CN114854230A - Nano silicon dioxide loaded graphite-like phase carbon nitride and preparation method thereof, and self-lubricating phenolic aldehyde laminated cloth bearing material and preparation method thereof - Google Patents
Nano silicon dioxide loaded graphite-like phase carbon nitride and preparation method thereof, and self-lubricating phenolic aldehyde laminated cloth bearing material and preparation method thereof Download PDFInfo
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- D06M11/77—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with silicon or compounds thereof
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Abstract
The invention provides nano silicon dioxide loaded graphite-like phase carbon nitride and a preparation method thereof, and a self-lubricating phenolic laminated cloth bearing material and a preparation method thereof, and relates to the technical field of lubricating materials. Mixing graphite-like phase carbon nitride, dopamine hydrochloride and Tris-HCl buffer solution for oxidation self-polymerization reaction to obtain polydopamine modified graphite-like phase carbon nitride; mixing the polydopamine modified graphite-like carbon nitride, a surfactant, ammonia water, an organic solvent and tetraethoxysilane for hydrolysis reaction to obtain the nano silicon dioxide loaded graphite-like carbon nitride. The nano silicon dioxide loaded graphite-like phase carbon nitride prepared by the invention is used for modifying the phenolic aldehyde laminated cloth bearing material, so that the phenolic aldehyde laminated cloth bearing material has the characteristics of low friction and high wear resistance on the basis of further improving the mechanical property of the phenolic aldehyde laminated cloth bearing material, and a self-lubricating transfer film is easily formed on the surface of a friction couple in the using process and is the self-lubricating phenolic aldehyde laminated cloth bearing material.
Description
Technical Field
The invention relates to the technical field of lubricating materials, in particular to nano silicon dioxide loaded graphite-like phase carbon nitride and a preparation method thereof, and a self-lubricating phenolic aldehyde laminated cloth bearing material and a preparation method thereof.
Background
The phenolic aldehyde laminated cloth material (also called phenolic aldehyde bakelite) is formed by laminating phenolic aldehyde resin as an adhesive and cotton fiber cloth as a reinforcement layer by layer, has the characteristics of high bearing capacity, wear resistance and the like, and has important application in the preparation of high-end equipment as materials of a bearing retainer, a shaft sleeve, a bushing, a water lubricated bearing and the like.
At present, a great deal of research on phenolic aldehyde laminated cloth materials is carried out, such as CN201710878723.5, CN200620107670.4, CN03111292.7 and the like, however, the existing phenolic aldehyde laminated cloth materials are lack of self-lubricating property and only can be compounded with lubricating oil, lubricating grease or water and other media for use, and in the practical application process, once dry friction is generated due to working condition change or lack of lubricating media, the materials are easy to wear and lose efficacy.
Disclosure of Invention
In view of the above, the present invention aims to provide a nano-silica-supported graphite-like carbon nitride and a preparation method thereof, and a self-lubricating phenolic laminated cloth bearing material and a preparation method thereof. The nano silicon dioxide loaded graphite-like phase carbon nitride prepared by the method modifies the phenolic aldehyde laminated cloth bearing material, and the obtained phenolic aldehyde laminated cloth bearing material is a self-lubricating material and has the characteristics of low friction and high wear resistance.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a preparation method of nano silicon dioxide loaded graphite-like phase carbon nitride, which comprises the following steps:
(1) mixing the graphite-like phase carbon nitride, dopamine hydrochloride and Tris-HCl buffer solution, and carrying out oxidative autopolymerization reaction to obtain polydopamine modified graphite-like phase carbon nitride;
(2) and mixing the polydopamine modified graphite-like carbon nitride, a surfactant, ammonia water, an organic solvent and tetraethoxysilane, and carrying out hydrolysis reaction to obtain the nano silicon dioxide loaded graphite-like carbon nitride.
Preferably, the pH value of the Tris-HCl buffer solution in the step (1) is 8.0-8.5; the dosage ratio of the dopamine hydrochloride to the Tris-HCl buffer solution is 1-5 g: 1L of the compound.
Preferably, the particle size of the graphite-like phase carbon nitride in the step (1) is 30-50 μm; the dosage ratio of the graphite-like phase carbon nitride to the Tris-HCl buffer solution is 1 g: 5-10 mL.
Preferably, the time of the oxidative self-polymerization reaction in the step (1) is 12-24 h.
Preferably, the surfactant in step (2) comprises one or more of sodium dodecyl sulfate, dodecyl trimethyl ammonium chloride and sodium octadecyl benzene sulfonate; the organic solvent comprises one or more of ethanol, isopropanol and n-butanol.
Preferably, the ratio of the polyamine-modified graphite-like phase carbon nitride to the organic solvent in the step (2) is 1 g: 10-20 mL; the mass of the surfactant is 1-3% of that of the organic solvent; the volume ratio of the ammonia water to the organic solvent is 1: 25-30; the volume ratio of the ethyl orthosilicate to the organic solvent is 1:15 to 20.
Preferably, the temperature of the hydrolysis reaction in the step (2) is 40-50 ℃, and the time is 12-24 hours.
The invention provides the nano silicon dioxide loaded graphite-like carbon nitride prepared by the preparation method in the technical scheme.
The invention provides a self-lubricating phenolic aldehyde laminated cloth bearing material, which is prepared from the raw materials of nano silicon dioxide loaded graphite-like phase carbon nitride, phenolic resin and cotton fiber cloth in the technical scheme; the mass ratio of the nano silicon dioxide loaded graphite-like carbon nitride to the phenolic resin to the cotton fiber cloth is (4-10): (30-50): (45-60).
The invention provides a preparation method of the self-lubricating phenolic aldehyde laminated cloth bearing material in the technical scheme, which comprises the following steps:
mixing the nano silicon dioxide loaded graphite-like carbon nitride with a phenolic resin solution to obtain a modified phenolic resin glue solution;
soaking the cotton fiber cloth in the modified phenolic resin glue solution, and then drying to obtain prepreg cloth;
and winding, rolling and forming the prepreg cloth, and sintering and curing to obtain the self-lubricating phenolic aldehyde laminated cloth bearing material.
Preferably, the solvent of the phenolic resin solution is ethanol; the solid content of the modified phenolic resin glue solution is 50-60 wt%, and the mass fraction of the nano silicon dioxide loaded graphite-like phase carbon nitride in the solid content is 10-20 wt%.
Preferably, the sizing amount of the prepreg cloth is 45-60 wt%.
Preferably, the sintering and curing step comprises a first sintering and curing stage, a second sintering and curing stage and a third sintering and curing stage which are sequentially carried out; the temperature of the first sintering and curing stage is 80-90 ℃, and the heat preservation time is 100-120 min; the temperature of the second sintering and curing stage is 110-120 ℃, and the heat preservation time is 100-120 min; the temperature of the third sintering and curing stage is 170-180 ℃, and the heat preservation time is 60-120 min.
The invention provides a preparation method of nano silicon dioxide loaded graphite-like phase carbon nitride, which comprises the following steps: mixing the graphite-like phase carbon nitride, dopamine hydrochloride and Tris-HCl buffer solution, and carrying out oxidative autopolymerization reaction to obtain polydopamine modified graphite-like phase carbon nitride; mixing the polydopamine modified graphite-like carbon nitride, a surfactant, ammonia water, an organic solvent and tetraethoxysilane, and carrying out hydrolysis reaction to obtain the nano silicon dioxide loaded graphite-like carbon nitride. The invention has the following beneficial effects:
the invention introduces the carbon nitride (namely graphite-like phase carbon nitride) with a graphite-like layered structure, has low friction coefficient, high wear resistance and higher hardness and modulus, is very easy to transfer to the surface of a friction couple to form a transfer film with high bearing and low shear strength in the friction process, obviously reduces the friction coefficient of the phenolic aldehyde laminated fabric material and improves the wear resistance;
the invention carries out polydopamine modification on the graphite-like phase carbon nitride, introduces hydroxyl and amino on the surface of the graphite-like phase carbon nitride, can be used as a secondary reaction platform to play a role of a chemical bridge, enables the graphite-like phase carbon nitride to be combined with nano silicon dioxide through covalent bonds, enables the nano silicon dioxide to grow on the surface of the carbon nitride in situ, can strengthen the synergistic lubrication effect between the carbon nitride and the nano silicon dioxide, enables the carbon nitride and the nano silicon dioxide particles to be simultaneously released to a friction interface in the friction process, on one hand, is beneficial to quickly forming a transfer film under the action of interface stress and frictional heat and shortens the frictional running-in time of materials, and on the other hand, the formed transfer film furthest exerts the high bearing and low friction properties of the carbon nitride and the easy adhesion properties of the nano silicon dioxide (the easy adhesion properties of the nano silicon dioxide can ensure the stability, stability and the like of the self-lubricating transfer film, Durable), exhibits extremely excellent frictional wear properties;
according to the invention, polar groups such as hydroxyl and amino are introduced on the surface of graphite-like carbon nitride through polydopamine modification, so that the hydrophilicity of the nano silicon dioxide loaded graphite-like carbon nitride can be improved, the uniform dispersion of the nano silicon dioxide loaded graphite-like carbon nitride in phenolic resin is realized, and the sedimentation after long-term standing is avoided; in addition, in the thermal curing process of the phenolic resin, polydopamine on the surface of the graphite-like carbon nitride can participate in a curing reaction, so that the interface bonding force between the graphite-like carbon nitride and the phenolic resin is enhanced, and the mechanical strength of the phenolic laminated cloth material is obviously improved.
The invention provides the nano silicon dioxide loaded graphite-like carbon nitride prepared by the preparation method in the technical scheme. The nano silicon dioxide loaded graphite-like carbon nitride is used for modifying the phenolic aldehyde laminated cloth bearing material, so that the phenolic aldehyde laminated cloth bearing material has low friction and high wear resistance on the basis of further improving the mechanical property of the phenolic aldehyde laminated cloth bearing material, a self-lubricating transfer film is easily formed on the surface of a friction couple in the use process, and the self-lubricating phenolic aldehyde laminated cloth bearing material is excellent in tribology property and can be used for medium conditions such as lubricating oil, lubricating grease or water and dry friction working conditions such as oil-free and water-free.
The results of the examples show that the nano silicon dioxide loaded graphite-like carbon nitride is used for modifying the phenolic laminated cloth bearing material, the radial tensile strength of the obtained self-lubricating phenolic laminated cloth bearing material is 109-116 MPa, the friction coefficient under the dry friction condition is 0.10-0.12, and the volumetric wear rate is 5.8-6.1 × 10 -7 mm 3 The friction coefficient of the lubricating grease is 0.03-0.05, and the volumetric wear rate is 0.36-0.38 multiplied by 10 under the condition of L252 lubricating grease lubrication -7 mm 3 (iv)/Nm; compared with the phenolic aldehyde laminated cloth material prepared in the prior art, the friction coefficient is reduced by 36.8-47.4% under the dry friction condition, the wear resistance is improved by 41.9-44.8%, and the wear resistance is improved by 26.9-30.7% under the grease lubrication condition.
Detailed Description
The invention provides a preparation method of nano silicon dioxide loaded graphite-like phase carbon nitride, which comprises the following steps:
(1) mixing the graphite-like phase carbon nitride, dopamine hydrochloride and Tris-HCl buffer solution, and carrying out oxidative autopolymerization reaction to obtain polydopamine modified graphite-like phase carbon nitride;
(2) and mixing the polydopamine modified graphite-like carbon nitride, a surfactant, ammonia water, an organic solvent and tetraethoxysilane, and carrying out hydrolysis reaction to obtain the nano silicon dioxide loaded graphite-like carbon nitride.
In the present invention, the raw materials used are all commercially available products well known to those skilled in the art unless otherwise specified.
The preparation method comprises the steps of mixing the graphite-like phase carbon nitride, dopamine hydrochloride and Tris-HCl buffer solution, and carrying out oxidation autopolymerization reaction to obtain the polydopamine modified graphite-like phase carbon nitride. In the present invention, the pH value of the Tris-HCl buffer is preferably 8.0-8.5, and more preferably 8.5, and the Tris-HCl buffer can be prepared by a commercial product known by a person skilled in the art or a preparation method known by a person skilled in the art; the preferable dosage ratio of the dopamine hydrochloride to the Tris-HCl buffer solution is 1-5 g: 1L, more preferably 2-3 g: 1L of the compound. In the invention, the particle size of the graphite-like phase carbon nitride is preferably 30-50 μm; the dosage ratio of the graphite-like phase carbon nitride to the Tris-HCl buffer solution is preferably 1 g: 5-10 mL, more preferably 1 g: 5-8 mL. In the invention, the specific operation of mixing the graphite-like phase carbon nitride, dopamine hydrochloride and Tris-HCl buffer solution is preferably as follows: dissolving dopamine hydrochloride in Tris-HCl buffer solution, and adding graphite-like phase carbon nitride. In the invention, the oxidation self-polymerization reaction is carried out at normal temperature; the time of the oxidation self-polymerization reaction is preferably 12-24 hours, more preferably 15-20 hours, and the time of the oxidation self-polymerization reaction is calculated from the completion of the addition of the graphite-like phase carbon nitride; the oxidative autopolymerization is preferably carried out under stirring. In the process of the oxidative autopolymerization reaction, dopamine hydrochloride undergoes oxidative autopolymerization to generate polydopamine, and the surface of the polydopamine has a large number of active groups such as phenolic hydroxyl groups, amino groups and the like, so that the polydopamine has strong adhesion performance and can be adhered to the surface of graphite-like carbon nitride; the graphite-like carbon nitride modified by polydopamine utilizes a large amount of active groups such as phenolic hydroxyl groups, amino groups and the like of the polydopamine on the surface as a secondary reaction platform, thereby providing possibility for subsequent silicon dioxide loading.
After the oxidative autopolymerization reaction, the reaction solution is preferably sequentially filtered, washed and dried to obtain the polydopamine modified graphite-like carbon nitride. The invention has no special requirements on the filtration mode, and the filtration mode which is well known by the technicians in the field can be adopted; the washing is preferably deionized water; the invention has no special requirements on the drying temperature and time, and the drying is carried out until the weight is constant.
After the polydopamine modified graphite-like phase carbon nitride is obtained, the polydopamine modified graphite-like phase carbon nitride, a surfactant, ammonia water, an organic solvent and tetraethoxysilane are mixed for hydrolysis reaction to obtain the nano silicon dioxide loaded graphite-like phase carbon nitride. In the present invention, the surfactant preferably includes one or more of sodium dodecyl sulfate, dodecyltrimethylammonium chloride, and sodium octadecylbenzenesulfonate, more preferably Sodium Dodecyl Sulfate (SDS); the organic solvent comprises one or more of ethanol, isopropanol and n-butanol, and ethanol is more preferable. In the present invention, the ratio of the amount of the polyamine-modified graphite-like phase carbon nitride to the amount of the organic solvent is preferably 1 g: 10-20 mL, more preferably 1 g: 15 mL; the mass of the surfactant is preferably 1-3% of that of the organic solvent, and more preferably 2%; the mass fraction of the ammonia water is preferably 25-28%, and the volume ratio of the ammonia water to the organic solvent is preferably 1: 25-30, specifically 1:25 or 1: 30; the volume ratio of the ethyl orthosilicate to the organic solvent is preferably 1:15 to 20, specifically 1:15 or 1: 20. In the invention, the concrete operation of mixing the polydopamine modified graphite-like carbon nitride, the surfactant, the ammonia water, the organic solvent and the tetraethoxysilane is preferably as follows: dispersing the polydopamine modified graphite-like phase carbon nitride in an organic solvent to obtain a polydopamine modified graphite-like phase carbon nitride dispersion liquid; adding a surfactant and ammonia water into the polydopamine modified graphite-like carbon nitride dispersion liquid, and stirring and mixing to obtain a mixed solution; and dropwise adding ethyl orthosilicate into the mixed solution. In the invention, the temperature of the hydrolysis reaction is preferably 40-50 ℃, more preferably 45 ℃, and the time is preferably 12-24 hours, more preferably 12-15 hours; the time of the hydrolysis reaction is calculated by starting from the end of the dropwise addition of the tetraethoxysilane. In the hydrolysis reaction process, the tetraethoxysilane is hydrolyzed and condensed to generate the nano silicon dioxide; ammonia water is used as a catalyst to accelerate the hydrolysis speed of the tetraethoxysilane; the surfactant can effectively prevent the agglomeration among the nano silicon dioxide particles to obtain nano silicon dioxide particles which have smaller particle size and show monodispersity; meanwhile, hydroxyl on the surface of the polydopamine modified graphite-like carbon nitride participates in the hydrolysis reaction of tetraethoxysilane, and is chemically bonded with nano silicon dioxide, so that nano silicon dioxide particles are loaded on the surface of the graphite-like carbon nitride in situ.
After the hydrolysis reaction, the obtained hydrolysis reaction liquid is preferably sequentially filtered, washed and dried to obtain the nano silicon dioxide loaded graphite-like phase carbon nitride. In the present invention, the washing is preferably ethanol washing.
The invention provides the nano silicon dioxide loaded graphite-like carbon nitride prepared by the preparation method in the technical scheme. The graphite-like phase carbon nitride in the nano silicon dioxide loaded graphite-like phase carbon nitride has low friction coefficient, high wear resistance and higher hardness and modulus, and is very easy to transfer to the surface of a friction couple in the friction process to form a transfer film with high bearing and low shear strength, so that the friction coefficient of the phenolic aldehyde laminated fabric material is remarkably reduced, and the wear resistance is improved; the graphite-like phase carbon nitride is modified by polydopamine, and hydroxyl and amino are introduced on the surface of the graphite-like phase carbon nitride, so that the graphite-like phase carbon nitride is combined with nano silicon dioxide through covalent bonds, and the nano silicon dioxide grows on the surface of the carbon nitride in situ, so that the synergistic lubrication effect between the carbon nitride and the nano silicon dioxide can be enhanced; polar groups such as hydroxyl, amino and the like are introduced on the surface of the graphite-like carbon nitride through polydopamine modification, so that the hydrophilicity of the nano silicon dioxide loaded graphite-like carbon nitride is improved, the uniform dispersion of the nano silicon dioxide loaded graphite-like carbon nitride in phenolic resin is realized, and the sedimentation after long-term standing is avoided; in addition, in the thermal curing process of the phenolic resin, polydopamine on the surface of the graphite-like carbon nitride can participate in a curing reaction, so that the interface bonding force between the graphite-like carbon nitride and the phenolic resin is enhanced, and the mechanical strength of the phenolic laminated cloth material is obviously improved.
The invention provides a self-lubricating phenolic aldehyde laminated cloth bearing material, which is prepared from the raw materials of nano silicon dioxide loaded graphite-like phase carbon nitride, phenolic resin and cotton fiber cloth. In the invention, the mass ratio of the nano silicon dioxide loaded graphite-like carbon nitride to the phenolic resin to the cotton fiber cloth is (4-10): (30-50): (45-60), preferably (5-10): (35-45): (45-55). The phenolic resin is not particularly required in the invention, and the phenolic resin which is well known to the person skilled in the art can be adopted; the cotton fiber cloth is preferably 20-100-yarn count plain cotton fiber cloth with surface desized. The phenolic laminated cloth bearing material provided by the invention has the characteristics of low friction and high wear resistance on the basis of further improving the mechanical properties of the phenolic laminated cloth bearing material, is easy to form a self-lubricating transfer film on the surface of a friction couple in the use process, is a self-lubricating phenolic laminated cloth bearing material with excellent tribology performance, and can be used for medium conditions such as lubricating oil, lubricating grease or water and dry friction working conditions such as oil-free and water-free.
The invention provides a preparation method of the self-lubricating phenolic aldehyde laminated cloth bearing material in the technical scheme, which comprises the following steps:
mixing the nano silicon dioxide loaded graphite-like carbon nitride with a phenolic resin solution to obtain a modified phenolic resin glue solution;
soaking the cotton fiber cloth in the modified phenolic resin glue solution, and then drying to obtain prepreg cloth;
and winding, rolling and forming the prepreg cloth, and sintering and curing to obtain the self-lubricating phenolic aldehyde laminated cloth bearing material.
The invention mixes the nano silicon dioxide loaded graphite-like carbon nitride with phenolic resin solution to obtain modified phenolic resin glue solution. In the present invention, the solvent of the phenolic resin solution is preferably ethanol; the operation of mixing the nano-silica supported graphite-like phase carbon nitride with the phenolic resin solution is preferably as follows: and adding the nano silicon dioxide loaded graphite-like carbon nitride into a phenolic resin solution, and uniformly dispersing by using a three-roll instrument. In the invention, the solid content of the modified phenolic resin glue solution is preferably 50-60 wt%, and the mass fraction of the nano-silica supported graphite-like carbon nitride (namely nano-silica supported graphite-like carbon nitride/(phenolic resin + nano-silica supported graphite-like carbon nitride)) in the solid content is preferably 10-20 wt%.
After the modified phenolic resin glue solution is obtained, the cotton fiber cloth is soaked in the modified phenolic resin glue solution and then is dried to obtain the prepreg cloth. In the invention, the drying temperature is preferably 100-110 ℃, and the time is preferably 2-3 min; the sizing amount of the prepreg cloth (namely the mass fraction of the modified phenolic resin in the prepreg cloth) is preferably 45-60 wt%, and more preferably 50 wt%.
After the prepreg cloth is obtained, the prepreg cloth is wound, rolled and molded, and then sintered and cured to obtain the self-lubricating phenolic aldehyde laminated cloth bearing material. In the invention, the winding and rolling molding is to wind the prepreg cloth on a winding machine and roll the prepreg cloth into a tubular shape; the process parameters of the winding and rolling molding preferably comprise: the temperature of the hot roller is 90-100 ℃, the pressure of the hot roller is 50-150N, the winding tension is 50-200N, and the winding speed is 0.5-1.0 m/min. In the present invention, the sintering and curing preferably includes a first sintering and curing stage, a second sintering and curing stage and a third sintering and curing stage which are performed in sequence; the temperature of the first sintering and curing stage is preferably 80-90 ℃, further preferably 80-85 ℃, and the heat preservation time is preferably 100-120 min, further preferably 110-120 min; the temperature of the second sintering and curing stage is preferably 110-120 ℃, further preferably 115-120 ℃, and the heat preservation time is preferably 100-120 min, further preferably 115-120 min; the temperature of the third sintering and curing stage is preferably 170-180 ℃, further preferably 175-180 ℃, and the heat preservation time is preferably 60-120 min, further preferably 60-80 min. And after the third sintering and curing, preferably naturally cooling to room temperature to obtain the self-lubricating phenolic aldehyde laminated cloth bearing material.
The nano-silica supported graphite-like phase carbon nitride and the preparation method thereof, and the self-lubricating phenolic laminated cloth bearing material and the preparation method thereof provided by the present invention are described in detail below with reference to the examples, but they should not be construed as limiting the scope of the present invention.
Example 1
The preparation method of the nano silicon dioxide loaded graphite-like phase carbon nitride comprises the following steps:
preparing 1000mL of Tris-HCl buffer solution (the pH value is 8.5), adding 2.0g of dopamine hydrochloride, dissolving the dopamine hydrochloride, placing 200g of graphite-like phase carbon nitride with the particle size of 30-50 mu m in the dopamine hydrochloride, stirring at normal temperature for reacting for 18 hours, filtering after the reaction is finished, washing with deionized water, and drying to obtain polydopamine modified graphite-like phase carbon nitride;
dispersing 200g of polydopamine modified graphite-like phase carbon nitride in 3000mL of ethanol, sequentially adding 47g of surfactant SDS and 120mL of ammonia water (the mass fraction of the ammonia water is 28%), stirring and dispersing uniformly, then dropwise adding 200g of tetraethoxysilane, stirring and reacting for 12h at the constant temperature of 45 ℃, filtering, washing with ethanol, and drying to obtain graphite-like phase carbon nitride with nano-silica loaded on the surface, namely the nano-silica loaded graphite-like phase carbon nitride.
A self-lubricating phenolic aldehyde laminated cloth bearing material is prepared by the following steps:
adding 200g of nano silicon dioxide loaded graphite-like phase carbon nitride into 1889g of phenolic resin ethanol solution with the solid content of 60%, homogenizing by a three-roller instrument, adding 578g of ethanol, and uniformly stirring to obtain modified phenolic resin glue solution;
dipping 100-yarn plain cotton cloth with the surface thereof being desized into the modified phenolic resin solution, and then drying the plain cotton cloth at the temperature of 100 ℃ for 3min to obtain prepreg cloth, wherein the gluing amount of the prepreg cloth is 50%;
winding the modified phenolic resin prepreg cloth into a tubular shape on a winding machine, wherein the winding process parameters are as follows: the temperature of a hot roller is 100 ℃, the pressure of the hot roller is 100N, the winding tension is 150N, and the winding speed is 1.0 m/min; putting the wound phenolic aldehyde laminated tube into an oven for sintering and curing, wherein the sintering process comprises the following steps: keeping the temperature at 80 deg.C for 120min, at 120 deg.C for 120min, and at 180 deg.C for 60 min. And after sintering, freely cooling to obtain the self-lubricating phenolic aldehyde laminated cloth bearing material.
Example 2
The preparation method of the nano silicon dioxide loaded graphite-like phase carbon nitride comprises the following steps:
preparation of polydopamine modified graphite-like phase carbon nitride as in example 1;
dispersing 200g of polydopamine modified graphite-like carbon nitride in 3000mL of ethanol, sequentially adding 47g of SDS (surfactant) and 100mL of ammonia water (the mass fraction of the ammonia water is 28%), stirring and dispersing uniformly, then dropwise adding 200g of tetraethoxysilane, stirring and reacting at the constant temperature of 45 ℃ for 12 hours, filtering, washing with ethanol, and drying to obtain the nano-silica supported graphite-like carbon nitride.
A self-lubricating phenolic laminated cloth bearing material, and the preparation method is the same as the example 1.
Example 3
The preparation method of the nano silicon dioxide loaded graphite-like phase carbon nitride comprises the following steps:
preparation of polydopamine modified graphite-like phase carbon nitride as in example 1;
dispersing 200g of polydopamine modified graphite-like carbon nitride in 3000mL of ethanol, sequentially adding 47g of SDS (surfactant) and 100mL of ammonia water (the mass fraction of the ammonia water is 28%), stirring and dispersing uniformly, then dropwise adding 150g of tetraethoxysilane, stirring and reacting at the constant temperature of 45 ℃ for 12 hours, filtering, washing with ethanol, and drying to obtain the nano-silica supported graphite-like carbon nitride.
A self-lubricating phenolic laminated cloth bearing material, and the preparation method is the same as the example 1.
Example 4
The preparation method of the nano-silica supported graphite-like carbon nitride is the same as that of example 1.
A self-lubricating phenolic aldehyde laminated cloth bearing material is prepared by the following steps:
adding 200g of nano silicon dioxide loaded graphite-like carbon nitride into 3000g of phenolic resin ethanol solution with solid content of 60%, homogenizing by a three-roll apparatus, adding 800g of ethanol, and uniformly stirring to obtain a modified phenolic resin adhesive;
the preparation of the modified phenolic resin prepreg, winding of the phenolic laminated tube and the sintering and curing process were the same as in example 1.
Example 5
The preparation method of the nano-silica supported graphite-like carbon nitride is the same as that of example 1.
A self-lubricating phenolic aldehyde laminated cloth bearing material is prepared by the following steps:
adding 200g of nano-silica supported graphite-like carbon nitride into 1334g of phenolic resin ethanol solution with the solid content of 60%, homogenizing by a three-roll apparatus, adding 466g of ethanol, and uniformly stirring to obtain modified phenolic resin glue solution;
the preparation of the modified phenolic resin prepreg, winding of the phenolic laminated tube and the sintering and curing process were the same as in example 1.
Comparative example 1
The phenolic laminated cloth material is obtained by comparing with the examples, one is phenolic bakelite pipe (marked as PF-1) purchased from the market, and the other is phenolic laminated cloth material (marked as PF-2) modified without lubricant according to the prior art, and the specific preparation process is as follows: 3000g of a phenolic resin ethanol solution with a solid content of 60% was taken, 600g of ethanol was added and stirred uniformly to obtain a phenolic resin glue solution, and the preparation of the phenolic resin prepreg, winding of the phenolic laminate tube, sintering and curing processes were the same as in example 1.
The self-lubricating phenolic aldehyde laminated cloth material prepared in the embodiment and the phenolic aldehyde laminated cloth material in the comparative example are respectively subjected to mechanical and tribological performance tests, and the test steps are as follows:
(1) the radial tensile strength is tested according to technical conditions of rolling bearing phenolic aldehyde laminated tube distribution cages (JB/T4037-2007), and is processed into a phi 45 x phi 42 x 9mm annular sample, and the radial tensile strength is obtained by calculating the maximum force during the stretch-breaking;
(2) the friction and wear performance test is carried out according to a plastic sliding friction and wear test method (GB/T3960-2016), the test equipment is an MRH-3 high-speed ring block friction and wear tester, and the dry friction test conditions are as follows: the test load is 300N, and the rotating speed is 0.42 m/s; testing the frictional wear performance under the grease lubrication condition, selecting Laobo anti L252 lubricating grease, and testing conditions are as follows: the test load is 100N, and the rotating speed is 3.0 m/s; the test time is 2h, the friction coefficient is directly read by the equipment, the wear width is measured by using a three-dimensional surface profiler, the volumetric wear rate is calculated, and the average value is calculated by measuring each sample for three times.
The test results are shown in tables 1 and 2:
table 1 coefficient of friction and volumetric wear rate under dry friction and radial tensile strength for phenolic laminates of examples 1-5 and comparative examples:
table 2 coefficient of friction and volumetric wear rate under L252 grease lubrication conditions for the phenolic laminates of example 1 and comparative example:
as can be seen from tables 1 and 2, compared with the phenolic laminate cloth material prepared by the prior art, the self-lubricating phenolic laminate cloth material prepared by the present invention has higher mechanical strength and very excellent frictional wear performance, wherein the friction coefficient of the self-lubricating phenolic laminate cloth material prepared by example 1 under dry friction condition is reduced by 47.4%, the wear resistance is improved by 44.8%, and the friction coefficient under grease lubrication condition is not obviously changed, but the wear resistance is improved by 30.7%.
The embodiments show that the nano silicon dioxide loaded graphite-like phase carbon nitride prepared by the invention is used for modifying the phenolic laminated cloth bearing material, so that the phenolic laminated cloth bearing material has the characteristics of low friction and high wear resistance and has excellent tribology performance on the basis of further improving the mechanical performance of the phenolic laminated cloth bearing material.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. A preparation method of nano silicon dioxide loaded graphite-like phase carbon nitride comprises the following steps:
(1) mixing graphite-like phase carbon nitride, dopamine hydrochloride and Tris-HCl buffer solution, and carrying out oxidation autopolymerization reaction to obtain polydopamine modified graphite-like phase carbon nitride;
(2) and mixing the polydopamine modified graphite-like carbon nitride, a surfactant, ammonia water, an organic solvent and tetraethoxysilane, and carrying out hydrolysis reaction to obtain the nano silicon dioxide loaded graphite-like carbon nitride.
2. The method according to claim 1, wherein the pH of the Tris-HCl buffer solution in the step (1) is 8.0 to 8.5; the dosage ratio of the dopamine hydrochloride to the Tris-HCl buffer solution is 1-5 g: 1L;
the particle size of the graphite-like phase carbon nitride is 30-50 mu m; the dosage ratio of the graphite-like phase carbon nitride to the Tris-HCl buffer solution is 1 g: 5-10 mL.
3. The method according to claim 1 or 2, wherein the time for the oxidative autopolymerization reaction in the step (1) is 12 to 24 hours.
4. The preparation method according to claim 1, wherein the surfactant in the step (2) comprises one or more of sodium dodecyl sulfate, dodecyl trimethyl ammonium chloride and sodium octadecyl benzene sulfonate; the organic solvent comprises one or more of ethanol, isopropanol and n-butanol;
the dosage ratio of the polyamine modified graphite-like carbon nitride to the organic solvent is 1 g: 10-20 mL; the mass of the surfactant is 1-3% of that of the organic solvent; the volume ratio of the ammonia water to the organic solvent is 1: 25-30; the volume ratio of the ethyl orthosilicate to the organic solvent is 1:15 to 20.
5. The preparation method according to claim 1 or 4, wherein the hydrolysis reaction in the step (2) is carried out at a temperature of 40-50 ℃ for 12-24 hours.
6. The nano-silica-supported graphite-like carbon nitride prepared by the preparation method of any one of claims 1 to 5.
7. A self-lubricating phenolic aldehyde laminated cloth bearing material is characterized in that the preparation raw materials comprise the nano silicon dioxide loaded graphite-like phase carbon nitride according to claim 6, phenolic resin and cotton fiber cloth; the mass ratio of the nano silicon dioxide loaded graphite-like carbon nitride to the phenolic resin to the cotton fiber cloth is (4-10): (30-50): (45-60).
8. A method of making a self-lubricating phenolic laminated cloth bearing material as claimed in claim 7, comprising the steps of:
mixing the nano silicon dioxide loaded graphite-like carbon nitride with a phenolic resin solution to obtain a modified phenolic resin glue solution;
soaking the cotton fiber cloth in the modified phenolic resin glue solution, and then drying to obtain prepreg cloth;
and winding, rolling and forming the prepreg cloth, and sintering and curing to obtain the self-lubricating phenolic aldehyde laminated cloth bearing material.
9. The method according to claim 8, wherein the solvent of the phenolic resin solution is ethanol; the solid content of the modified phenolic resin glue solution is 50-60 wt%, and the mass fraction of the nano silicon dioxide loaded graphite-like carbon nitride in the solid content is 10-20 wt%; the gluing amount of the prepreg cloth is 45-60 wt%.
10. The production method according to claim 8, wherein the sintering and curing include a first sintering and curing stage, a second sintering and curing stage, and a third sintering and curing stage which are performed in this order; the temperature of the first sintering and curing stage is 80-90 ℃, and the heat preservation time is 100-120 min; the temperature of the second sintering and curing stage is 110-120 ℃, and the heat preservation time is 100-120 min; the temperature of the third sintering and curing stage is 170-180 ℃, and the heat preservation time is 60-120 min.
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