A composite lubricating composition and preparation method thereof

Abstract

The present invention belongs to the technical field of lubricating materials, and specifically relates to a composite lubricating composition and a preparation method thereof. The composite lubricating composition comprises the following components by weight: 100-200 parts of modified phenolic resin, 20-30 parts of solid lubricant, 5-20 parts of polytetrafluoroethylene, 10-20 parts of fiber-reinforced material, 5-15 parts of polymer elastomer, 10-20 parts of tackifier, 15-25 parts of coupling agent, and 2-5 parts of antioxidant. The composite lubricating composition provided by the present invention has a lower wear rate and friction coefficient, and excellent overall performance.

Description

Technical Field

[0001] The invention belongs to the technical field of lubricating materials, and in particular relates to a composite lubricating composition and a preparation method thereof. Background Art

[0002] With the rapid development of modern industry, the performance requirements for lubricating materials are increasing day by day. In many working conditions, such as high temperature, high pressure, high load and other harsh environments, traditional lubricating materials are often difficult to meet the needs. Phenolic resin has the advantages of good heat resistance, mechanical properties and chemical stability. It has broad application prospects to develop composite lubricating materials based on it as a basic material. For example, in the field of mechanical manufacturing, phenolic resin-based composite lubricating materials can be made into wear-resistant parts such as sleeves and gaskets, which are used in various mechanical transmission devices; in the field of aerospace, phenolic resin-based composite lubricating materials are used in engine bearings, seals and other parts to ensure the normal operation of the engine and improve the reliability and service life of the engine.

[0003] Although phenolic resin has many advantages, it also has some limitations, such as high brittleness. In order to improve these properties, phenolic resin needs to be modified or compounded with other materials. Summary of the invention

[0004] In view of the deficiencies in the prior art, the present invention provides a composite lubricating composition and a preparation method thereof.

[0005] The invention provides a composite lubricating composition, which comprises the following components in parts by weight: 100-200 parts of modified phenolic resin, 20-30 parts of solid lubricant, 5-20 parts of polytetrafluoroethylene, 10-20 parts of fiber reinforcement material, 5-15 parts of polymer elastomer, 10-20 parts of tackifier, 15-25 parts of coupling agent and 2-5 parts of antioxidant, wherein the modified phenolic resin is obtained by modifying the phenolic resin with an organic silicon compound, and the molar ratio of the organic silicon compound to the phenolic resin is less than or equal to 1:2.

[0006] Preferably, the composite lubricating composition comprises the following components in parts by weight: 120-180 parts of modified phenolic resin, 22-28 parts of solid lubricant, 10-15 parts of polytetrafluoroethylene, 15-20 parts of fiber reinforcement material, 8-15 parts of polymer elastomer, 15-18 parts of tackifier, 18-20 parts of coupling agent, and 2-4 parts of antioxidant.

[0007] The modified phenolic resin may be 100 parts, 120 parts, 140 parts, 160 parts, 180 parts, 200 parts, etc.

[0008] The solid lubricant 20-30 parts can be 20 parts, 21 parts, 22 parts, 23 parts, 24 parts, 25 parts, 26 parts, 27 parts, 28 parts, 29 parts, 30 parts. The solid lubricant has a layered or lamellar crystal structure. During the friction process, these layered structures can slide relatively between two friction surfaces, thereby converting the direct friction between the solids into the internal friction between the solid lubricant layers, so that the friction coefficient is reduced. In addition, the solid lubricant can also reduce the wear of the composite lubricating composition, improve its load-bearing capacity, improve high temperature performance, etc.

[0009] Preferably, the modified phenolic resin is obtained by modifying the phenolic resin with an organic silicon compound, wherein the organic silicon compound is methyl silicone oil or amino silicone oil. After modification, the phenolic resin can be endowed with excellent demoulding property, temperature resistance and self-lubricating property, so that the composite lubricating composition can still maintain a good lubricating effect in a high temperature environment.

[0010] Preferably, the organosilicon compound modified phenolic resin to obtain the modified phenolic resin comprises the following steps:

[0011] Step 1: Add the organosilicon compound and the solvent into a reaction kettle, heat to 30°C-40°C and stir evenly, add the catalyst, continue stirring and reacting for 0.5-1h to obtain an organosilicon prepolymer;

[0012] Step 2: Add the phenolic resin to another reaction kettle, add the solvent, heat to 40°C-60°C, and stir for 0.5-1h to completely dissolve the phenolic resin;

[0013] Step 3: slowly add the organosilicon prepolymer prepared in step 1 to the dissolved phenolic resin so that the molar ratio of the organosilicon prepolymer to the phenolic resin is less than or equal to 1:2, heat to 70°C-100°C, and keep stirring for 1-2h;

[0014] Step 4: After the reaction is completed, the product is filtered, washed, and dried to obtain a modified phenolic resin.

[0015] After the phenolic resin is modified with silicone, the heat resistance and water resistance of the composite lubricating composition can be improved, and its friction performance, toughness and impact resistance can also be improved; the processing performance can also be optimized. The melt viscosity of the phenolic resin modified with silicone is reduced and the fluidity is increased, making it easier to fill the mold cavity during processing and easier to form, which can effectively reduce molding defects and improve production efficiency and product quality; the presence of silicone helps to improve the dispersion uniformity of the filler in the phenolic resin matrix and avoid the occurrence of filler agglomeration, thereby making the performance of the composite lubricating composition more stable and reliable, and further improving the comprehensive performance of the material.

[0016] Preferably, the solvent is ethanol or acetone, and the catalyst is hydrochloric acid or sulfuric acid.

[0017] Preferably, the solid lubricant is one or more of graphite, boron nitride, molybdenum disulfide, and tungsten disulfide.

[0018] Preferably, the fiber reinforcement material is one or more of carbon fiber, glass fiber, aramid fiber and basalt fiber.

[0019] Preferably, the polymer elastomer is one or more of nitrile rubber, silicone rubber, polyurethane elastomer, chloroprene rubber. The polymer elastomer has a unique molecular chain structure, and the molecular chains are connected by weak interaction forces, and can undergo a large degree of reversible deformation when subjected to external forces. When the polymer elastomer is added to the phenolic resin-based composite lubricating material, it can effectively improve the rigidity of the material, making it more soft and elastic. In addition, the polymer elastomer can also enhance the impact resistance of the material, improve the wear resistance of the material, and increase the weather resistance and chemical stability of the material.

[0020] Preferably, the tackifier is one or more of epoxy resin, terpene resin, and polyamide resin; the coupling agent is one or more of aminosilane coupling agent, acryloxysilane coupling agent, epoxysilane coupling agent, titanate coupling agent, and aluminate coupling agent; the antioxidant is one or more of butylated hydroxyanisole and dibutylated hydroxytoluene. The coupling agent molecule contains both inorganic-philic groups and organic-philic groups. The inorganic-philic groups can react chemically with active groups such as hydroxyl groups on the surface of the inorganic filler to form covalent bonds, build a strong chemical bond bridge between the inorganic filler and the modified phenolic resin, enhance the bonding force between the two, and improve the integrity and stability of the composite lubricating material. Due to the presence of the coupling agent, the compatibility between the inorganic filler and the modified phenolic resin is significantly improved, reducing the phase separation phenomenon caused by the differences in the chemical structure and physical properties of the two, so that the filler can be more evenly dispersed in the modified phenolic resin matrix, thereby improving the performance uniformity of the composite lubricating composition.

[0021] The present invention also provides a method for preparing a composite lubricating composition, which is used to prepare the composite lubricating composition described above, and comprises the following steps:

[0022] Step S1: preheating the modified phenolic resin to 80° C.-100° C. to soften it and make it fluid;

[0023] Step S2: pre-treating the solid lubricant, the fiber-reinforced material, the polymer elastomer, the tackifier, the coupling agent, and the antioxidant, respectively, including drying and grinding;

[0024] Step S3: adding solid lubricant, polytetrafluoroethylene, fiber reinforcement material, polymer elastomer, tackifier, coupling agent, and antioxidant to the preheated modified phenolic resin in sequence, stirring at a stirring speed of 600-1000 r / min for 2-3 hours;

[0025] Step S4: hot pressing the uniformly mixed materials into a desired shape, with the hot pressing temperature being 160° C.-240° C. and the hot pressing pressure being 15-30 MPa.

[0026] The technical solution provided by the present invention has at least the following advantages compared with the prior art:

[0027] 1. The composite lubricating composition of the present invention uses modified phenolic resin as a matrix, and utilizes its good heat resistance and mechanical properties to provide a stable structural support for the entire material, so that it can maintain good performance in a high temperature environment.

[0028] 2. The composite lubricating composition of the present invention effectively reduces the friction coefficient of the material, improves the lubrication performance, and reduces the friction loss of the equipment during operation by adding solid lubricants and polymer elastomers; the fiber-reinforced material further improves the strength and toughness of the material, enabling it to withstand greater loads and impact forces; the use of other additives improves the comprehensive performance of the material, enabling it to adapt to more complex working conditions.

[0029] 3. The preparation method of the composite lubricating composition provided by the present invention is highly operable, and the raw materials are easily available, and can be applied to materials such as bearing materials, sleeve materials or gaskets. BRIEF DESCRIPTION OF THE DRAWINGS

[0030] The above and other purposes, features and advantages of the present invention will become more apparent through a more specific description of the preferred embodiments of the present invention shown in the accompanying drawings. The same reference numerals indicate the same parts in all the accompanying drawings, and the drawings are not deliberately scaled to the actual size, but the focus is on illustrating the subject matter of the present application.

[0031] Figure 1 are photographs of compositions prepared in Examples 1-7 of the present invention;

[0032] Figure 2 are photos of the compositions prepared in Comparative Examples 1-8 of the present invention;

[0033] Figure 3 The friction coefficient curve of the composition prepared in Examples 1-7 of the present invention;

[0034] Figure 4 The friction coefficient curves of the compositions prepared in Comparative Examples 1-8 of the present invention are shown in FIG. DETAILED DESCRIPTION

[0035] The technical solution of the present invention is further described in detail below in conjunction with specific embodiments so that those skilled in the art can better understand the present invention and implement it, but the embodiments are not intended to limit the present invention.

[0036] In order to better illustrate the scheme of the present invention, the following are specific embodiments.

[0037] Example 1

[0038] The composition of the composite lubricating composition is as follows: by weight: 100 parts of modified phenolic resin, 20 parts of graphite, 5 parts of polytetrafluoroethylene, 10 parts of glass fiber, 5 parts of nitrile rubber, 10 parts of epoxy resin, 15 parts of aminosilane coupling agent and 2 parts of butylated hydroxyanisole.

[0039] The preparation method comprises the following steps:

[0040] (1) Preparation method of modified phenolic resin: add an organosilicon compound and a solvent into a reaction kettle, heat to 35°C and stir evenly, add a catalyst, continue stirring and reacting for 0.5h to obtain an organosilicon prepolymer;

[0041] Step 2: Add phenolic resin to another reaction kettle, add solvent, heat to 50°C, and stir for 0.5h to dissolve all the phenolic resin;

[0042] Step 3: slowly add the organosilicon prepolymer prepared in step 1 to the dissolved phenolic resin so that the molar ratio of the organosilicon prepolymer to the phenolic resin is 1:2, heat to 80° C., and keep stirring for 1 hour;

[0043] Step 4: After the reaction is completed, the product is filtered, washed, and dried to obtain a modified phenolic resin.

[0044] (2) Preparation method of composite lubricating composition:

[0045] Step S1: preheating the modified phenolic resin to 85° C. to soften it and make it fluid;

[0046] Step S2: pre-treating the graphite, glass fiber, nitrile rubber, epoxy resin, aminosilane coupling agent, and butylated hydroxyanisole, respectively, including drying and grinding;

[0047] Step S3: adding graphite, polytetrafluoroethylene, glass fiber, nitrile rubber, epoxy resin, aminosilane coupling agent, and butylated hydroxyanisole to the preheated modified phenolic resin in sequence, stirring at a stirring speed of 1000 r / min for 2 hours;

[0048] Step S4: hot pressing the uniformly mixed material into a desired shape, with the hot pressing temperature being 200° C. and the hot pressing pressure being 2 MPa.

[0049] Example 2

[0050] The composition of the composite lubricating composition is as follows: by weight: 180 parts of modified phenolic resin, 28 parts of graphite, 15 parts of polytetrafluoroethylene, 20 parts of glass fiber, 15 parts of nitrile rubber, 18 parts of epoxy resin, 20 parts of aminosilane coupling agent and 4 parts of butylated hydroxyanisole.

[0051] The preparation method is the same as that in Example 1.

[0052] Example 3

[0053] The composition of the composite lubricating composition is as follows: by weight: 100 parts of modified phenolic resin, 20 parts of boron nitride, 5 parts of polytetrafluoroethylene, 10 parts of glass fiber, 5 parts of nitrile rubber, 10 parts of epoxy resin, 15 parts of aminosilane coupling agent and 2 parts of butylated hydroxyanisole.

[0054] The preparation method is the same as that in Example 1.

[0055] Example 4

[0056] The composition of the composite lubricating composition is as follows: by weight: 100 parts of modified phenolic resin, 20 parts of graphite, 5 parts of polytetrafluoroethylene, 10 parts of basalt fiber, 5 parts of nitrile rubber, 10 parts of epoxy resin, 15 parts of aminosilane coupling agent and 2 parts of butylated hydroxyanisole.

[0057] The preparation method is the same as that in Example 1.

[0058] Example 5

[0059] The composition of the composite lubricating composition is as follows: by weight: 100 parts of modified phenolic resin, 20 parts of graphite, 5 parts of polytetrafluoroethylene, 10 parts of glass fiber, 5 parts of polyurethane elastomer, 10 parts of epoxy resin, 15 parts of aminosilane coupling agent and 2 parts of butylated hydroxyanisole.

[0060] The preparation method is the same as that in Example 1.

[0061] Example 6

[0062] The composition of the composite lubricating composition is as follows: by weight: 100 parts of modified phenolic resin, 20 parts of graphite, 5 parts of polytetrafluoroethylene, 10 parts of glass fiber, 5 parts of nitrile rubber, 10 parts of epoxy resin, 15 parts of titanate coupling agent and 2 parts of butylated hydroxyanisole.

[0063] The preparation method is the same as that in Example 1.

[0064] Example 7

[0065] The composition of the composite lubricating composition is the same as that of Example 1.

[0066] Preparation method:

[0067] (1) The preparation method of modified phenolic resin is the same as that in Example 1.

[0068] (2) Preparation method of composite lubricating composition:

[0069] Step S1: preheating the modified phenolic resin to 85° C. to soften it and make it fluid;

[0070] Step S2: pre-treating the graphite, glass fiber, nitrile rubber, epoxy resin, aminosilane coupling agent, and butylated hydroxyanisole, respectively, including drying and grinding;

[0071] Step S3: adding graphite, polytetrafluoroethylene, glass fiber, nitrile rubber, epoxy resin, aminosilane coupling agent, and butylated hydroxyanisole to the preheated modified phenolic resin in sequence, stirring at a speed of 600 r / min for 3 hours;

[0072] Step S4: hot pressing the uniformly mixed material into a desired shape, with the hot pressing temperature being 200° C. and the hot pressing pressure being 2 MPa.

[0073] Comparative Example 1

[0074] The composition of the composite lubricating composition is compared with that of Example 1, except that the modified phenolic resin is replaced with phenolic resin.

[0075] Preparation method: The preparation method of the composite lubricating composition is the same as that in Example 1.

[0076] Comparative Example 2

[0077] The composition of the composite lubricating composition is different from that of Example 1, except that no solid lubricant is added.

[0078] The preparation method is the same as that in Example 1.

[0079] Comparative Example 3

[0080] The composition of the composite lubricating composition is different from that of Example 1, except that polytetrafluoroethylene is not added.

[0081] The preparation method is the same as that in Example 1.

[0082] Comparative Example 4

[0083] The composition of the composite lubricating composition is different from that of Example 1, except that no fiber reinforcement material is added.

[0084] The preparation method is the same as that in Example 1.

[0085] Comparative Example 5

[0086] The composition of the composite lubricating composition is different from that of Example 1 except that no polymer elastomer is added.

[0087] The preparation method is the same as that in Example 1.

[0088] Comparative Example 6

[0089] The composition of the composite lubricating composition is different from that of Example 1, except that no coupling agent is added.

[0090] The preparation method is the same as that in Example 1.

[0091] Comparative Example 7

[0092] The composition of the composite lubricating composition is the same as that of Example 1.

[0093] Preparation method Compared with Example 1, in the preparation method of the modified phenolic resin, the molar ratio of the silicone prepolymer to the phenolic resin is equal to 1:1, and the rest is the same as Example 1.

[0094] Comparative Example 8

[0095] The composition of the composite lubricating composition is the same as that of Example 1.

[0096] Preparation Method Compared with Example 1, in the preparation method of the composite lubricating composition, the stirring speed in step S3 is 300 r / min, the stirring time is 2 hours, and the rest is the same as Example 1.

[0097] Please refer to Figure 1-Figure 2 , which is a physical picture of the composition prepared in Examples 1-7 and Comparative Examples 1-8, and the performance test of the composition prepared in Examples 1-7 and Comparative Examples 1-8 is performed:

[0098] Friction and wear test: The friction test was carried out using a UMT rotary friction and wear tester. The test conditions were: load 15N, rotation radius 5mm, rotation speed 100rpm, silicon nitride ball for the grinding pair, and test time 1h. After the test, the wear scar was observed using a white light interferometer, the wear scar volume was measured, and the wear rate was calculated.

[0099] The friction test results are shown in Table 1. Figure 3-Figure 4 As shown:

[0100] Table 1 Test results data

[0101]

[0102] Table 1 is a comparison table of the wear rate and friction coefficient of Examples 1-7 and Comparative Examples 1-8. It can be seen from Table 1 that:

[0103] The composite lubricating composition of the invention uses modified phenolic resin as a matrix and is composed of composite solid lubricants, polytetrafluoroethylene, fiber reinforcement materials, polymer elastomers and other components, so that the composite lubricating composition has excellent wear resistance and low friction coefficient.

[0104] From the comparison between Examples 1-7, it can be seen that when the composite lubricating composition provided by the present invention meets the weight ratio and component selection specified in this scheme, the prepared composite lubricating composition has a low wear rate and friction coefficient and has relatively excellent and balanced wear reduction and anti-wear properties.

[0105] By comparing Example 1 and Example 7, it can be seen that when preparing the composite lubricating composition, a lower rotation speed and a longer reaction time are used, and the overall performance of the prepared composite lubricating composition is slightly reduced, that is, the overall performance of the composite lubricating composition prepared by using a higher rotation speed for reaction is better.

[0106] By comparing Example 1 and Comparative Example 1, it can be seen that the modified phenolic resin used in the present invention as the matrix can make the wear rate and friction coefficient of the prepared composite lubricating composition lower and the overall performance better than that of the unmodified phenolic resin.

[0107] Comparing Example 1 with Comparative Example 2, it can be seen that without adding a solid lubricant, the overall performance of the prepared composite lubricating composition deteriorates. Comparing Example 1 with Comparative Example 3, it can be seen that without adding polytetrafluoroethylene, the overall performance of the prepared composite lubricating composition deteriorates. Comparing Example 1 with Comparative Example 4, it can be seen that without adding a fiber reinforcement material, the overall performance of the prepared composite lubricating composition deteriorates. Comparing Example 1 with Comparative Example 5, it can be seen that without adding a polymer elastomer, the overall performance of the prepared composite lubricating composition deteriorates, and the overall performance of the composite lubricating composition of Comparative Example 5 decreases more than that of Comparative Examples 2 to Comparative Example 4.

[0108] Comparing Example 1 and Comparative Example 6, it can be seen that in Comparative Example 6, no coupling agent is added, the compatibility between the inorganic filler in the prepared material and the modified phenolic resin is very poor, the wear rate of the prepared composite lubricating material is very large, and it is not suitable for practical application.

[0109] By comparing Example 1 and Comparative Example 7, it can be seen that when modifying the phenolic resin, the amount of silicone prepolymer is increased, but the reaction temperature is not increased, resulting in insufficient reactivity of the silicone prepolymer, incomplete modification of the phenolic resin, and ultimately reduced overall performance of the composite lubricating composition obtained.

[0110] By comparing Example 1 and Comparative Example 8, it can be seen that when preparing the composite lubricating composition, a very slow stirring speed was used, and the reaction time was not increased accordingly, so that the components in the prepared composite lubricating composition were not completely dispersed in the modified phenolic resin, the wear rate thereof increased, and the overall performance decreased.

[0111] The above are only preferred embodiments of the present invention, and are not intended to limit the patent scope of the present invention. Any equivalent structure or equivalent process transformation made using the contents of the present invention specification, or directly or indirectly applied in other related technical fields, are also included in the patent protection scope of the present invention.

Claims

1. A method for preparing a composite lubricating composition, characterized in that: The composite lubricating composition comprises the following components by weight: 100 parts of modified phenolic resin, 20 parts of graphite, 5 parts of polytetrafluoroethylene, 10 parts of glass fiber, 5 parts of nitrile rubber, 10 parts of epoxy resin, 15 parts of aminosilane coupling agent, and 2 parts of butylated hydroxyanisole; Alternatively, the composite lubricating composition comprises the following components, measured in parts by weight: 180 parts of modified phenolic resin, 28 parts of graphite, 15 parts of polytetrafluoroethylene, 20 parts of glass fiber, 15 parts of nitrile rubber, 18 parts of epoxy resin, 20 parts of aminosilane coupling agent, and 4 parts of butylated hydroxyanisole; The modified phenolic resin is obtained by modifying the phenolic resin with an organic silicon compound, wherein the molar ratio of the organic silicon compound to the phenolic resin is 1:2; the organic silicon compound is amino silicone oil; The preparation method comprises the following steps: Step S1: preheating the modified phenolic resin to 80°C-100°C to soften it and make it fluid; Step S2: pre-treating the solid lubricant, the fiber-reinforced material, the polymer elastomer, the tackifier, the coupling agent, and the antioxidant, respectively, including drying and grinding; Step S3: adding solid lubricant, polytetrafluoroethylene, fiber reinforcement material, polymer elastomer, tackifier, coupling agent, and antioxidant to the preheated modified phenolic resin in sequence, stirring at a stirring speed of 1000 r / min for 2 hours; Step S4: hot pressing the uniformly mixed material into a desired shape, with the hot pressing temperature being 160°C-240°C and the hot pressing pressure being 15-30 MPa; The solid lubricant is graphite; the fiber reinforcement material is glass fiber; the polymer elastomer is nitrile rubber; the tackifier is epoxy resin; the coupling agent is aminosilane coupling agent; and the antioxidant is butylated hydroxyanisole.

2. The preparation method according to claim 1, characterized in that: The process of modifying the phenolic resin with an organosilicon compound to obtain the modified phenolic resin comprises the following steps: Step 1: Add the organosilicon compound and the solvent into a reaction kettle, heat to 30°C-40°C and stir evenly, add the catalyst, continue stirring and reacting for 0.5-1 h to obtain an organosilicon prepolymer; Step 2: Add the phenolic resin to another reaction kettle, add the solvent, heat to 40 ℃-60 ℃, and stir for 0.5-1 h to completely dissolve the phenolic resin; Step 3: slowly add the organosilicon prepolymer prepared in step 1 to the dissolved phenolic resin so that the molar ratio of the organosilicon prepolymer to the phenolic resin is 1:2, heat to 70°C-100°C, and keep stirring for 1-2 hours; Step 4: After the reaction is completed, the product is filtered, washed, and dried to obtain a modified phenolic resin.

3. The preparation method according to claim 2, characterized in that: The solvent is ethanol or acetone, and the catalyst is hydrochloric acid or sulfuric acid.

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