Salt-like compound thickener, grease and preparation method
By preparing a salt-like compound thickener composed of alternating ZrO6 octahedra and HPO4 tetrahedra, the problem of low viscoelasticity of layered zirconium phosphate gel was solved, efficient lubrication effect and simplified preparation process were achieved, reducing dependence on lithium resources.
Patent Information
- Application Number
- CN202311045484.7
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2023-08-18
- Publication Date
- 2025-09-12
- Estimated Expiration
- 2043-08-18
AI Technical Summary
When existing interlayer pillared N,N'-dimethylpiperazine layered zirconium phosphate materials and interlayer pillared quinoline layered zirconium phosphate materials are used as grease thickeners, the viscoelasticity of the gel is relatively low, and they are not suitable as thickeners.
A salt-like compound thickener is used, including layers alternately connected by ZrO6 octahedra and HPO4 tetrahedra and long-chain organic ions, which are prepared by a single hydrothermal synthesis method. The long-chain organic ions include single-long carbon chain or double-long carbon chain organic ammonium cations, with a carbon chain length of C12 to C20 and a grain size of 100 to 300 nm.
The thickening effect of grease is improved, the volume wear is as low as 1.67*10-4mm3, the average friction coefficient is 0.088, it has excellent lubrication effect, simplifies the preparation process, reduces dependence on lithium resources, and is suitable for a variety of actual working conditions.
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Figure CN117089382B_ABST
Abstract
Description
Technical Field
[0001] The present application belongs to the technical field of grease materials, and specifically relates to a salt-like compound thickener, grease, and a preparation method. Background Art
[0002] Grease is a widely used lubricant product that provides lubrication, sealing, and other protective functions. Its applications span a wide range of fields, including agriculture, mining, metallurgy, transportation, and aviation. Grease is a semi-solid lubricant composed of a base oil, a thickener, and additives. The thickener forms the grease's network structure, within which the base oil and additives are dispersed. The thickener's microstructure not only determines the base oil's thickening capacity and physical and chemical properties, but also has a significant impact on the grease's tribological performance.
[0003] Metal soaps are a classic thickener in lubricating greases. Traditional grease metal soaps are typically formed by the reaction of inorganic bases with fatty acids to form metal salts, forming soap fibers. Their basic structure consists of two components: an anion of a fatty carboxylic acid with an alkyl chain, and a metal cation. During the grease saponification process, the lipophilic metal soap molecules aggregate into soap fibers through ionic and van der Waals forces. The soap fibers attract each other, forming a three-dimensional gel network. The base oil is primarily fixed to the voids of the structural framework through capillary forces, adsorbed on the surface of the soap fibers, and penetrates into the interior. In other words, the long-chain organic metal salt self-assembles within the base oil to form the grease.
[0004] Among traditional metal soap-based greases, lithium-based greases are currently the most widely used. However, with the development of the new energy industry and the widespread use of lithium-ion batteries, the demand for lithium resources has skyrocketed. Lithium resources have become a strategic resource, and the status of lithium-based greases as general-purpose greases is increasingly threatened. Therefore, the development of new, sustainable, and environmentally friendly thickeners is imperative.
[0005] Zirconium phosphate materials can exhibit excellent tribological properties as lubricating additives. The applicant previously discovered that by adding interlayer pillared N,N'-dimethylpiperazine layered zirconium phosphate materials [C6H 16 N2] 0.5 Zr(H 0.5 PO4)2H2O or interlayer pillared quinoline layered zirconium phosphate materials (C9H8N)4(H2O)4[Zr8P 12 O 40(OH)8F8] as a grease additive can significantly improve the friction reduction and anti-wear ability of grease, see Chinese patents ZL201710262447.X. and ZL201710262446.5. However, the following problems exist in the application of the above-mentioned layered zirconium phosphate material as a grease thickener: The results of rheological studies show that the layered zirconium phosphate material of interlayer pillared N,N'-dimethylpiperazine and the layered zirconium phosphate material of interlayer pillared quinoline have the problem of low viscoelasticity of the gel when used as a thickener, and are not suitable as a thickener. Summary of the Invention
[0006] The purpose of the present application is to provide a salt-like compound thickener, grease and preparation method, which are used to solve the problem in the prior art that the layered zirconium phosphate materials of interlayer pillared N,N'-dimethylpiperazine and the layered zirconium phosphate materials of interlayer pillared quinoline have low viscoelasticity of the gel when used as thickeners, making them unsuitable as thickeners.
[0007] To achieve the above purpose, a technical solution adopted in this application is:
[0008] A salt-like compound thickener is provided, comprising layers and long-chain organic ions located between the layers. The layers comprise one or more metal oxides, and the layers and the long-chain organic ions have opposite charges.
[0009] In one or more embodiments, the layer is composed of ZrO6 octahedrons and HPO4 tetrahedrons connected alternately, and there is PO on the layer. - The anion, the long-chain organic ion includes a single-long carbon chain organic ammonium cation or a double-long carbon chain organic ammonium cation, the carbon chain length of the long-chain organic ion is C12 to C20, and the grain size of the salt-like compound thickener is 100 to 300 nm.
[0010] To achieve the above purpose, another technical solution adopted by this application is:
[0011] A method for preparing a salt-like compound thickener is provided, comprising the following steps:
[0012] Zirconium oxychloride octahydrate, deionized water, phosphoric acid and a long-chain organic ammonium salt are uniformly stirred and reacted at high temperature. After the reaction is completed, the mixture is washed and dried to obtain the salt-like compound thickener;
[0013] The long-chain organic ammonium salt includes a single-long carbon chain organic ammonium salt or a double-long carbon chain organic ammonium salt, and the carbon chain length of the long-chain organic ammonium salt is C12 to C20. The grain size of the salt-like compound thickener is 100 to 300 nm.
[0014] In one or more embodiments, the molar ratio of the zirconium oxychloride octahydrate, deionized water, phosphoric acid and long-chain organic ammonium salt is 1:(180-220):(6-10):(0.8-1.2), the temperature of the high-temperature reaction is 90-110° C., and the reaction time is 20-30 h.
[0015] In one or more embodiments, the long-chain organic ammonium salt is a linear or branched quaternary ammonium salt.
[0016] To achieve the above purpose, another technical solution adopted in this application is:
[0017] A lubricating grease is provided, comprising the following raw materials in percentage by weight:
[0018] 5-30% of the salt-like compound thickener described in any of the above embodiments;
[0019] Dispersant, 0.5-20%;
[0020] Antioxidant, 0.01-5%;
[0021] Rust inhibitor, 0.01-5%;
[0022] Extreme pressure anti-wear agent, 0.1-10%;
[0023] The balance is base oil.
[0024] In one or more embodiments, the weight percentage of the salt-like compound thickener is 5% to 25%, the weight percentage of the dispersant is 0.5 to 5%; the weight percentage of the antioxidant is 0.1 to 3%; the weight percentage of the rust inhibitor is 0.1 to 3%; and the weight percentage of the extreme pressure anti-wear agent is 0.5 to 5%.
[0025] In one or more embodiments, the dispersant comprises one or more combinations of methanol, ethanol, propanol, butanol, acetone, propylene carbonate, ethyl acetate, ethyl butyrate, ethyl hexanoate, and ethyl octanoate.
[0026] The antioxidant includes one or more combinations of amine antioxidants and phenolic antioxidants, wherein the amine antioxidant includes one or more combinations of naphthylamine, diphenylamine, p-phenylenediamine, and phenothiazine, and the phenolic antioxidant includes one or more combinations of 2,6-di-tert-butyl-p-cresol, butylated hydroxyanisole, tea polyphenols, vitamin C, tocopherol, and phytic acid;
[0027] The rust inhibitor comprises one or more combinations of dodecenylsuccinic acid T746, sodium petroleum sulfonate, barium dinonylnaphthalene sulfonate, zinc dinonylnaphthalene sulfonate, calcium dinonylnaphthalene sulfonate, dodecenylbutanediamine, N-oleoylsarcosine octadecylamine salt, 2-aminoethylheptadecenylimidazoline dodecenylbutanediamine, zinc naphthenate, aluminum stearate, benzotriazole and trisodium phosphate;
[0028] The extreme pressure anti-wear agent includes one or more combinations of sulfur-containing extreme pressure anti-wear agents, phosphorus-containing extreme pressure anti-wear agents and halogen extreme pressure anti-wear agents;
[0029] The base oil includes one or more combinations of mineral oil, synthetic oil, base oil derived from Fischer-Tropsch synthesis, alkyl naphthalene base oil derived from coal tar, and animal and vegetable oils.
[0030] In one or more embodiments, the volume wear of the grease under the conditions of load 200N, frequency 50Hz, step size 1mm, temperature 80℃, and time 30min is 1.67-2.15*10 -4 mm 3 , the average friction coefficient is 0.088~0.099.
[0031] To achieve the above purpose, another technical solution adopted in this application is:
[0032] A method for preparing the grease according to any of the above embodiments is provided, comprising the following steps:
[0033] The salt-like compound thickener is washed with water and centrifuged to obtain a sample; the sample is evenly mixed with the dispersant, ultrasonically treated for 0.5 to 2 hours, mixed with the base oil at room temperature, and thickened for 2 to 4 hours; after the thickening, the sample is aged in an oven at 100 to 150° C. for 3 to 5 hours; after cooling to room temperature, the antioxidant, the rust inhibitor, and the extreme pressure anti-wear agent are added, and the grease is ground with a grinder to obtain the grease.
[0034] To achieve the above purpose, another technical solution adopted in this application is:
[0035] A method for preparing the grease according to any of the above embodiments is provided, comprising the following steps:
[0036] The salt-like compound thickener is washed with water and centrifuged to obtain a sample; the sample is evenly mixed with the dispersant, ultrasonically treated for 0.5 to 2 hours, and then added to the base oil at 150 to 180° C. and thickened for 2 to 4 hours; after the thickening is completed, the sample is aged in an oven at 100 to 150° C. for 3 to 5 hours; after cooling to room temperature, the antioxidant, the rust inhibitor and the extreme pressure anti-wear agent are added, and the grease is ground with a grinder to obtain the grease.
[0037] To achieve the above purpose, another technical solution adopted in this application is:
[0038] A method for preparing the grease according to any of the above embodiments is provided, comprising the following steps:
[0039] The salt-like compound thickener is washed with water and centrifuged to obtain a sample; the sample and the dispersant are mixed evenly, ultrasonically treated for 0.5 to 2 hours, and then frozen to -10 to -25°C to obtain a frozen sample; the frozen sample is added to the base oil at 150 to 180°C and thickened for 2 to 4 hours; after the thickening is completed, the sample is aged in an oven at 100 to 150°C for 3 to 5 hours; after cooling to room temperature, the antioxidant, the rust inhibitor and the extreme pressure anti-wear agent are added, and the grease is ground with a grinder to obtain the grease.
[0040] Different from the prior art, the present invention has the following advantages:
[0041] Based on the "salt" structure of grease metal soap, this application proposes the concept of "salt-like compounds" as grease thickeners. Grease prepared with intercalated zirconium phosphate as a thickener has achieved excellent thickening effect. The prepared grease has typical grease characteristics. The volume wear of the grease prepared based on the salt-like compound thickener is as low as 1.67*10 -4 mm 3 , the average friction coefficient reaches 0.088, with excellent lubrication effect;
[0042] The salt-like compound thickener of the present application can regulate material properties such as interlayer spacing, host-guest interaction, particle size and morphology through synthetic means. The material preparation and product performance have the advantages of being adjustable and controllable, and are easy to produce on a large scale to meet the needs of various actual working conditions. It can alleviate the current grease market's heavy dependence on lithium resources.
[0043] The layer of the salt compound thickener of the present application is a metal oxide, and the grease generally has a high dropping point, good wide temperature characteristics, good colloidal stability, mechanical stability and oxidation stability;
[0044] The salt-like compound thickener of the present application not only thickens the base oil but also functions as an additive. The salt-like compound particles uniformly dispersed in the base oil will fill the rough contact surface of the friction pair as the friction pair moves. On the contact surface of the friction pair, there is not only an oil film of the base oil, but also a solid film and chemical film of the salt-like compound to prevent direct contact between the upper and lower friction pairs, thereby improving the wear performance of the contact surface and extending the service life of the equipment. The salt-like compound grease is a "dual-function" lubricant that has both grease characteristics and excellent tribological properties, providing a new path for the development of new grease thickener systems in the future.
[0045] The salt-like compound thickener of the present application is prepared by a single hydrothermal synthesis method. The presence of a long-chain organic base in the synthesis system helps to reduce the grain size of the salt-like compound thickener, increase the bonding strength between the long-chain organic ions and the base oil between the layers, and improve the thickening effect and the lubricating properties of the grease.
[0046] The lubricating grease of the present application is directly prepared using base oil and a salt-like compound thickener, thereby omitting the saponification reaction step and simplifying the preparation process. BRIEF DESCRIPTION OF THE DRAWINGS
[0047] Figure 1 is the XRD diffraction pattern of the thickener prepared in Examples 2 and 6;
[0048] Figure 2 is the XRD diffraction pattern of the thickener prepared in Examples 2, 8, and 9;
[0049] Figure 3 1 is the XRD diffraction pattern of the thickener prepared in Example 2 and Comparative Example 1;
[0050] Figure 4 is the viscoelasticity curve of the gel samples prepared from the greases of Examples 1 to 3;
[0051] Figure 5 is the viscoelasticity curve of the gel sample prepared from the grease of Examples 2, 4, and 5;
[0052] Figure 6 is the viscoelasticity curve of the gel samples prepared from the greases of Examples 2, 6, and 7;
[0053] Figure 7 is the viscoelasticity curve of the gel sample prepared from the grease of Examples 2, 8, and 9;
[0054] Figure 8 1 is the viscoelasticity curve of the gel samples prepared from the greases of Example 1 and Comparative Example 1;
[0055] Figure 9 2 are the viscoelasticity curves of the gel samples prepared from the greases of Example 2, Comparative Examples 2 and 3. DETAILED DESCRIPTION
[0056] The present application will be described in detail below in conjunction with various embodiments. However, these embodiments do not limit the present application, and any structural, methodological, or functional changes made by a person skilled in the art based on these embodiments are included within the scope of protection of the present application.
[0057] Metal soap-based grease thickeners are essentially long-chain fatty acid metal salts—salts composed of long-chain organic ions and metal ions. Lithium-based greases are currently the most widely used type of grease. These thickeners are derived from the saponification reaction of lithium hydroxide and fatty acids in a base oil. In recent years, with the development of the new energy industry and the widespread use of lithium-ion batteries, the demand for lithium resources has skyrocketed. Lithium has become a strategic resource, and the status of lithium-based greases as a general-purpose grease is increasingly under threat. Therefore, the development of new, sustainable, and environmentally friendly thickeners is imperative.
[0058] Based on the structure of existing metal soap-based grease thickeners, the applicant designed a class of salt-like compounds as thickeners. The crystal structure of this class of salt compounds is similar to that of metal soap salts and is also composed of two parts: one part is a charged layer composed of metal oxides, and the other part is a long-chain organic ion with a charge between the layers. This structural composition constitutes a compound similar to soap "salt". This patent refers to this compound as a "salt-like compound".
[0059] The selection types of long-chain organic ions in salt-like compounds are diverse. The material properties of salt-like compounds, such as interlayer spacing, host-guest interaction, grain size and morphology, can be regulated through synthetic means. The material preparation and product performance have the advantages of being adjustable and controllable, and can meet the needs of various actual working conditions.
[0060] The present application also specifically provides a salt-like compound thickener, wherein the layer of the salt-like compound is composed of ZrO6 octahedrons and HPO4 tetrahedrons alternately connected, and there is PO on the layer. - The anion and the long-chain organic ion include a single-long carbon chain organic ammonium cation or a double-long carbon chain organic ammonium cation. The carbon chain length of the long-chain organic ion is C12 to C20. The crystal size of the salt-like compound thickener is 100 to 300 nm.
[0061] Unlike the applicant's prior application for an organic amine-intercalated zirconium phosphate material, the salt-like compound thickener of this application functions as a thickener. Its smaller crystal size improves its dispersion in the base oil and strengthens its bond with oil molecules, thereby forming a structural framework and adsorbing and fixing the base oil. Furthermore, the organic hydrocarbon groups between the layers are long-chain organic hydrocarbons with a carbon chain length greater than 12, which are highly lipophilic. This further enhances the bond between the salt-like compound thickener and the base oil, thereby improving lubrication performance.
[0062] Based on this type of salt compound thickener, grease can be directly prepared using the salt compound thickener and base oil, which simplifies the preparation method, reduces the demand for metal resources such as lithium, and can improve the overall lubrication and anti-wear effects of the grease.
[0063] Specifically, the present application also provides a method for preparing the above-mentioned salt-like compound thickener, comprising the following steps:
[0064] Zirconium oxychloride octahydrate, deionized water, phosphoric acid and a long-chain organic ammonium salt are uniformly stirred and then placed in a reactor for high-temperature reaction. After the reaction is completed, the mixture is taken out, cleaned and dried to obtain a salt-like compound thickener.
[0065] The long-chain organic ammonium salt includes a single-long carbon chain organic ammonium salt or a double-long carbon chain organic ammonium salt, and the carbon chain length of the long-chain organic ammonium salt is C12 to C20, and the grain size of the salt-like compound thickener is 100 to 300 nm.
[0066] The molar ratio of zirconium oxychloride octahydrate, deionized water, phosphoric acid and long-chain organic ammonium salt can be 1:(180-220):(6-10):(0.8-1.2), the temperature of the high-temperature reaction can be 90-110° C., and the reaction time can be 20-30 h.
[0067] In one embodiment, the long-chain organic ammonium salt is a linear or branched quaternary ammonium salt, specifically, dodecyltrimethylammonium bromide, tetradecyltrimethylammonium bromide, hexadecyltrimethylammonium bromide and octadecyltrimethylammonium bromide, hexadecyldimethylethylammonium bromide, dodecyltrimethylammonium chloride, tetradecyltrimethylammonium chloride, hexadecyltrimethylammonium chloride and octadecyltrimethylammonium chloride or ditetradecyltrimethylammonium bromide, dihexadecyltrimethylammonium bromide and dioctadecyltrimethylammonium bromide, etc.
[0068] Compared with the traditional technology of preparing intercalated materials through methylamine pre-intercalation, the applicant used a one-time hydrothermal method to directly intercalate long-chain organic ammonium ions into the interlayers, which helps to reduce the grain size of the product, thereby improving the bonding strength with the base oil when used as a thickener.
[0069] The applicant also provides a grease composed of the following raw materials in weight percentage: the above-mentioned salt compound thickener, 5-30%; dispersant, 0.5-20%; antioxidant, 0.01-5%; rust inhibitor, 0.01-5%; extreme pressure anti-wear agent, 0.1-10%; and the balance is base oil.
[0070] In one embodiment, the weight percentage of the salt-like compound thickener is preferably 5% to 25%, the weight percentage of the dispersant is preferably 0.5 to 5%; the weight percentage of the antioxidant is preferably 0.1 to 3%; the weight percentage of the rust inhibitor is preferably 0.1 to 3%; and the weight percentage of the extreme pressure anti-wear agent is preferably 0.5 to 5%.
[0071] In another embodiment, the weight percentage of the salt-like compound thickener is preferably 10-20%.
[0072] In one embodiment, the antioxidant may include one or more combinations of amine antioxidants and phenolic antioxidants. Amine antioxidants may include naphthylamine, diphenylamine, p-phenylenediamine, phenothiazine, and the like; phenolic antioxidants may include 2,6-di-tert-butyl-p-cresol, butylated hydroxyanisole, tea polyphenols, vitamin C, tocopherol, phytic acid, and the like. Preferred antioxidants include 2,6-di-tert-butyl-4-methylphenol (BHT) and diphenylamine.
[0073] In one embodiment, the dispersant may include one or more combinations of methanol, ethanol, propanol, butanol, acetone, propylene carbonate, ethyl acetate, ethyl butyrate, ethyl hexanoate, and ethyl octanoate.
[0074] In one embodiment, the antioxidant may include one or more combinations of amine antioxidants and phenolic antioxidants, wherein the amine antioxidant may include one or more combinations of naphthylamine, diphenylamine, p-phenylenediamine, and phenothiazine, and the phenolic antioxidant may include one or more combinations of 2,6-di-tert-butyl-p-cresol, butylated hydroxyanisole, tea polyphenols, vitamin C, tocopherol, and phytic acid.
[0075] In one embodiment, the rust inhibitor may include one or more combinations of dodecenylsuccinate T746, sodium petroleum sulfonate, barium dinonylnaphthalene sulfonate, zinc dinonylnaphthalene sulfonate, calcium dinonylnaphthalene sulfonate, dodecenylbutanediamine, N-oleoylsarcosine octadecylamine salt, 2-aminoethylheptadecenylimidazoline dodecenylbutanediamine, zinc naphthenate, aluminum stearate, benzotriazole, and trisodium phosphate.
[0076] In one embodiment, the extreme pressure anti-wear agent may include one or more combinations of sulfur-containing extreme pressure anti-wear agents, phosphorus-containing extreme pressure anti-wear agents, and halogen-based extreme pressure anti-wear agents, such as zinc dialkyl dithiophosphate ZDDP, molybdenum dialkyl dithiophosphate MoDDP, sulfurized isobutylene T321, tricresyl phosphate, etc. Zinc dialkyl dithiophosphate ZDDP and molybdenum dialkyl dithiophosphate MoDDP are preferably used as extreme pressure anti-wear agents.
[0077] In one embodiment, the base oil may include one or more combinations of mineral oil, synthetic oil, base oil derived from Fischer-Tropsch synthesis, alkylated naphthalene base oil derived from coal tar, and animal and vegetable oils. Mineral oil may include paraffins and cycloalkanes produced by solvent treatment or hydroprocessing; synthetic oil may include polyalphaolefins, polyol esters, polyethers, and silicone oils, such as PAO8, dioctyl sebacate, and methyl silicone oil; mineral oil may include naphthenic mineral oil, paraffinic mineral oil, and intermediate base mineral oil, such as 500SN and 150BS; vegetable oil may include castor oil, soybean oil, coconut oil, cottonseed oil, palm oil, and peanut oil; and coal-to-liquids are downstream products produced from coal via direct or indirect liquefaction routes.
[0078] The technical solution of this application is further explained in detail below with reference to the accompanying drawings and specific implementation methods.
[0079] Example 1:
[0080] A lubricating grease is prepared by the following method:
[0081] According to the molar ratio of 1:200:8:1, zirconium oxychloride octahydrate (ZrOCl2·8H2O), water (H2O), phosphoric acid (H3PO4) and octadecyltrimethylammonium bromide (C 21 H 46 BrN) were added to 25 ml of polytetrafluoroethylene liner in sequence, and the drugs were fully stirred with a stirring rod. Then, the liner of the kettle was placed into the reactor and tightened. The kettle was placed in an oven at 100°C. After reacting in the oven for 1 day, the kettle was taken out and washed with distilled water. The product was air-dried at room temperature to obtain a salt-like compound thickener STAB-ZrP;
[0082] 5 parts by weight of a salt-like compound thickener STAB-ZrP were washed with hot water and centrifuged. 2 parts by weight of a dispersant were added and ultrasonically dispersed for 45 minutes. The mixed sample was then added to 92.4 parts of a naphthenic mineral base oil and thickened under magnetic stirring for 1 hour. The mixture was then aged in a 120°C oven for 5 hours and naturally cooled to room temperature. 0.5 parts by weight of an antioxidant diphenylamine and 0.1 parts by weight of zinc dialkyl dithiophosphate ZDDP were then added. The mixture was rolled three times on a three-roll mill to obtain a grease containing 5.0 wt% of nano-STAB-ZrP.
[0083] Example 2:
[0084] A lubricating grease is prepared by the following method:
[0085] According to the molar ratio of 1:200:8:1, zirconium oxychloride octahydrate (ZrOCl2·8H2O), water (H2O), phosphoric acid (H3PO4) and octadecyltrimethylammonium bromide (C 21 H 46 BrN) were added to 25 ml of polytetrafluoroethylene liner in sequence, and the drugs were fully stirred with a stirring rod. Then, the liner of the kettle was placed into the reactor and tightened. The kettle was placed in an oven at 100°C. After reacting in the oven for 1 day, the kettle was taken out and washed with distilled water. The product was air-dried at room temperature to obtain a salt-like compound thickener STAB-ZrP;
[0086] 10 parts by weight of a salt-like compound thickener STAB-ZrP was washed with hot water and centrifuged. 4 parts by weight of a dispersant was added and ultrasonically dispersed for 1 hour. The mixed sample was then added to 84.0 parts of a naphthenic mineral base oil and thickened by magnetic stirring for 1 hour. The mixture was then aged in a 120°C oven for 5 hours and naturally cooled to room temperature. 0.5 parts by weight of an antioxidant diphenylamine, 0.5 parts by weight of zinc dialkyl dithiophosphate ZDDP, and 0.1 parts of a rust inhibitor zinc naphthenate were then added. The mixture was rolled three times on a three-roll mill to obtain a grease containing 10.0 wt% of nano-STAB-ZrP.
[0087] Example 3:
[0088] A lubricating grease is prepared by the following method:
[0089] According to the molar ratio of 1:200:8:1, zirconium oxychloride octahydrate (ZrOCl2·8H2O), water (H2O), phosphoric acid (H3PO4) and octadecyltrimethylammonium bromide (C 21 H 46 BrN) were added to 25 ml of polytetrafluoroethylene liner in sequence, and the drugs were fully stirred with a stirring rod. Then, the liner of the kettle was placed into the reactor and tightened. The kettle was placed in an oven at 100°C. After reacting in the oven for 1 day, the kettle was taken out and washed with distilled water. The product was air-dried at room temperature to obtain a salt-like compound thickener STAB-ZrP;
[0090] 15 parts by weight of a salt-like compound thickener, STAB-ZrP, was washed with hot water and centrifuged. 5 parts by weight of a dispersant was added and ultrasonically dispersed for 1 hour. The mixed sample was then added to 78.5 parts of a naphthenic mineral base oil and thickened by magnetic stirring for 1 hour. The mixture was then aged in a 120°C oven for 5 hours and naturally cooled to room temperature. 0.5 parts by weight of diphenylamine, 0.5 parts by weight of molybdenum dialkyl dithiophosphate MoDDP, and 0.5 parts of a rust inhibitor, benzotriazole, were then added. The mixture was rolled three times on a three-roll mill to obtain a grease containing 15.0 wt% of nano-STAB-ZrP.
[0091] Example 4:
[0092] A lubricating grease is prepared by the following method:
[0093] According to the molar ratio of 1:200:8:1, zirconium oxychloride octahydrate (ZrOCl2·8H2O), water (H2O), phosphoric acid (H3PO4) and octadecyltrimethylammonium bromide (C 21 H 46BrN) were added to 25 ml of polytetrafluoroethylene liner in sequence, and the drugs were fully stirred with a stirring rod. Then, the liner of the kettle was placed into the reactor and tightened. The kettle was placed in an oven at 100°C and reacted in the oven for 1 day. After that, the sample was taken out and washed with distilled water. The product was air-dried at room temperature to obtain a salt-like compound thickener SMAB-ZrP;
[0094] 10 parts by weight of a salt-like compound thickener SMAB-ZrP was first washed with hot water and centrifuged, and 4 parts by weight of a dispersant was added. After ultrasonic dispersion for 1 hour, the evenly mixed sample was slowly added to 84.9 parts by weight of a mixed base oil of PAO8 oil and cycloalkyl oil preheated to 150°C. After thickening under magnetic stirring for 2 hours, it was placed in a 150°C oven for aging for 5 hours, naturally cooled to room temperature, and then 0.5 parts by weight of zinc dialkyl dithiophosphate ZDDP, 0.5 parts by weight of an antioxidant 2,6-di-tert-butyl-p-cresol, and 0.1 parts of a rust inhibitor zinc cycloalkylate were added. The grease was rolled three times on a three-roll mill to obtain a grease containing 10.0 wt% of nano-STAB-ZrP.
[0095] Example 5:
[0096] A lubricating grease is prepared by the following method:
[0097] According to the molar ratio of 1:200:8:1, zirconium oxychloride octahydrate (ZrOCl2·8H2O), water (H2O), phosphoric acid (H3PO4) and octadecyltrimethylammonium bromide (C 21 H 46 BrN) were added to 25 ml of polytetrafluoroethylene liner in sequence, and the drugs were fully stirred with a stirring rod. Then, the liner of the kettle was placed into the reactor and tightened. The kettle was placed in an oven at 100°C. After reacting in the oven for 1 day, the kettle was taken out and washed with distilled water. The product was air-dried at room temperature to obtain a salt-like compound thickener STAB-ZrP;
[0098] 10 parts by weight of a salt-like compound thickener STAB-ZrP were washed with hot water and centrifuged, and 4 parts by weight of a dispersant were added. After ultrasonic dispersion for 1 hour, the sample was first frozen to -25°C, and then 85.5 parts by weight of a base oil mixed with PAO8 and alkyl naphthalene, which had been preheated to 150°C, was slowly added to the frozen sample. After thickening under magnetic stirring for 3 hours, the sample was placed in a 150°C oven for aging for 5 hours, naturally cooled to room temperature, and then 0.5 parts by weight of zinc dialkyl dithiophosphate ZDDP, 0.5 parts by weight of an antioxidant 2,6-di-tert-butyl-p-cresol, and 0.5 parts of a rust inhibitor trisodium phosphate were added. The sample was rolled three times on a three-roll mill to obtain a grease containing 10.0 wt% of nano-STAB-ZrP.
[0099] Example 6:
[0100] A lubricating grease is prepared by the following method:
[0101] According to the molar ratio of 1:200:8:1, zirconium oxychloride octahydrate (ZrOCl2·8H2O), water (H2O), phosphoric acid (H3PO4) and dioctadecyltrimethylammonium bromide (C 38 H 80 BrN), and added into 25 ml of polytetrafluoroethylene liner in sequence, and stirred the drugs thoroughly with a stirring rod. Then, the liner of the kettle was placed into the reactor and tightened, and the kettle was placed in an oven at 100 ° C. After reacting in the oven for 1 day, it was taken out and washed with distilled water. The product was air-dried at room temperature to obtain a salt-like compound thickener DSAB-ZrP;
[0102] 10 parts by weight of a salt-like compound thickener DSAB-ZrP were washed with hot water and centrifuged, and 3 parts by weight of a dispersant were added. After ultrasonic dispersion, the uniformly mixed sample was thickened with 85.5 parts by weight of a base oil mixed with PAO8 and castor oil. After thickening under magnetic stirring for 3 hours, the sample was placed in a 100°C oven for aging for 5 hours, naturally cooled to room temperature, and then 0.5 parts by weight of dialkyl dithiophosphate molybdenum MoDDP, 0.5 parts by weight of an antioxidant 2,6-di-tert-butyl-p-cresol, and 0.5 parts of a rust inhibitor zinc naphthenate were added. The grease was rolled three times on a three-roll mill to obtain a grease containing 10.0 wt% of nano-DSAB-ZrP.
[0103] Example 7:
[0104] A lubricating grease is prepared by the following method:
[0105] According to the molar ratio of 0.8:200:8:1, zirconium oxychloride octahydrate (ZrOCl2·8H2O), water (H2O), phosphoric acid (H3PO4) and dioctadecyltrimethylammonium bromide (C 38 H 80 BrN), and added into 25 ml of polytetrafluoroethylene liner in sequence, and stirred the drugs thoroughly with a stirring rod. Then, the liner of the kettle was placed into the reactor and tightened, and the kettle was placed in an oven at 100 ° C. After reacting in the oven for 1 day, it was taken out and washed with distilled water. The product was air-dried at room temperature to obtain a salt-like compound thickener DSAB-ZrP;
[0106] 10 parts by weight of a salt-like compound thickener DSAB-ZrP was washed with hot water and centrifuged, and 5 parts by weight of a dispersant was added. After ultrasonic dispersion for 1 hour, the uniformly mixed sample was slowly added with 83.5 parts by weight of a base oil mixed with PAO8 and alkylnaphthalene that had been preheated to 150°C. After thickening under magnetic stirring for 3 hours, the sample was placed in a 100°C oven for aging for 5 hours, naturally cooled to room temperature, and then 0.5 parts by weight of zinc dialkyl dithiophosphate ZDDP, 0.5 parts by weight of an antioxidant 2,6-di-tert-butyl-p-cresol, and 0.5 parts of a rust inhibitor zinc naphthenate were added. The sample was rolled three times on a three-roll mill to obtain a grease containing 10.0 wt% of nano-DSAB-ZrP.
[0107] Example 8:
[0108] A lubricating grease is prepared by the following method:
[0109] According to the molar ratio of 1.5:200:8:1, zirconium oxychloride octahydrate (ZrOCl2·8H2O), water (H2O), phosphoric acid (H3PO4) and tetradecyltrimethylammonium bromide (C 17 H 38 BrN) were added to 25 ml of polytetrafluoroethylene liner in sequence, and the drugs were fully stirred with a stirring rod. Then, the liner of the kettle was placed into the reactor and tightened. The kettle was placed in an oven at 100°C. After reacting in the oven for 1 day, the kettle was taken out and washed with distilled water. The product was air-dried at room temperature to obtain a salt-like compound thickener MTAB-ZrP;
[0110] 10 parts by weight of the salt-like compound thickener MTAB-ZrP were first washed with hot water and centrifuged, and 5 parts by weight of a dispersant were added. After ultrasonic dispersion for 1 hour, the uniformly mixed sample was added to 83.9 parts by weight of a cycloalkyl mineral oil base oil. After magnetic stirring for 1 hour, the mixture was placed in a 120°C oven and heated for 5 hours. The mixture was naturally cooled to room temperature, and then 0.5 parts by weight of an antioxidant diphenylamine, 0.5 parts by weight of zinc dialkyl dithiophosphate ZDDP, and 0.1 parts of a rust inhibitor zinc cyclohexane were added. The mixture was rolled three times on a three-roll mill to obtain a grease containing 10.0 wt% of nano-MTAB-ZrP.
[0111] Example 9:
[0112] A lubricating grease is prepared by the following method:
[0113] According to the molar ratio of 1.2:200:8:1, zirconium oxychloride octahydrate (ZrOCl2·8H2O), water (H2O), phosphoric acid (H3PO4) and hexadecyltrimethylammonium bromide (C 19 H 42 BrN), and added into 25 ml of polytetrafluoroethylene liner in sequence, and stirred the drugs thoroughly with a stirring rod. Then, the liner of the kettle was placed into the reactor and tightened, and the kettle was placed in an oven at 100 ° C. After reacting in the oven for 1 day, it was taken out and washed with distilled water. The product was air-dried at room temperature to obtain a salt-like compound thickener CTAB-ZrP;
[0114] 10 parts by weight of a salt-like compound thickener CTAB-ZrP was washed with hot water and centrifuged. 5 parts by weight of a dispersant was added and ultrasonically dispersed for 1 hour. The uniformly mixed sample was then added to 83.9 parts by weight of a cycloalkyl mineral oil base oil. The mixture was magnetically stirred for 2 hours and then heated in a 150°C oven for 5 hours. The mixture was naturally cooled to room temperature. 0.5 parts by weight of an antioxidant diphenylamine, 0.5 parts by weight of zinc dialkyl dithiophosphate ZDDP, and 0.1 parts of a rust inhibitor zinc naphthenate were then added. The mixture was rolled three times on a three-roll mill to obtain a grease containing 10.0 wt% of nano-CTAB-ZrP.
[0115] Comparative Example 1:
[0116] A lubricating grease is prepared by the following method:
[0117] Methylamine, α-zirconium phosphate and octadecyltrimethylammonium bromide (C 21 H 46 BrN), firstly prepare a methylamine pre-intercalated α-zirconium phosphate suspension with methylamine and α-zirconium phosphate, then add octadecyltrimethylammonium bromide to the suspension, stir at room temperature for 24 hours, and the product is centrifuged, washed with distilled water, and dried at room temperature to obtain a thickener M-STAB-ZrP;
[0118] 5 parts by weight of thickener M-STAB-ZrP were washed with hot water and centrifuged. 2 parts by weight of a dispersant was added and ultrasonically dispersed for 45 minutes. The mixed sample was then added to 92.4 parts of a naphthenic mineral base oil. After thickening under magnetic stirring for 1 hour, the sample was aged in a 120°C oven for 5 hours and naturally cooled to room temperature. 0.5 parts by weight of antioxidant diphenylamine and 0.1 parts by weight of zinc dialkyl dithiophosphate ZDDP were then added. The grease was rolled three times on a three-roll mill to obtain a grease containing 5.0 wt% of M-STAB-ZrP.
[0119] Comparative Example 2:
[0120] A lubricating grease is prepared by the following method:
[0121] Zirconium oxychloride octahydrate (ZrOCl2·8H20), water, phosphoric acid, hydrofluoric acid, and N,N'-dimethylpiperazine were weighed in a molar ratio of 1.0:83:2.0:4.0:3.0 and added sequentially to a 25 ml polytetrafluoroethylene liner. The chemicals were fully stirred with a stirring rod. The liner was then placed in a reactor, tightened, and placed in an oven at 180°C. After reacting in the oven for 72 hours, the reactor was taken out, washed, and air-dried at room temperature to obtain layered zirconium phosphate ZrPO4-DES8 with N,N'-dimethylpiperazine as the thickener interlayer pillar.
[0122] 10 parts by weight of thickener ZrPO4-DES8 were first washed with hot water and centrifuged, and then 4 parts by weight of dispersant were added. After ultrasonic dispersion for 1 hour, the evenly mixed sample was added with 84.0 parts of cycloalkyl mineral oil base oil. After magnetic stirring and thickening for 1 hour, it was placed in a 120°C oven for aging for 5 hours, and naturally cooled to room temperature. Then, 0.5 parts by weight of antioxidant diphenylamine, 0.5 parts by weight of dialkyl dithiophosphate zinc ZDDP and 0.1 parts of rust inhibitor zinc cyclohexane were added, and the mixture was rolled three times on a three-roll mill to obtain a grease containing 10.0wt% ZrPO4-DES8.
[0123] Comparative Example 3:
[0124] A lubricating grease is prepared by the following method:
[0125] Zirconium oxychloride octahydrate (ZrOCl2·8H20), water, phosphoric acid, hydrofluoric acid, and quinoline were weighed in a molar ratio of 1:91:2:2:3 and added sequentially to a 25 ml polytetrafluoroethylene liner. The chemicals were fully stirred with a stirring rod. The liner was then placed in a reactor, tightened, and placed in an oven at 180°C. After reacting in the oven for 5 days, the reactor was removed, washed, and air-dried at room temperature to obtain layered zirconium phosphate ZrPOF-Q1 with quinoline as the thickener interlayer pillar.
[0126] 10 parts by weight of thickener ZrPOF-Q1 were washed with hot water and centrifuged, and then 4 parts by weight of dispersant were added. After ultrasonic dispersion for 1 hour, the mixed sample was added with 84.0 parts of cycloalkyl mineral oil base oil. After magnetic stirring and thickening for 1 hour, it was placed in a 120°C oven for aging for 5 hours and naturally cooled to room temperature. Then, 0.5 parts by weight of antioxidant diphenylamine, 0.5 parts by weight of zinc dialkyl dithiophosphate ZDDP and 0.1 parts of rust inhibitor zinc cyclohexane were added, and the mixture was rolled three times on a three-roll mill to obtain a grease containing 10.0wt% of ZrPOF-Q1.
[0127] Effect Example 1: Characterization Analysis
[0128] The crystal structures of the thickeners prepared in Examples 2, 6, 8, 9 and Comparative Example 1 were characterized and analyzed using X-ray powder diffractometer (XRD). Figures 1 to 3 The test conditions are scanning angle 2-40°, tube voltage 30kV, current 15mA, scanning speed 4°min -1 .
[0129] in, Figure 1 is the XRD diffraction pattern of the thickener prepared in Examples 2 and 6, Figure 2 is the XRD diffraction pattern of the thickener prepared in Examples 2, 8, and 9, Figure 3 2 are XRD diffraction patterns of the thickeners prepared in Example 2 and Comparative Example 1.
[0130] As shown in the figure, the thickeners prepared in Examples 2, 6, 8, and 9 and Comparative Example 1 exhibit essentially identical physical properties, all possessing a structure with long-chain organic ammonium cations inserted between layers. Calculations indicate that the crystal sizes of the thickeners prepared in Examples 2, 6, 8, and 9 range from 100 to 300 nm. Smaller crystal sizes contribute to improved thickening effects on grease.
[0131] Effect Example 2:
[0132] The rheological characterization of the gel samples prepared from the greases of Examples 1 to 9 and Comparative Examples 1 to 3 was performed using an Anton Paar 302 rheological analyzer. The viscoelasticity of the gel was analyzed using an oscillating mode, and the measurement system used a rotor (radius: 25 mm) and a frosted plate (plate gap: 1 mm) to obtain the following: Figures 4 to 9 .
[0133] in, Figure 4 is the viscoelasticity curve of the gel samples prepared from the greases of Examples 1 to 3; Figure 5 is the viscoelasticity curve of the gel sample prepared from the grease of Examples 2, 4, and 5; Figure 6 is the viscoelasticity curve of the gel samples prepared from the greases of Examples 2, 6, and 7; Figure 7 is the viscoelasticity curve of the gel sample prepared from the grease of Examples 2, 8, and 9; Figure 8 1 is the viscoelasticity curve of the gel samples prepared from the greases of Example 1 and Comparative Example 1; Figure 9 2 are the viscoelasticity curves of the gel samples prepared from the greases of Example 2, Comparative Examples 2 and 3.
[0134] See also Figure 4 The storage modulus (G') of the gel samples of Example 1, Example 2 and Example 3 are 20805Pa, 44219Pa and 50188Pa, respectively. It can be seen that under the same shear strain conditions, the viscoelasticity of the gel samples increases with the increase of the addition amount of nano-STAB-ZrP.
[0135] See also Figure 5 The storage moduli (G') of the gel samples from Examples 2, 4, and 5 were 44219 Pa, 50289 Pa, and 39274 Pa, respectively. All three examples, containing 10.0 wt% nano-STAB-ZrP, achieved excellent thickening results. Example 2 employed a room-temperature thickening process, with the base oil maintained at room temperature; Example 4 employed a room-temperature puffing process, with the base oil preheated; and Example 5 employed a low-temperature puffing process, with the sample pre-frozen and then mixed with the preheated base oil.
[0136] From the above data, it can be seen that for the 10.0wt% nano-STAB-ZrP gel samples prepared by different thickening processes, under the same shear strain conditions, the viscoelasticity of the room temperature expanded gel sample is the highest, followed by the room temperature thickening, and the low temperature expansion is the lowest.
[0137] See also Figure 6 The storage modulus (G') of the gel samples of Example 2, Example 6 and Example 7 were 44219Pa, 20850Pa and 22176Pa, respectively. Both Example 6 and Example 7 achieved excellent thickening effects, but the thickening effect of 10.0wt% nano-DSAB-ZrP prepared in Examples 6 and 7 was weaker than that of Example 2. At the same time, Example 6 adopted a room temperature thickening process, and Example 7 adopted a room temperature puffing process, and the viscoelastic values of the two were similar.
[0138] See also Figure 7 The storage moduli (G') of the gel samples of Examples 2, 8, and 9 were 44219 Pa, 27258 Pa, and 36615 Pa, respectively. Both Examples 8 and 9 achieved excellent thickening effects. These data indicate that, under the same room-temperature thickening process, the longer the interlayer organic base carbon chain, the better the thickening effect. Specifically, the STAB-ZrP gel sample of Example 2 exhibited the highest viscoelasticity, followed by the CTAB-ZrP gel sample of Example 9 and the MTAB-ZrP gel sample of Example 8.
[0139] See also Figure 8 The storage moduli (G') of the gel samples of Example 1 and Comparative Example 1 were 20805 Pa and 1978 Pa, respectively, indicating that the thickening effect of Comparative Example 1 was very poor. This is mainly because, under the same room temperature thickening process and the same addition amount, the viscoelasticity of the micro-STAB-ZrP gel sample prepared by methylamine pre-intercalation was significantly lower than that of the nano-STAB-ZrP gel sample.
[0140] See also Figure 9 The storage moduli (G') of the gel samples of Example 2, Comparative Example 2, and Comparative Example 3 were 44219 Pa, 905 Pa, and 71 Pa, respectively. The thickening effects of Comparative Examples 2 and 3 were very poor. The above data indicate that the interlayer-pillared N,N'-dimethylpiperazine layered zirconium phosphate material and the interlayer-pillared quinoline layered zirconium phosphate material are not suitable for use as grease thickeners.
[0141] The salt-like thickener of interlayer long-chain organic ions of the present application can significantly enhance the thickening effect of grease and improve the viscoelastic value of the grease product.
[0142] Effect Example 3: Lubrication Performance Test
[0143] The friction reduction and anti-wear properties of the gel samples prepared from the greases of Examples 1 to 9 and Comparative Examples 1 to 3 were characterized using an Optimol SRV-V tribometer from Germany and in accordance with ASTM D5707-14. The data in the table below are obtained. Specifically, the friction pair employed a ball-on-disc contact mechanism, consisting of an upper steel ball and a lower steel disc. During operation, the lower specimen was fixed while the upper specimen reciprocated. The SRV automatically outputs and records real-time dynamic friction coefficient curves, and volumetric wear was measured using a 3D white-light interferometer.
[0144]
[0145]
[0146] As can be seen from the data in the table above, the volume wear of the greases prepared in Examples 1 to 6 ranges from 1.67 to 2.15*10 -4 mm 3 The average friction coefficient is between 0.088 and 0.099, and the volume wear of the grease prepared in Example 3 is as low as 1.67*10 -4 mm 3 , the average friction coefficient reached 0.088.
[0147] Comparing the data of Examples 1 to 3, it can be seen that as the amount of STAB-ZrP added increases, the friction reduction and anti-wear performance is enhanced.
[0148] Comparing the data of Examples 2, 4, and 5, it can be seen that the friction reduction and anti-wear properties of Example 4 using the room temperature puffing process and Example 5 using the low temperature puffing process are similar, but both are weaker than Example 2 using the room temperature thickening process.
[0149] Comparing the data of Examples 2, 6, and 7, it can be seen that the anti-friction and anti-wear properties of the 10.0 wt% nano-DSAB-ZrP gel samples prepared by the room temperature thickening process of Example 6 and the room temperature puffing process of Example 7 are similar, and the anti-wear properties are slightly better than that of Example 2.
[0150] Comparing the data of Examples 2, 8 and 9, it can be seen that under the same room temperature thickening process, the longer the carbon chain of the organic base between the layers, the better the friction reduction and anti-wear performance.
[0151] Comparing the data of Examples 2, 3 and Comparative Examples 1 to 3, it can be seen that the friction reduction and anti-wear performance of Comparative Examples 1 to 3 is significantly weaker than that of Example 2 and Example 3, and the friction reduction and anti-wear performance of Comparative Example 1 is better than that of Comparative Examples 2 and 3. The presence of interlayer long-chain organic ions not only helps to thicken the base oil, but also helps to improve the friction performance. The salt-type thickener of interlayer long-chain organic ions in this application can significantly enhance the friction reduction and anti-wear performance of grease compared with the existing interlayer pillared N,N'-dimethylpiperazine layered zirconium phosphate material and interlayer pillared quinoline layered zirconium phosphate material.
[0152] The foregoing description of the present disclosure is provided to enable any person skilled in the art to implement or use the present disclosure. Various modifications to the present disclosure will be readily apparent to those skilled in the art, and the general principles herein may be applied to other variations without departing from the scope of the present disclosure. Therefore, the present disclosure is not limited to the examples and designs described herein, but is intended to be consistent with the widest range of principles and novel features disclosed herein.
Claims
1. A lubricating grease, characterized in that: It is composed of the following raw materials in weight percentage: Salt compound thickener, 5~30%; Dispersant, 0.5~20%; Antioxidant, 0.01~5%; Rust inhibitor, 0.01~5%; Extreme pressure anti-wear agent, 0.1~10%; The balance is base oil; The salt-like compound thickener comprises layers and long-chain organic ions located between the layers, the layers comprise one or more metal oxides, and the layers and the long-chain organic ions have opposite charges; The layer is composed of ZrO6 octahedrons and HPO4 tetrahedrons connected alternately, and there is PO on the layer. - The anion, the long-chain organic ion includes a single-long carbon chain organic ammonium cation or a double-long carbon chain organic ammonium cation, the carbon chain length of the long-chain organic ion is C12~C20, and the grain size of the salt-like compound thickener is 100~300nm.
2. The lubricating grease according to claim 1, characterized in that The preparation method of the salt-like compound thickener comprises the following steps: Zirconium oxychloride octahydrate, deionized water, phosphoric acid and a long-chain organic ammonium salt are uniformly stirred and reacted at high temperature. After the reaction is completed, the salt-like compound thickener is obtained by washing and drying.
3. The lubricating grease according to claim 2, characterized in that The molar ratio of the zirconium oxychloride octahydrate, deionized water, phosphoric acid and long-chain organic ammonium salt is 1:(180-220):(6-10):(0.8-1.2), the temperature of the high-temperature reaction is 90-110° C., and the reaction time is 20-30 hours.
4. The lubricating grease according to claim 1, wherein The weight percentage of the salt-like compound thickener is 5-25%, the weight percentage of the dispersant is 0.5-5%, the weight percentage of the antioxidant is 0.1-3%, the weight percentage of the rust inhibitor is 0.1-3%, and the weight percentage of the extreme pressure anti-wear agent is 0.5-5%.
5. The lubricating grease according to claim 1, wherein The dispersant comprises one or more of methanol, ethanol, propanol, butanol, acetone, propylene carbonate, ethyl acetate, ethyl butyrate, ethyl hexanoate, and ethyl octanoate; The antioxidant includes one or more combinations of amine antioxidants and phenolic antioxidants, wherein the amine antioxidant includes one or more combinations of naphthylamine, diphenylamine, p-phenylenediamine, and phenothiazine, and the phenolic antioxidant includes one or more combinations of 2,6-di-tert-butyl-p-cresol, butylated hydroxyanisole, tea polyphenols, vitamin C, tocopherol, and phytic acid; The rust inhibitor comprises one or more combinations of dodecenylsuccinic acid T746, sodium petroleum sulfonate, barium dinonylnaphthalene sulfonate, zinc dinonylnaphthalene sulfonate, calcium dinonylnaphthalene sulfonate, dodecenylbutanediamine, N-oleoylsarcosine octadecylamine salt, 2-aminoethylheptadecenylimidazoline dodecenylbutanediamine, zinc naphthenate, aluminum stearate, benzotriazole and trisodium phosphate; The extreme pressure anti-wear agent includes one or more combinations of sulfur-containing extreme pressure anti-wear agents, phosphorus-containing extreme pressure anti-wear agents and halogen extreme pressure anti-wear agents; The base oil includes one or more combinations of mineral oil, synthetic oil, base oil derived from Fischer-Tropsch synthesis, alkyl naphthalene base oil derived from coal tar, and animal and vegetable oils.
6. The lubricating grease according to claim 1, wherein The volume wear of the grease under the conditions of load 200 N, frequency 50 Hz, step size 1 mm, temperature 80 ℃, and time 30 min is 1.67~2.15×10 -4 mm 3 , the average friction coefficient is 0.088~0.
099.
7. A method for preparing the lubricating grease according to any one of claims 1 to 6, characterized in that: include: The salt-like compound thickener is washed with water and centrifuged to obtain a sample; the sample is evenly mixed with the dispersant, ultrasonically treated for 0.5 to 2 hours, mixed with the base oil at room temperature, and thickened for 2 to 4 hours; after the thickening, the sample is aged in an oven at 100 to 150° C. for 3 to 5 hours; after cooling to room temperature, the antioxidant, the rust inhibitor, and the extreme pressure anti-wear agent are added, and the grease is ground using a grinder to obtain the grease.
8. A method for preparing the lubricating grease according to any one of claims 1 to 6, characterized in that: include: washing the salt-like compound thickener with water, and centrifuging to obtain a sample; The sample and the dispersant are mixed evenly, ultrasonically treated for 0.5 to 2 hours, and then added to the base oil at 150 to 180° C. and thickened for 2 to 4 hours. After the thickening is completed, the sample is aged in an oven at 100 to 150° C. for 3 to 5 hours. After cooling to room temperature, the antioxidant, the rust inhibitor and the extreme pressure anti-wear agent are added, and the grease is ground with a grinder to obtain the grease.
9. A method for preparing the lubricating grease according to any one of claims 1 to 6, characterized in that: include: The salt-like compound thickener is washed with water and centrifuged to obtain a sample; the sample and the dispersant are mixed evenly, ultrasonically treated for 0.5 to 2 hours, and then frozen to -10 to 25°C to obtain a frozen sample; the frozen sample is added to the base oil at 150 to 180°C and thickened for 2 to 4 hours; after the thickening is completed, the sample is aged in an oven at 100 to 150°C for 3 to 5 hours; after cooling to room temperature, the antioxidant, the rust inhibitor and the extreme pressure anti-wear agent are added, and the grease is ground with a grinder to obtain the grease.
Citation Information
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