Grease composition and method for producing the same

Abstract

The present application provides a kind of grease composition and its preparation method.The grease composition of the present application includes the following components based on the total weight of the grease composition: 65% to 90% base oil, 8% to 30% lithium-based thickener or composite lithium-based thickener, 0.1% to 2% anti-rust agent, 0.1% to 5% organic sulfur phosphorus compound, wherein the structure of the organic sulfur phosphorus compound is shown in formula (I): wherein the definition of each group is described in the specification.The grease composition of the present application has excellent extreme pressure, anti-wear, oxidation resistance and corrosion prevention properties.

Description

Technical Field

[0001] This invention relates to a grease composition, and more particularly to a lithium-based or complex lithium-based grease composition. Background Technology

[0002] Grease, as an important lubricating, protective, and sealing material, is mainly used in the friction parts of machinery and also on metal surfaces to fill gaps and prevent rust. It has a wide range of uses in daily life. With the advancement of technology and the requirements of environmental regulations, grease additives are developing towards a trend of "compound and micro-dosage". More and more compound additives have emerged, which can do the work of many additives. This not only enhances the synergistic effect between additives, but also reduces the amount of additives used and lowers costs.

[0003] CN 106317109A discloses a thiophosphate type extreme pressure anti-wear agent, which exhibits good rust prevention, thermal stability, and hydrolytic stability, but its anti-wear and friction-reducing properties are not superior to those of existing technologies. CN 102260572B discloses a phosphorus-nitrogen type extreme pressure anti-wear agent, which has good antioxidant, rust prevention, and corrosion prevention properties and can be used as a multifunctional additive for industrial lubricating greases. However, it can only be used as a supplement to sulfur-phosphorus composite extreme pressure anti-wear agents, and it does not exhibit good extreme pressure anti-wear performance on its own.

[0004] Currently, phosphorus-containing additives exhibit good anti-wear and friction-reducing properties, but lack strong antioxidant properties. The trend in lubricating grease additive development is towards multi-functionality. Developing multi-functional additives can improve additive performance, reduce the variety and amount of additives in the formulation system, improve formulation applicability, and help meet energy-saving and environmental protection requirements. Summary of the Invention

[0005] This invention proposes a grease composition and its preparation method.

[0006] The lubricating grease composition of the present invention, based on the total weight of the lubricating grease composition, comprises the following components: 65% to 90% base oil, 8% to 30% lithium-based thickener or complex lithium-based thickener, 0.1% to 2% rust inhibitor, and 0.1% to 5% organosulfur-phosphorus compound, wherein the structure of the organosulfur-phosphorus compound is shown in formula (I):

[0007]

[0008] In formula (I), there are a L groups and b sulfur-containing phosphorus groups, where a is an integer between 1 and 8, and b is an integer between 1 and 10. The a L groups may be the same as or different from each other, and each is independently selected from the groups shown in formula (II).

[0009]

[0010] In formula (II), HO is bonded to the benzene ring; y R groups are bonded to the benzene ring; y is selected from integers between 0 and 4; and the R groups are selected from H and C. 1-10 Straight-chain or branched alkyl groups; n is an integer between 1 and 5; R1 is independently selected from C 1-10 Straight-chain or branched alkylene groups; the R2s in the n repeating units may be the same or different from each other, and each is independently selected from single bonds and C bonds. 1-10 Straight-chain or branched alkylene groups; R3 is selected from H and C. 1-10 Straight-chain or branched alkyl; the A groups in the n repeating units may be the same or different from each other, and each is independently selected from the groups shown in formula (III) and formula (IV).

[0011]

[0012] The R4 groups are each independently selected from H and C. 1-10 Straight-chain or branched alkyl; * in formulas (III) and (IV) represents a bonding end that is bonded to formula (II);

[0013] In formulas (III) and (IV), △ represents the bonding end bonded to b sulfur-containing phosphorus groups; each of the X groups in the b sulfur-containing phosphorus groups may be the same as or different from each other, and each is independently selected from the bonding end bonded to a L group, H, OH, R', OR', SR'; each of the R0 groups in the b sulfur-containing phosphorus groups may be the same as or different from each other, and each is independently selected from H, OH, R', OR', SR'; wherein R' is selected from C 1-20 Straight-chain or branched alkyl groups, C 6-10 aryl, with one or more C 1-10 Straight-chain or branched alkyl-substituted C 6-10 aryl, C 1-20 The R' is a heterohydrocarbon group containing an oxygen atom or a sulfur atom, wherein the R' is optionally substituted by one or more groups selected from halogens and hydroxyl groups;

[0014] In each thiophosphorus group, there is one or two X's selected from the binding ends that are bonded to the L group; the various groups in the organothiophosphorus compound conform to the bonding rules.

[0015] According to the present invention, preferably, in formula (I), a is an integer between 1 and 4, and b is an integer between 1 and 6; in formula (II), HO is located at the meta position on the chain containing R1 on the benzene ring, y is an integer between 1 and 3, y R groups are located at the para or ortho position on the chain containing R1 on the benzene ring, and the R groups are selected from C 1-4 Straight-chain or branched alkyl groups (preferably tert-butyl), n is an integer between 1 and 3, and R1 is independently selected from C1. 1-4 A straight-chain or branched alkylene group, wherein the R2 in each of the n repeating units is independently selected from single bonds and C bonds. 1-4Straight-chain or branched alkylene groups, R3 selected from H and C 1-4 Straight-chain or branched alkyl groups; each of the R4 groups is independently selected from H and C. 1-4 Straight-chain or branched alkyl groups; wherein R' is selected from C 1-10 Straight-chain or branched alkyl, phenyl, and compounded by one or more C 1-10 Straight-chain or branched alkyl-substituted phenyl, C 1-10 It contains heterohydrocarbon groups containing oxygen or sulfur atoms.

[0016] According to the present invention, when both X groups in each thiophosphoric group are selected from the binding ends that are bonded to the L group, the two X groups can be bonded to the same L group or to two different L groups respectively.

[0017] According to the present invention, the two bonding ends (i.e. the two *) in formula (III) or formula (IV) that are bonded to formula (II) can be bonded to the group in formula (II) in any manner, for example, they can be bonded to formula (II) in one direction or in the opposite direction.

[0018] In the context of this invention, the heteroalkyl group refers to a group whose carbon chain structure is interrupted by one or more (e.g., 1 to 5, 1 to 4, 1 to 3, 1 to 2, or 1) heterogroups selected from -Sx- and -O-, wherein x is an integer between 1 and 5 (preferably an integer between 1 and 4, more preferably 1, 2, or 3); the hydrocarbon group can be a straight-chain or branched alkyl, a straight-chain or branched cycloalkyl, a straight-chain or branched aryl, or a mixed hydrocarbon group containing two or more of the groups selected from alkyl, cycloalkyl, and aryl. From the perspective of structural stability, preferably, when multiple heterogroups are present, no two of the heterogroups are directly bonded together.

[0019] According to the present invention, examples of the organosulfur-phosphorus compounds include one or more of the following structural compounds:

[0020]

[0021]

[0022] According to the present invention, the method for preparing the organosulfur-phosphorus compound includes the following steps:

[0023] (1) React the compound shown in formula (α) with the peroxide;

[0024]

[0025] In formula (α), HO is bonded to the benzene ring; y R groups are bonded to the benzene ring; y is selected from integers between 0 and 4; and the R groups are selected from H and C.1-10 Straight-chain or branched alkyl groups; n is an integer between 1 and 5; R1 is independently selected from C 1-10 Straight-chain or branched alkylene groups; the R2s in the n repeating units may be the same or different from each other, and each is independently selected from single bonds and C bonds. 1-10 Straight-chain or branched alkylene groups; R3 is selected from H and C. 1-10 Straight-chain or branched alkyl; the A" in the n repeating units may be the same as or different from each other, and each is independently selected from... The R4 groups therein are each independently selected from H and C. 1-10 Straight-chain or branched alkyl groups;

[0026] (2) React the reaction product of step (1) with the compound shown in formula (β) and collect the product;

[0027]

[0028] In formula (β), each X' group may be the same as or different from each other, and each is independently selected from H, OH, R', OR', SR'; R0 is selected from H, OH, R', OR', SR'; and R' is selected from C. 1-20 Straight-chain or branched alkyl groups, C 6-10 aryl, with one or more C 1-10 Straight-chain or branched alkyl-substituted C 6-10 aryl, C 1-20 The R' is a heterohydrocarbon group containing an oxygen atom or a sulfur atom, wherein the R' is optionally substituted by one or more groups selected from halogens and hydroxyl groups; in formula (β), at least one X' group is selected from OH.

[0029] According to the present invention, preferably, HO is located at the meta position on the chain containing R1 on the benzene ring, y is an integer between 1 and 3, y R groups are located at the para or ortho position on the chain containing R1 on the benzene ring, and the R groups are selected from C 1-4 Straight-chain or branched alkyl groups (more preferably tert-butyl), n is an integer between 1 and 3, and R1 is independently selected from C1. 1-4 A straight-chain or branched alkylene group, wherein the R2 in each of the n repeating units is independently selected from single bonds and C bonds. 1-4 Straight-chain or branched alkylene groups, R3 selected from H and C 1-4 Straight-chain or branched alkyl groups; each of the R4 groups is independently selected from H and C. 1-4 Straight-chain or branched alkyl groups; wherein R' is selected from C 1-10 Straight-chain or branched alkyl, phenyl, and compounded by one or more C 1-10 Straight-chain or branched alkyl-substituted phenyl, C 1-10 It contains heterohydrocarbon groups containing oxygen or sulfur atoms.

[0030] According to the present invention, in step (1), the compound represented by formula (α) can be selected from cashew phenol and alkylated cashew phenol. The alkylated cashew phenol can be obtained by reacting cashew phenol with an alkylating agent, for example, by reacting cashew phenol with tert-butyl chloride to obtain tert-butylated cashew phenol.

[0031] According to the present invention, in step (1), the peroxide is preferably one or more of hydrogen peroxide, formic acid, peracetic acid, persulfonic acid, m-chloroperoxybenzoic acid, tert-butyl hydroperoxide, tert-butyl peracetic acid, methyl ethyl ketone peroxide, benzoyl peroxide and cyclohexanone peroxide, more preferably one or more of hydrogen peroxide, formic acid, peracetic acid and persulfonic acid.

[0032] According to the present invention, in step (2), the compound represented by formula (β) can be selected from alkoxythiophosphoric acid, aryloxythiophosphoric acid, alkylthiophosphoric acid, arylthiophosphoric acid, alkoxythiophosphonic acid, alkylthiophosphonic acid, hydroxy-substituted alkylthiophosphoric acid, etc. For example, phenylthiophosphonic acid, ethylthiophosphonic acid, phenoxythiophosphoric acid, ethylthiophosphoric acid, hydroxymethylthiophosphonic acid, phenylthiomethoxythiophosphoric acid, thiophosphoric acid, or one or more of these can be selected.

[0033] According to the present invention, the equivalence ratio between the compound represented by formula (α) and the peroxide and the compound represented by formula (β) is preferably 1:0.5 to 10:0.5 to 10, more preferably 1:2 to 5:2 to 5.

[0034] According to the present invention, the reaction temperature of step (1) is preferably 0 to 100°C, more preferably 20 to 80°C; the reaction temperature of step (2) is preferably 50 to 150°C, more preferably 70 to 120°C.

[0035] According to the present invention, a catalyst may be added in step (1), preferably an acidic catalyst, more preferably a Lewis acid catalyst, such as one or more of concentrated sulfuric acid, zinc chloride, aluminum trichloride, benzenesulfonic acid and titanate, and the amount of catalyst added is preferably 0.01% to 3% of the compound shown in formula (α). After the reaction in step (1) is completed, the catalyst may be removed by alkaline washing or water washing.

[0036] According to the present invention, a catalyst may be added in step (2), preferably an acidic catalyst, more preferably a Lewis acid catalyst, such as one or more of concentrated sulfuric acid, zinc chloride, aluminum trichloride, benzenesulfonic acid and titanate, and the amount of catalyst added is preferably 0.5% to 10% of the compound shown in formula (α). After the reaction in step (2) is completed, the catalyst may be removed by alkaline washing or water washing.

[0037] According to the present invention, the reaction steps (1) and (2) can be carried out in the presence of a diluent and / or a solvent, or without the use of a diluent and / or a solvent.

[0038] According to the present invention, the diluent may be selected from one or more of API Group I, II, III, IV and V base oils. Common products or grades include 150SN, 200SN, 350SN, 500SN, 650SN, 150BS, HVI-100, HVI-150, HVI-200, HVI-350, HVI-400, HVI-500, HVI-150BS, PAO4, PAO6, PAO8, PAO10, alkylbenzene, alkylnaphthalene, etc.

[0039] According to the present invention, the solvent may be water, C 6-20 Aromatic hydrocarbons (such as benzene, toluene, xylene, and cumene), C 6-10 Alkanes (such as n-hexane, cyclohexane, and petroleum ether), solvent gasoline, etc. These solvents may be used individually, or in combination of two or more. The solvents may be removed after the reaction is complete, using methods known to those skilled in the art, such as under normal or reduced pressure.

[0040] According to a particular embodiment of the present invention, the diluent and / or solvent may be added at any stage of the reaction step in the amounts conventional in the art, without particular limitation.

[0041] According to the present invention, the reaction can be carried out under the protection of an inert gas atmosphere. Examples of inert gases include nitrogen and argon, and there is no particular limitation.

[0042] According to the present invention, the aforementioned preparation method can produce a single organosulfur phosphorus compound, a mixture of multiple organosulfur phosphorus compounds, or a mixture of one or more organosulfur phosphorus compounds with the aforementioned diluent (if used) as the reaction product. These reaction products are all contemplated by the present invention, and their different forms do not affect the achievement of the effects of the present invention. Therefore, in the context of this specification, these reaction products are collectively referred to as organosulfur phosphorus compounds without distinction. In view of this, according to the present invention, there is no absolute necessity for further purification of the reaction product or for further separation of an organosulfur phosphorus compound with a specific structure from the reaction product. Of course, such purification or separation is preferred for further enhancing the intended effects of the present invention, but is not necessary for the present invention. Nevertheless, methods for purification or separation, such as column chromatography or preparative chromatography, can be cited as examples.

[0043] According to the present invention, the base oil may be one or more selected from mineral oil, synthetic oil, ester oil, polyether, and silicone oil, preferably with a viscosity of 2 to 100 mm at 100°C. 2 The base oil has a viscosity of 4-50 mm at 100°C, more preferably a viscosity of 4-50 mm. 2 The base oil is denoted as / s. The mineral oil includes one or more of naphthenic mineral oil, paraffinic mineral oil, and intermediate mineral oil, such as 500SN, 150BS, etc.; the synthetic oil includes one or more of polyalphaolefin, alkylbenzene, and alkylnaphthalene; the ester oil includes one or more of diester, polyol ester, and complex ester, such as trimethylolpropane ester, pentaerythritol fatty acid ester, dioctyl sebacate, etc.; the polyether includes perfluoropolyether and / or polyethylene glycol ether; the silicone oil includes one or more of methyl silicone oil, ethyl silicone oil, and methylphenyl silicone oil.

[0044] According to the present invention, the lithium-based thickener and the composite lithium-based thickener can be any thickener known in the prior art, and there is no particular limitation.

[0045] According to the present invention, optionally, the lithium-based thickener is obtained by a saponification reaction of a fatty acid and lithium hydroxide. The fatty acid is preferably C. 12 ~C 20 Fatty acids and / or hydroxy fatty acids.

[0046] According to the present invention, optionally, the composite lithium-based thickener is obtained by a saponification reaction between a composite acid and lithium hydroxide. The composite acid includes C... 12 ~C 20 Fatty acids and / or hydroxy fatty acids with C6-C6 11 A mixture of dicarboxylic acids; the C 12 ~C 20 The fatty acids and / or hydroxy fatty acids may be selected from one or more of lauric acid, myristic acid, palmitic acid, oleic acid, stearic acid, and 12-hydroxystearic acid, more preferably 12-hydroxystearic acid and / or stearic acid; the C6~C 11 The preferred dicarboxylic acid is one with a molecular weight of less than 300, such as one or more of terephthalic acid, adipic acid, azelaic acid, and sebacic acid, with sebacic acid being more preferred. The C 12 ~C 20 Fatty acids and / or hydroxy fatty acids with C6-C6 11 The molar ratio of the dicarboxylic acid is preferably 1:0.05 to 1.0, more preferably 1:0.1 to 0.8.

[0047] According to the present invention, the rust inhibitor is preferably selected from one or more of organic carboxylic acid rust inhibitors, organic carboxylate rust inhibitors, organic amine rust inhibitors, ester rust inhibitors, sulfur-nitrogen heterocyclic rust inhibitors, and inorganic salt rust inhibitors, more preferably from organic carboxylate rust inhibitors and / or sulfur-nitrogen heterocyclic rust inhibitors, such as zinc naphthenate, barium dinonylnaphthalenesulfonate, and benzotriazole, with common commercial brands including T704, T705, T706, etc. According to the present invention, preferably, based on the total weight of the grease composition, the grease composition comprises 70%–90% base oil, 8%–25% lithium-based thickener or complex lithium-based thickener, 0.2%–2% rust inhibitor, and 0.2%–5% organosulfur-phosphorus compound.

[0048] According to the present invention, the method for preparing the lubricating grease composition includes: adding a portion of base oil and all of the fatty acids or complex acids to a reaction vessel, stirring and heating to 75°C to 100°C, adding an aqueous lithium hydroxide solution, and carrying out a saponification reaction; after the saponification reaction is completed, heating to 205°C to carry out high-temperature refining, and then adding the remaining base oil; cooling to 130°C or below, adding a rust inhibitor and an organosulfur-phosphorus compound; and grinding into grease.

[0049] According to the present invention, the portion of base oil is preferably 1 / 3 to 2 / 3 of the total base oil; the saponification reaction time is preferably 20 min to 100 min; and the high-temperature refining time is preferably 5 min to 100 min.

[0050] The grease composition of the present invention has excellent extreme pressure anti-wear, anti-oxidation and anti-corrosion properties. Attached Figure Description

[0051] Figure 1 The infrared spectrum of the product of Example 2 is shown below.

[0052] Figure 2 The image shows the carbon NMR spectrum of the product from Example 2. Detailed Implementation

[0053] In this specification, the term "single bond" is sometimes used in the definition of a group. A "single bond" means that the group does not exist. For example, suppose the structural formula is -CH2-A-CH3, where group A is defined as selected from single bonds and methyl groups. Therefore, if A is a single bond, it means that group A does not exist, and the structural formula is correspondingly simplified to -CH2-CH3.

[0054] The present invention will be further illustrated by the following embodiments, but these are not intended to limit the scope of the invention.

[0055] The main raw materials used are as follows:

[0056] Cashew phenol, Shanghai Wujing Chemical Technology Co., Ltd., industrial products

[0057] Zinc chloride, Sinopharm Chemical Reagent Co., Ltd., analytical grade

[0058] Concentrated sulfuric acid, Sinopharm Chemical Reagent Co., Ltd., analytical grade.

[0059] Hydrogen peroxide (30%), Sinopharm Chemical Reagent Co., Ltd., analytical grade.

[0060] Formic acid, Sinopharm Chemical Reagent Co., Ltd., analytical grade

[0061] Phenylethiophosphonic acid, Sinopharm Chemical Reagent Co., Ltd., chemically pure

[0062] Ethiophosphonic acid, Sinopharm Chemical Reagent Co., Ltd., chemically pure

[0063] Ethiophosphoric acid, Sinopharm Chemical Reagent Co., Ltd., chemically pure

[0064] tert-butyl chloride, Sinopharm Chemical Reagent Co., Ltd., analytical grade

[0065] Toluene, Sinopharm Chemical Reagent Co., Ltd., analytical grade

[0066] PAO 6 synthetic oil, Shanghai Zejun Trading Co., Ltd., industrial products.

[0067] 12-Hydroxystearic acid, Tongliao Tonghua Castor Chemical Co., Ltd., Industrial Product

[0068] Sebacic acid, Tongliao Xinghe Biotechnology Co., Ltd., industrial product

[0069] Lithium hydroxide, Chengdu Tianqi Lithium Industry Co., Ltd., industrial product

[0070] Rust Inhibitor T706, Nanjing Aubeck Fine Chemical Co., Ltd., Industrial Products

[0071] T306, Zibo Huihua Petroleum Additives Co., Ltd., Industrial Product

[0072] T351, Wuhan Jinghe Chemical Co., Ltd., Industrial Products

[0073] Antioxidant V81, Beijing Lifuruida Science & Trade Co., Ltd., Industrial Products

[0074] Example 1: Preparation of tert-butylated epoxy cashew phenol

[0075] Take 100g of cashew nut shell powder, 8g of formic acid, 0.3g of sulfuric acid, and 200g of hydrogen peroxide, and add them to a three-necked flask equipped with a mechanical stirrer, reflux condenser, and temperature control. Turn on the stirrer and heat. Maintain the reaction temperature at 70℃ and react for 3 hours. After the reaction is complete, cool down to obtain a brownish-red transparent liquid. Filter the reaction product and wash it with 5% KOH solution, then wash it with distilled water until neutral. Distill the organic phase under reduced pressure at 100Pa and 150℃ for 1 hour to remove water and unreacted raw materials, obtaining an orange-red transparent liquid epoxidized cashew nut shell powder.

[0076] 35g of epoxidized cashew nut shell phenol was dissolved in 100ml of acetone. After dissolution, the solution was transferred to a 250ml three-necked reaction flask, and 0.9g of zinc chloride catalyst was added. The mixture was stirred and heated. The reaction temperature was maintained at 60℃. 9.5g of tert-butyl chloride was slowly added dropwise to the reaction flask. After the addition was complete, the reaction was continued for 3 hours. After the reaction was completed, the temperature was lowered to obtain a brownish-red transparent liquid. The reaction product was filtered and washed with 5% KOH solution, then washed with distilled water until neutral. The product was then distilled under reduced pressure at 1000Pa and 120℃ for 1 hour to remove the solvent, water, and unreacted raw materials, yielding a brownish-red viscous liquid, tert-butylated epoxidized cashew nut shell phenol.

[0077] An example reaction formula for the above reaction is shown below.

[0078]

[0079]

[0080] Example 2

[0081] 2g of the tert-butylated epoxy cashew phenol prepared in Example 1, 0.02g of concentrated sulfuric acid, 10g of water, and 100g of toluene were added to a three-necked flask equipped with a mechanical stirrer and a reflux condenser. The mixture was stirred, heated, and refluxed at 85°C for 1 hour. Then, 2g of phenylthiophosphonic acid was added dropwise. After the addition was complete, the reaction was continued under reflux for 5 hours, and then the reaction was stopped. The product was washed with water until neutral, and finally the solvent was evaporated to obtain the organosulfur-phosphorus compound W-01 of the present invention.

[0082] Since the reactants are a mixture of tert-butylated epoxy cashew phenols such as monoepoxy, diepoxy, and triepoxy, the reaction products are a mixture of numerous organosulfur and phosphorus compounds. Therefore, the following are some representative examples of the main reaction formulas for the reaction of tert-butylated epoxy cashew phenols with monoepoxy.

[0083]

[0084] The product prepared in Example 2 was subjected to infrared spectroscopy and nuclear magnetic resonance analysis. The infrared spectrum is shown in the figure. Figure 1 The analysis results are shown in Table 1, and the NMR spectra are shown in Table 1. Figure 2 The analysis results are shown in Table 2.

[0085] Table 1 Infrared analysis results of the products

[0086]

[0087] Table 1 shows that the product contains characteristic peaks such as C-OH stretching vibration peak, P=S stretching vibration peak, benzene ring skeleton stretching vibration peak, POC stretching vibration peak, and PC stretching vibration peak, which indicates that the synthesized product is the target compound.

[0088] Table 2. Results of NMR spectroscopy analysis of the products

[0089]

[0090] The C element assignments for the OH groups on the benzene ring in Table 2 indicate the presence of phenolic structures in the products; the C element assignments for PC indicate the presence of phenyl phosphide structures; the C element assignments for OC indicate the presence of ester groups on the alkyl chains; and the C element assignments for tert-butyl quaternary structures indicate the presence of tert-butyl structures. The C element assignments can indicate that the synthesized products are the target compounds.

[0091] Example 3

[0092] 2g of the tert-butylated epoxy cashew phenol prepared in Example 1, 0.01g of concentrated sulfuric acid, 10g of water, and 100g of toluene were added to a three-necked flask equipped with a mechanical stirrer and a reflux condenser. The mixture was stirred, heated, and refluxed at 95°C for 1 hour. Then, 3.2g of ethyl thiophosphonic acid was added dropwise. After the addition was complete, the reaction was refluxed for another 3 hours, and then the reaction was stopped. The product was washed with water until neutral, and finally the solvent was evaporated to obtain the organosulfur-phosphorus compound W-02.

[0093] Example 4

[0094] 2g of the tert-butylated epoxy cashew phenol prepared in Example 1, 0.05g of concentrated sulfuric acid, 10g of water, and 100g of toluene were added to a three-necked flask equipped with a mechanical stirrer and a reflux condenser. The mixture was stirred, heated, and refluxed at 110°C for 1 hour. Then, 2.5g of ethylthiophosphoric acid was added dropwise. After the addition was complete, the reaction was continued under reflux for 6 hours, at which point the reaction was stopped. The product was washed with water until neutral, and finally the solvent was evaporated to obtain the organosulfur-phosphorus compound W-03.

[0095] Example 5

[0096] 400g of PAO 6 synthetic oil (viscosity 5.69mm at 100℃) 290g of 12-hydroxystearic acid and 30g of sebacic acid were added to a reaction vessel, stirred and heated, and an aqueous solution containing 26.5g of lithium hydroxide was added at 80°C. The reaction was carried out for 30 minutes, and the temperature was continuously raised to 210°C for high-temperature refining for 15 minutes. 460g of PAO 6 synthetic oil was added, and the mixture was cooled to 130°C. 2.5g of W-01 prepared in Example 2 and 2g of T706 were added. The mixture was then ground three times with a three-roll mill to obtain the lubricating grease composition of the present invention. Its properties are shown in Table 3.

[0097] Example 6

[0098] 400g of PAO 6 synthetic oil (viscosity 5.69mm at 100℃) 2 90g of 12-hydroxystearic acid and 30g of sebacic acid were added to a reaction vessel, stirred and heated, and an aqueous solution containing 26.5g of lithium hydroxide was added at 80°C. The reaction was carried out for 30 minutes, and the temperature was continuously raised to 210°C for high-temperature refining for 15 minutes. 460g of PAO 6 synthetic oil was added, and the mixture was cooled to 130°C. 2.5g of W-02 prepared in Example 3 and 2g of T706 were added. The mixture was then ground three times with a three-roll mill to obtain the lubricating grease composition of the present invention. Its properties are shown in Table 3.

[0099] Example 7

[0100] 400g of PAO 6 synthetic oil (viscosity 5.69mm at 100℃) 2 90g of 12-hydroxystearic acid and 30g of sebacic acid were added to a reaction vessel, stirred and heated, and an aqueous solution containing 26.5g of lithium hydroxide was added at 80°C. The reaction was carried out for 30 minutes, and the temperature was continuously raised to 210°C for high-temperature refining for 15 minutes. 460g of PAO 6 synthetic oil was added, and the mixture was cooled to 130°C. 2.5g of W-03 prepared in Example 4 and 2g of T706 were added. The mixture was then ground three times with a three-roll mill to obtain the grease composition of the present invention. Its properties are shown in Table 3.

[0101] Example 8

[0102] 400g of PAO 6 synthetic oil (viscosity 5.69mm at 100℃) 2 120g of 12-hydroxystearic acid was added to a reaction vessel, stirred and heated, and an aqueous solution containing 17g of lithium hydroxide was added at 80°C. The reaction was carried out for 30 minutes, and the temperature was continuously raised to 210°C for high-temperature refining for 15 minutes. 460g of PAO 6 synthetic oil was added, and the mixture was cooled to 130°C. 2.5g of W-01 prepared in Example 2 and 2g of T706 were added. The mixture was then ground three times with a three-roll mill to obtain the grease composition of the present invention. Its properties are shown in Table 3.

[0103] Example 9

[0104] 400g of PAO 6 synthetic oil (viscosity 5.69mm at 100℃) 2 90g of 12-hydroxystearic acid and 30g of sebacic acid were added to a reaction vessel, stirred and heated, and an aqueous solution containing 26.5g of lithium hydroxide was added at 80°C. The reaction was carried out for 30 minutes, and the temperature was continuously raised to 210°C for high-temperature refining for 15 minutes. 460g of PAO 6 synthetic oil was added, and the mixture was cooled to 130°C. 25g of W-01 prepared in Example 2 and 2g of T706 were added. The mixture was then ground three times with a three-roll mill to obtain the lubricating grease composition of the present invention. Its properties are shown in Table 3.

[0105] Example 10

[0106] 400g of PAO 6 synthetic oil (viscosity 5.69mm at 100℃) 2 90g of 12-hydroxystearic acid and 30g of sebacic acid were added to a reaction vessel, stirred and heated, and an aqueous solution containing 26.5g of lithium hydroxide was added at 80°C. The reaction was carried out for 30 minutes, and the temperature was continuously raised to 210°C for high-temperature refining for 15 minutes. 460g of PAO 6 synthetic oil was added, and the mixture was cooled to 130°C. 2.5g of W-01 prepared in Example 2 and 10g of T706 were added. The mixture was then ground three times with a three-roll mill to obtain the lubricating grease composition of the present invention. Its properties are shown in Table 3.

[0107] Comparative Example 1

[0108] 400g of PAO 6 synthetic oil (viscosity 5.69mm at 100℃) 2 90g of 12-hydroxystearic acid and 30g of sebacic acid were added to a reaction vessel, stirred and heated, and an aqueous solution containing 26.5g of lithium hydroxide was added at 80℃. The reaction was carried out for 30 minutes, and the temperature was continuously raised to 210℃ for high-temperature refining for 15 minutes. 460g of PAO 6 synthetic oil was added, and the mixture was cooled to 130℃. 2.5g of T306 and 2g of T706 were added. The mixture was then ground three times with a three-roll mill to obtain a comparative grease composition. Its properties are shown in Table 4.

[0109] Comparative Example 2

[0110] 400g of PAO 6 synthetic oil (viscosity 5.69mm at 100℃) 2 90g of 12-hydroxystearic acid and 30g of sebacic acid were added to a reaction vessel, stirred and heated. At 80°C, an aqueous solution containing 26.5g of lithium hydroxide was added, and the reaction was carried out for 30 minutes. The temperature was then continuously raised to 210°C for high-temperature refining for 15 minutes. 460g of PAO 6 synthetic oil was added, and the mixture was cooled to 130°C. 2.5g of T351 and 2g of T706 were added. The mixture was then ground three times with a three-roll mill to obtain a comparative grease composition. Its properties are shown in Table 4.

[0111] Comparative Example 3

[0112] 400g of PAO 6 synthetic oil (viscosity 5.69mm at 100℃) 2 90g of 12-hydroxystearic acid and 30g of sebacic acid were added to a reaction vessel, stirred and heated. At 80°C, an aqueous solution containing 26.5g of lithium hydroxide was added, and the reaction was carried out for 30 minutes. The temperature was then continuously raised to 210°C for high-temperature refining for 15 minutes. 460g of PAO 6 synthetic oil was added, and the mixture was cooled to 130°C. 2.5g of V81 and 2g of T706 were added. The mixture was then ground three times with a three-roll mill to obtain a comparative grease composition. Its properties are shown in Table 4.

[0113] Comparative Example 4

[0114] 400g of PAO 6 synthetic oil (viscosity 5.69mm at 100℃) 2 90g of 12-hydroxystearic acid and 30g of sebacic acid were added to a reaction vessel, stirred and heated. At 80°C, an aqueous solution containing 26.5g of lithium hydroxide was added, and the reaction was carried out for 30 minutes. The temperature was then continuously raised to 210°C for high-temperature refining for 15 minutes. 460g of PAO 6 synthetic oil was added, and the mixture was cooled to 130°C. 2.5g of T306, 2.5g of V81, and 2g of T706 were added. The mixture was then ground three times with a three-roll mill to obtain a comparative grease composition. Its properties are shown in Table 4.

[0115] Comparative Example 5

[0116] 400g of PAO 6 synthetic oil (viscosity 5.69mm at 100℃) 2 90g of 12-hydroxystearic acid and 30g of sebacic acid were added to a reaction vessel, stirred and heated. At 80°C, an aqueous solution containing 26.5g of lithium hydroxide was added, and the reaction was carried out for 30 minutes. The temperature was then raised to 210°C and refined for 15 minutes. 460g of PAO 6 synthetic oil was added, and the mixture was cooled to 130°C. 2.5g of T351, 2.5g of V81, and 2g of T706 were added. The mixture was then ground three times with a three-roll mill to obtain a comparative grease composition. Its properties are shown in Table 4.

[0117] Table 3. Evaluation of Lubricating Grease Performance

[0118]

[0119] Table 4 Comparison of Lubricating Grease Performance Evaluation

[0120]

Claims

1. A grease composition, based on the total weight of the grease composition, comprising the following components: 65% to 90% base oil, 8% to 30% lithium-based thickener or complex lithium-based thickener, 0.1% to 2% rust inhibitor, and 0.1% to 5% organosulfur-phosphorus compound, wherein the organosulfur-phosphorus compound is one or more of the following structural compounds: 。 2. The lubricating grease composition according to claim 1, characterized in that, The method for preparing the organosulfur-phosphorus compound includes the following steps: (1) To react (α) compound with peroxide; The (α) compound is tert-butylated cashew nut shell; the peroxide is selected from one or more of hydrogen peroxide, peroxyformic acid, peracetic acid, persulfonic acid, m-chloroperoxybenzoic acid, tert-butyl hydroperoxide, tert-butyl peracetic acid, methyl ethyl ketone peroxide, benzoyl peroxide and cyclohexanone peroxide. (2) React the reaction product of step (1) with compound (β) and collect the product; The (β) compound is selected from one or more of phenylthiophosphonic acid, ethylthiophosphonic acid, and ethylthiophosphoric acid.

3. The lubricating grease composition according to claim 2, characterized in that, The equivalence ratio between (α) compounds and peroxides and (β) compounds is 1:0.5~10:0.5~10.

4. The lubricating grease composition according to claim 2, characterized in that, The reaction temperature in step (1) is 0~100℃; the reaction temperature in step (2) is 50~150℃.

5. The lubricating grease composition according to any one of claims 1 to 4, characterized in that, The base oil is a polyalphaolefin; the lithium-based thickener is obtained by saponification reaction of fatty acids and lithium hydroxide; the composite lithium-based thickener is obtained by saponification reaction of composite acids and lithium hydroxide; the rust inhibitor is selected from one or more of the following: organic carboxylic acid rust inhibitors, organic carboxylate rust inhibitors, organic amine rust inhibitors, ester rust inhibitors, sulfur-nitrogen heterocyclic rust inhibitors, and inorganic salt rust inhibitors.

6. A method for preparing the lubricating grease composition of claim 5, comprising: Add some base oil and all of the fatty acids or complex acids to the reaction vessel, stir and heat to 75℃~100℃, add lithium hydroxide aqueous solution to carry out saponification reaction; after the saponification reaction is completed, heat to 205~230℃ for high-temperature refining, and then add the remaining base oil; cool to 130℃ or below, add rust inhibitor and organosulfur and phosphorus compounds; grind into grease.

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