexity of equipment operating conditions, higher requirements are placed on complex calcium-based grease, especially when used under harsh conditions such as high temperature and high load. Simple complex calcium-based grease can no longer fully meet these requirements.

[0003] In order to improve the lubrication performance of complex calcium-based grease, various solid additives can be added. These solid additives can form a dispersed phase in the grease and improve the extreme pressure and anti-wear and friction reduction properties of the grease. At present, common solid additives include molybdenum disulfide and graphite. However, these traditional solid additives still have some problems in practical applications, such as insufficient stability and easy oxidation.

[0004] Layered zirconium phosphate is a new type of inorganic functional material. Its unique layered structure is easy to modify the surface and has excellent chemical stability. Due to the low shear strength between its adjacent layers, layered zirconium phosphate can significantly enhance the extreme pressure and anti-wear and friction reduction properties of grease, so it is suitable as a solid additive for grease. However, this material does not contain lipophilic groups and has poor dispersibility in grease, which affects its lubrication performance. Summary of the invention

[0005] The purpose of the present invention is to provide a composite calcium-based grease and a preparation method thereof, wherein the obtained grease has good extreme pressure and anti-wear and friction-reducing properties.

[0006] In order to solve the above technical problems, the present invention adopts the following technical solutions: The present invention provides a composite calcium-based lubricating grease, characterized in that it comprises the following components in percentage by weight: Basic complex calcium-based grease: 90-94%, Zirconium phosphate modified with decanyltrimethylammonium chloride: 5-9%, Dinonyldiphenylamine: 1%.

[0007] The present invention provides a method for preparing a composite calcium-based lubricating grease, which is characterized by comprising the following steps: The basic composite calcium-based grease, zirconium phosphate modified with decanyltrimethylammonium chloride, and dinonyldiphenylamine are stirred and mixed uniformly and ground to obtain the composite calcium-based grease.

[0008] In the above preparation method, the weight ratio of the basic composite calcium-based grease, the zirconium phosphate modified by decanyltrimethylammonium chloride, and the dinonyldiphenylamine is 90-94:5-9:1.

[0009] In the above preparation method, the preparation method of the basic composite calcium-based grease is as follows: 1 / 3-2 / 3 of the total amount of the base lubricating oil is mixed with calcium hydroxide and poured into a reaction container, heated and stirred at a stirring speed of 70-80 rpm, when the temperature in the reaction container rises to 35°C-45°C, acetic acid is added, and the mixture is kept warm for 30-60 minutes to carry out a saponification reaction; after the reaction is completed, the temperature in the reaction container is heated to 75-85°C, dodecyl hydroxystearic acid is added, and the mixture is kept warm for 60-90 minutes to carry out a saponification reaction; after the reaction is completed, 1 / 5 of the total amount of the base lubricating oil is added to the reaction container, and the mixture is continued to be heated to 200-220°C and kept warm for 10-15 minutes; then the heating is stopped; when the temperature in the reaction container drops to 115-125°C, the remaining base lubricating oil is added, and when the temperature in the reaction container drops to 95-105°C, the stirring is stopped, and after the temperature drops to room temperature, a semi-solid fluid is obtained; the semi-solid fluid is ground to obtain the basic composite calcium-based grease.

[0010] In the preparation method of the above-mentioned basic composite calcium-based grease, the base lubricating oil is any one of polyalphaolefin, paraffin-based mineral oil, soybean oil or pentaerythritol ester; the weight ratio of calcium hydroxide, base lubricating oil, acetic acid and dodecyl hydroxystearic acid is 1-1.5:24-26:1:3-4.

[0011] In the above preparation method, the preparation method of the decanyltrimethylammonium chloride modified zirconium phosphate is: phosphoric acid, zirconium oxychloride octahydrate, methanol, and decanyltrimethylammonium chloride are stirred and mixed, heated for synthesis reaction to generate a suspension, and then centrifuged, washed, and dried to obtain decanyltrimethylammonium chloride modified zirconium phosphate.

[0012] In the preparation method of the above-mentioned decanyltrimethylammonium chloride-modified zirconium phosphate, the molar ratio of the phosphoric acid, zirconium oxychloride octahydrate, methanol, and decanyltrimethylammonium chloride is 8-13:1:180-230:1-2; the synthesis reaction temperature is 80-130°C, and the reaction time is 10-35h.

[0013] The beneficial effects of the present invention are as follows: (1) The present invention introduces lipophilic decanyltrimethylammonium chloride between the layered zirconium phosphate layers for functional modification. Compared with the prior art, the zirconium phosphate modified with decanyltrimethylammonium chloride is used as a solid lubricating additive to prepare grease, which is more evenly dispersed in the grease. The obtained grease product has stronger extreme pressure and anti-wear and friction-reducing properties and can meet more application conditions.

[0014] (2) The present invention prepares a modified zirconium phosphate material by mixing and heating phosphoric acid, zirconium oxychloride octahydrate, methanol, and decanyltrimethylammonium chloride to carry out a synthesis reaction. When the molar ratio of the above raw materials is controlled to be 8-13:1:180-230:1-2, the prepared modified zirconium phosphate material still retains the original layered structure of zirconium phosphate, and can effectively improve the lubrication performance of grease products.

[0015] (3) In the preparation process of the basic composite calcium-based grease of the present invention, the base oil is added step by step, so that the soap fibers can be more stably dispersed in the base oil, thereby improving the lubrication performance.

[0016] (4) The present invention prepares a composite calcium-based grease with good extreme pressure and anti-wear and friction-reducing properties by adjusting the ratio of basic composite calcium-based grease, zirconium phosphate modified with decanyltrimethylammonium chloride, and dinonyldiphenylamine. The preparation method of the grease is simple and easy to industrialize. BRIEF DESCRIPTION OF THE DRAWINGS

[0017] Figure 1 It is the SEM spectrum of the zirconium phosphate material modified with dodecyltrimethylammonium chloride obtained in Example 1 and Comparative Example 3.

[0018] Figure 2 1 is the XRD spectrum of the zirconium phosphate material modified with decanyltrimethylammonium chloride obtained in Example 1 and Comparative Example 3. DETAILED DESCRIPTION

[0019] The present invention will be further explained by the following examples, but the present invention is not limited to these examples. Example 1

[0020] Phosphoric acid, zirconium oxychloride octahydrate, methanol, and decanyltrimethylammonium chloride are added to a polytetrafluoroethylene liner at a molar ratio of 9:1:190:1.5, 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 heating and synthesis reaction. The synthesis reaction temperature is controlled to be 110° C. and the reaction is carried out for 30 hours to generate a suspension. The suspension is taken out, and then centrifuged, washed, and dried to obtain decanyltrimethylammonium chloride-modified zirconium phosphate, abbreviated as DC-ZrP. Weigh 120g of polyalphaolefin, first mix 65g of polyalphaolefin and 5.76g of calcium hydroxide, pour into the fat making kettle, heat and stir, the stirring speed is 75rmp, when the temperature in the fat making kettle rises to 40°C, add 4.8g of acetic acid, and keep warm for 50min to carry out saponification reaction; after the reaction is completed, heat the temperature in the fat making kettle to 80°C, add 16.8g of dodecyl hydroxystearic acid, and keep warm for 80min to carry out saponification reaction; after the reaction is completed, add 24g of polyalphaolefin, continue to heat to 215°C, keep warm for 14min, and then stop heating; when the temperature in the fat making kettle drops to 120°C, add 31g of polyalphaolefin, when the temperature in the fat making kettle drops to 100°C, stop stirring, and after the temperature drops to room temperature, a semi-solid fluid is obtained; roll and grind 5 times using a three-roll grinder to obtain a basic composite calcium-based grease; 5 g of zirconium phosphate modified with decantrimethylammonium chloride and 1 g of dinonyldiphenylamine were added in sequence to 94 g of basic composite calcium-based grease, the mixture was stirred for 7 minutes, and the mixture was rolled and ground 5 times using a three-roll mill to obtain a composite calcium-based grease with modified layered zirconium phosphate as a solid lubricating additive. The composition of the grease is as follows: basic composite calcium-based grease: 94%; zirconium phosphate modified with decantrimethylammonium chloride: 5%; dinonyldiphenylamine: 1%, named 5% DC-ZrP grease. Example 2

[0021] Using the zirconium phosphate modified with the decanyltrimethylammonium chloride prepared in Example 1; The preparation method of basic composite calcium-based grease is the same as that of Example 1; 7g of zirconium phosphate modified with decantrimethylammonium chloride and 1g of dinonyldiphenylamine were added in sequence to 92g of basic composite calcium-based grease, the mixture was stirred for 7 minutes, and the mixture was rolled and ground 5 times on a three-roll mill to obtain a composite calcium-based grease with modified layered zirconium phosphate as a solid lubricating additive. The components of the grease are: basic composite calcium-based grease: 92%; zirconium phosphate modified with decantrimethylammonium chloride: 7%; and dinonyldiphenylamine: 1%. The grease was named 7%DC-ZrP grease. Example 3

[0022] Using the zirconium phosphate modified with the decanyltrimethylammonium chloride prepared in Example 1; The preparation method of basic composite calcium-based grease is the same as that of Example 1; 9g of zirconium phosphate modified with decantrimethylammonium chloride and 1g of dinonyldiphenylamine were added in sequence to 90g of basic composite calcium-based grease, the mixture was stirred for 7 minutes, and the mixture was rolled and ground 5 times using a three-roll mill to obtain a composite calcium-based grease with modified layered zirconium phosphate as a solid lubricating additive. The components of the grease are: basic composite calcium-based grease: 90%; zirconium phosphate modified with decantrimethylammonium chloride: 9%; and dinonyldiphenylamine: 1%. The grease was named 9%DC-ZrP grease. Example 4

[0023] Phosphoric acid, zirconium oxychloride octahydrate, methanol, and decanyltrimethylammonium chloride are added to a polytetrafluoroethylene liner at a molar ratio of 10:1:200:1.3, 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 heating and synthesis reaction. The synthesis reaction temperature is controlled to be 90° C. and the reaction is carried out for 15 hours to generate a suspension. The suspension is taken out, and then centrifuged, washed, and dried to obtain decanyltrimethylammonium chloride-modified zirconium phosphate; Weigh 120g of paraffin-based mineral oil, first mix 65g of paraffin-based mineral oil and 5.76g of calcium hydroxide, pour them into the fat-making kettle, heat and stir, the stirring speed is 75rmp, when the temperature in the fat-making kettle rises to 40°C, add 4.8g of acetic acid, and keep warm for 50min to carry out saponification reaction; after the reaction is completed, heat the temperature in the fat-making kettle to 80°C, add 16.8g of dodecyl hydroxystearic acid, and keep warm for 80min to carry out saponification reaction; after the reaction is completed, add 24g of paraffin-based mineral oil, continue to heat to 215°C, keep warm for 14min, and then stop heating; when the temperature in the fat-making kettle drops to 120°C, add 31g of paraffin-based mineral oil, when the temperature in the fat-making kettle drops to 100°C, stop stirring, and after the temperature drops to room temperature, a semi-solid fluid is obtained; roll and grind 5 times using a three-roll grinder to obtain a basic composite calcium-based grease; 5 g of zirconium phosphate modified with decantrimethylammonium chloride and 1 g of dinonyldiphenylamine were added to 94 g of basic composite calcium-based grease in sequence, the mixture was stirred for 7 minutes, and the mixture was rolled and ground 5 times using a three-roll mill to obtain a composite calcium-based grease with modified layered zirconium phosphate as a solid lubricating additive. The composition of the grease is as follows: basic composite calcium-based grease: 94%; zirconium phosphate modified with decantrimethylammonium chloride: 5%; dinonyldiphenylamine: 1%, named 5%DC-ZrP-4 grease. Example 5

[0024] Phosphoric acid, zirconium oxychloride octahydrate, methanol, and decanyltrimethylammonium chloride are added to a polytetrafluoroethylene liner at a molar ratio of 11:1:210:1.7, 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 heating and synthesis reaction. The synthesis reaction temperature is controlled to be 100° C. and the reaction is carried out for 20 hours to generate a suspension. The suspension is taken out, and then centrifuged, washed, and dried to obtain decanyltrimethylammonium chloride-modified zirconium phosphate; Weigh 120g soybean oil, first mix 65g soybean oil and 5.76g calcium hydroxide, pour into the fat making kettle, heat and stir, the stirring speed is 75rmp, when the temperature in the fat making kettle rises to 40°C, add 4.8g acetic acid, and keep warm for 50min to carry out saponification reaction; after the reaction is completed, heat the temperature in the fat making kettle to 80°C, add 16.8g dodecyl hydroxystearic acid, and keep warm for 80min to carry out saponification reaction; after the reaction is completed, add 24g soybean oil, continue to heat to 215°C, keep warm for 14min, and then stop heating; when the temperature in the fat making kettle drops to 120°C, add 31g soybean oil, when the temperature in the fat making kettle drops to 100°C, stop stirring, and after the temperature drops to room temperature, a semi-solid fluid is obtained; roll and grind 5 times using a three-roll grinder to obtain a basic composite calcium-based grease; 5 g of zirconium phosphate modified with decantrimethylammonium chloride and 1 g of dinonyldiphenylamine were added in sequence to 94 g of basic composite calcium-based grease, the mixture was stirred for 7 minutes, and the mixture was rolled and ground 5 times using a three-roll mill to obtain a composite calcium-based grease with modified layered zirconium phosphate as a solid lubricating additive. The composition of the grease is as follows: basic composite calcium-based grease: 94%; zirconium phosphate modified with decantrimethylammonium chloride: 5%; dinonyldiphenylamine: 1%, named 5%DC-ZrP-5 grease. Example 6

[0025] Phosphoric acid, zirconium oxychloride octahydrate, methanol, and decanyltrimethylammonium chloride are added to a polytetrafluoroethylene liner at a molar ratio of 12:1:220:1.9, 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 heating synthesis reaction. The synthesis reaction temperature is controlled to be 120° C. and the reaction is carried out for 25 hours to generate a suspension. The suspension is taken out, and then centrifuged, washed, and dried to obtain decanyltrimethylammonium chloride-modified zirconium phosphate; Weigh 120g of pentaerythritol ester, first mix 65g of pentaerythritol ester and 5.76g of calcium hydroxide, pour into the fat making kettle, heat and stir, the stirring speed is 75rmp, when the temperature in the fat making kettle rises to 40°C, add 4.8g of acetic acid, and keep warm for 50min to carry out saponification reaction; after the reaction is completed, heat the temperature in the fat making kettle to 80°C, add 16.8g of dodecyl hydroxystearic acid, and keep warm for 80min to carry out saponification reaction; after the reaction is completed, add 24g of pentaerythritol ester, continue to heat to 215°C, keep warm for 14min, and then stop heating; when the temperature in the fat making kettle drops to 120°C, add 31g of pentaerythritol ester, when the temperature in the fat making kettle drops to 100°C, stop stirring, and after the temperature drops to room temperature, a semi-solid fluid is obtained; roll and grind 5 times using a three-roll grinder to obtain a basic composite calcium-based grease; 5 g of zirconium phosphate modified with decantrimethylammonium chloride and 1 g of dinonyldiphenylamine were added in sequence to 94 g of basic composite calcium-based grease, the mixture was stirred for 7 minutes, and the mixture was rolled and ground 5 times using a three-roll mill to obtain a composite calcium-based grease with modified layered zirconium phosphate as a solid lubricating additive. The composition of the grease is as follows: basic composite calcium-based grease: 94%; zirconium phosphate modified with decantrimethylammonium chloride: 5%; dinonyldiphenylamine: 1%, named 5%DC-ZrP-5 grease. Example 7

[0026] Phosphoric acid, zirconium oxychloride octahydrate, methanol, and decanyltrimethylammonium chloride are added to a polytetrafluoroethylene liner at a molar ratio of 8:1:180:1, 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 heating and synthesis reaction. The synthesis reaction temperature is controlled to be 80° C. and the reaction is carried out for 10 hours to generate a suspension. The suspension is taken out, and then centrifuged, washed, and dried to obtain decanyltrimethylammonium chloride-modified zirconium phosphate; Weigh 120g of polyalphaolefin, first mix 40g of polyalphaolefin and 5g of calcium hydroxide, pour into the fat making kettle, heat and stir, the stirring speed is 70rmp, when the temperature in the fat making kettle rises to 35°C, add 5g of acetic acid, and keep warm for 30min to carry out saponification reaction; after the reaction is completed, heat the temperature in the fat making kettle to 75°C, add 15g of dodecyl hydroxystearic acid, and keep warm for 60min to carry out saponification reaction; after the reaction is completed, add 24g of polyalphaolefin, continue to heat to 200°C, keep warm for 10min, and then stop heating; when the temperature in the fat making kettle drops to 115°C, add 56g of polyalphaolefin, when the temperature in the fat making kettle drops to 95°C, stop stirring, and after the temperature drops to room temperature, a semi-solid fluid is obtained; roll and grind 5 times using a three-roll grinder to obtain a basic composite calcium-based grease; 5 g of zirconium phosphate modified with decantrimethylammonium chloride and 1 g of dinonyldiphenylamine were added to 94 g of basic composite calcium-based grease in sequence, the mixture was stirred for 7 minutes, and the mixture was rolled and ground 5 times using a three-roll mill to obtain a composite calcium-based grease with modified layered zirconium phosphate as a solid lubricating additive. The composition of the grease is as follows: basic composite calcium-based grease: 94%; zirconium phosphate modified with decantrimethylammonium chloride: 5%; dinonyldiphenylamine: 1%, and the grease was named 5%DC-ZrP-6 grease. Example 8

[0027] Phosphoric acid, zirconium oxychloride octahydrate, methanol, and decanyltrimethylammonium chloride are added to a polytetrafluoroethylene liner at a molar ratio of 13:1:230:2, 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 heating and synthesis reaction. The synthesis reaction temperature is controlled to be 130° C. and the reaction is carried out for 35 hours to generate a suspension. The suspension is taken out, and then centrifuged, washed, and dried to obtain decanyltrimethylammonium chloride-modified zirconium phosphate; Weigh 120g of polyalphaolefin, first mix 80g of polyalphaolefin and 6.92g of calcium hydroxide, pour into the fat making kettle, heat and stir, the stirring speed is 80rmp, when the temperature in the fat making kettle rises to 45°C, add 4.62g of acetic acid, and keep warm for 60min to carry out saponification reaction; after the reaction is completed, heat the temperature in the fat making kettle to 85°C, add 18.46g of dodecyl hydroxystearic acid, and keep warm for 90min to carry out saponification reaction; after the reaction is completed, add 24g of polyalphaolefin, continue to heat to 220°C, keep warm for 15min, and then stop heating; when the temperature in the fat making kettle drops to 125°C, add 16g of polyalphaolefin, when the temperature in the fat making kettle drops to 105°C, stop stirring, and after the temperature drops to room temperature, a semi-solid fluid is obtained; roll and grind 5 times using a three-roll grinder to obtain a basic composite calcium-based grease; 5 g of zirconium phosphate modified with decantrimethylammonium chloride and 1 g of dinonyldiphenylamine were added in sequence to 94 g of basic composite calcium-based grease, the mixture was stirred for 7 minutes, and the mixture was rolled and ground 5 times using a three-roll mill to obtain a composite calcium-based grease with modified layered zirconium phosphate as a solid lubricating additive. The components of the grease are: basic composite calcium-based grease: 94%; zirconium phosphate modified with decantrimethylammonium chloride: 5%; dinonyldiphenylamine: 1%, named 5%DC-ZrP-7 grease. Comparative Example 1

[0028] The solid lubricating additive in this comparative example is layered zirconium phosphate; The preparation method of basic composite calcium-based grease is the same as that of Example 1; 5 g of layered zirconium phosphate and 1 g of dinonyldiphenylamine were added to 94 g of basic composite calcium-based grease in sequence, the mixture was stirred for 7 minutes, and the mixture was rolled and ground 5 times using a three-roll mill to obtain a composite calcium-based grease with layered zirconium phosphate as a solid lubricating additive. The composition of the grease is as follows: basic composite calcium-based grease: 94%; layered zirconium phosphate: 5%; dinonyldiphenylamine: 1%, named 5% α-ZrP grease.

[0029] This comparative example provides a composite calcium-based grease using layered zirconium phosphate as a solid lubricating additive, which is contrasted with Example 1. Comparative Example 2

[0030] The solid lubricating additive in this comparative example is molybdenum disulfide; The preparation method of basic composite calcium-based grease is the same as that of Example 1; Add 5g of molybdenum disulfide and 1g of dinonyldiphenylamine in sequence to 94g of basic composite calcium-based grease, mix and stir for 7 minutes, and roll grind 5 times on a three-roll grinder to obtain a composite calcium-based grease with molybdenum disulfide as a solid lubricating additive. Its components are: basic composite calcium-based grease: 94%; molybdenum disulfide: 5%; dinonyldiphenylamine: 1%, named 5% MoS2 grease.

[0031] This comparative example provides a composite calcium-based grease using molybdenum disulfide as a solid lubricating additive, which is compared with Example 1. Comparative Example 3

[0032] Phosphoric acid, zirconium oxychloride octahydrate, methanol and decanyltrimethylammonium chloride are added into a polytetrafluoroethylene liner at a molar ratio of 8:5:180:1, and the mixture is stirred and evenly mixed. The polytetrafluoroethylene liner is placed into a reactor and tightened, and then the reactor is placed in an oven for heating synthesis reaction. The synthesis reaction temperature is controlled to be 110°C, and the reaction is carried out for 30 hours to generate a suspension. The suspension is taken out, centrifuged, washed and dried to obtain decanyltrimethylammonium chloride-modified zirconium phosphate.

[0033] In this comparative example, the decanyltrimethylammonium chloride-modified zirconium phosphate is prepared using synthesis conditions outside the parameter range of claim 7, which is compared with the decanyltrimethylammonium chloride-modified zirconium phosphate prepared in Example 1. Comparative Example 4

[0034] Weigh 120g of polyalphaolefin and 5.76g of calcium hydroxide, mix and pour into a fat-making kettle, heat and stir at a stirring speed of 75rmp. When the temperature in the fat-making kettle rises to 40°C, add 4.8g of acetic acid and keep warm for 50min to carry out saponification reaction. After the reaction is completed, heat the temperature in the fat-making kettle to 80°C, add 16.8g of dodecyl hydroxystearic acid, and keep warm for 80min to carry out saponification reaction. After the reaction is completed, continue to heat to 215°C, keep warm for 14min, and then stop heating. When the temperature in the fat-making kettle drops to 100°C, stop stirring, and after the temperature drops to room temperature, a semi-solid fluid is obtained. Roll and grind 5 times using a three-roll grinder to obtain a basic composite calcium-based grease. The basic composite calcium-based grease prepared in this comparative example adopts the method of adding the base oil in one step, and is compared with the basic composite calcium-based grease prepared in Example 1. Test example

[0035] 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. The extreme pressure performance was measured by the maximum no-seizure load (P B ) and sintering load (P D ) value, the larger the value, the better the performance; the anti-wear performance is measured by the wear spot diameter (WSD) value, the smaller the value, the better the performance; the anti-friction performance is measured by the friction coefficient (μ) value, the smaller the value, the better the performance. The test results are shown in Table 1 (P in Table 1 B and P D The value is measured by step-by-step load. If the test requirements are not met, the test value of the lower load level is taken).

[0036]

[0037] From the lubricating data of the greases in Example 1, Comparative Example 1 and Comparative Example 2, it can be seen that after adding DC-ZrP, α-ZrP and MoS2 to the basic composite calcium-based grease, the maximum no-seizure load (P B ) and sintering load (P D) is significantly higher than 5% α-ZrP grease and 5% MoS2 grease; the wear spot diameter (WSD) and friction coefficient (μ) of 5% DC-ZrP grease are lower than those of 5% α-ZrP grease and 5% MoS2 grease. Compared with the prior art, the present invention introduces lipophilic decanyltrimethylammonium chloride between the layered zirconium phosphate layers for functional modification. The modified layered material is more conducive to stable dispersion in the grease, and the obtained grease product has stronger extreme pressure and anti-wear and friction reduction properties, which can meet more application conditions.

[0038] From the lubrication data of the basic complex calcium-based grease of Example 1 and the basic complex calcium-based grease of Comparative Example 4, it can be seen that the maximum non-seizure load (P B ) and sintering load (P D ) are 726N and 1236N respectively, significantly higher than the latter's 588N and 785N; the former's wear spot diameter (WSD) and friction coefficient (μ) are lower than the latter. Compared with adding base oil in one step, adding base oil in steps can make soap fibers more stably dispersed in the base oil, thereby improving the lubrication performance of the basic composite calcium-based grease.

[0039] From Table 1, it can be seen that after adding the zirconium phosphate material modified with decanyl trimethyl ammonium chloride, the maximum non-seizure load (P B ) and sintering load (P D ) were significantly improved, indicating that the material can significantly enhance the extreme pressure performance of grease; the wear spot diameter (WSD) and friction coefficient (μ) of the composite calcium-based grease were significantly reduced, indicating that the material can significantly enhance the extreme pressure and anti-wear and friction-reducing properties of grease.

[0040] from Figure 1 It can be seen that the modified zirconium phosphate material prepared in Example 1 still retains the original layered structure of zirconium phosphate, while the morphology of the modified zirconium phosphate material prepared in Comparative Example 3 has changed and no longer has a layered structure; Figure 2 It can be seen that the modified zirconium phosphate material prepared in Example 1 has an obvious modification characteristic peak, while the modified zirconium phosphate material prepared in Comparative Example 3 has an unclear modification characteristic peak, indicating that when the molar ratio of phosphoric acid, zirconium oxychloride octahydrate, methanol, and decanyltrimethylammonium chloride is controlled to be 8-13:1:180-230:1-2, the prepared modified zirconium phosphate material still retains the original layered structure of zirconium phosphate, and can effectively improve the lubrication performance of the grease product.

[0041] The above embodiments are only for the purpose of illustrating the technical solution of the present invention and should not be considered as limiting. Although described in detail, professionals and technicians can make modifications or equivalent substitutions without departing from the scope of the present invention, and these changes still belong to the protection scope of the present invention.

Claims

1. A composite calcium-based grease, characterized in that: The composition includes the following weight percentages: Basic complex calcium-based grease: 90-94%, Zirconium phosphate modified with decanyltrimethylammonium chloride: 5-9%, Dinonyldiphenylamine: 1%.

2. A method for preparing the complex calcium-based grease as claimed in claim 1, characterized in that: The following steps are involved: The basic composite calcium-based grease, zirconium phosphate modified with decanyltrimethylammonium chloride, and dinonyldiphenylamine are stirred and mixed uniformly and ground to obtain the composite calcium-based grease.

3. The preparation method according to claim 2, characterized in that: The weight ratio of the basic composite calcium-based grease, the zirconium phosphate modified by decanyltrimethylammonium chloride, and the dinonyldiphenylamine is 90-94:5-9:

1.

4. The preparation method according to claim 2, characterized in that: The preparation method of the basic composite calcium-based grease is as follows: 1 / 3-2 / 3 of the total amount of the basic lubricating oil is mixed with calcium hydroxide and poured into a reaction container, heated and stirred at a stirring speed of 70-80 rpm, when the temperature in the reaction container rises to 35-45° C., acetic acid is added, and the mixture is kept warm for 30-60 minutes to carry out a saponification reaction; after the reaction is completed, the temperature in the reaction container is heated to 75-85° C., dodecyl hydroxystearic acid is added, and the mixture is kept warm for 60-90 minutes to carry out a saponification reaction; after the reaction is completed, 1 / 5 of the total amount of the basic lubricating oil is added into the reaction container, and the mixture is heated to 200-220° C. and kept warm for 10-15 minutes; then the heating is stopped; when the temperature in the reaction container drops to 115-125° C., the remaining basic lubricating oil is added, when the temperature in the reaction container drops to 95-105° C., the stirring is stopped, and after the temperature drops to room temperature, a semi-solid fluid is obtained; and the semi-solid fluid is ground to obtain the basic composite calcium-based grease.

5. The preparation method according to claim 4, characterized in that: The base lubricant is any one of polyalphaolefin, paraffin-based mineral oil, soybean oil and pentaerythritol ester; the weight ratio of calcium hydroxide, base lubricant, acetic acid and dodecyl hydroxystearic acid is 1-1.5:24-26:1:3-4.

6. The preparation method according to claim 2, characterized in that: The preparation method of the decanyltrimethylammonium chloride modified zirconium phosphate is as follows: phosphoric acid, zirconium oxychloride octahydrate, methanol and decanyltrimethylammonium chloride are stirred and mixed, heated for synthesis reaction to generate a suspension, and then centrifuged, washed and dried to obtain the decanyltrimethylammonium chloride modified zirconium phosphate.

7. The preparation method according to claim 6, characterized in that: The molar ratio of phosphoric acid, zirconium oxychloride octahydrate, methanol and decanyltrimethylammonium chloride is 8-13:1:180-230:1-2; the synthesis reaction temperature is 80-130°C, and the reaction time is 10-35h.

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