CN112063263A - Super-hydrophobic rGO-Ag-modified epoxy resin anticorrosive paint and preparation method thereof - Google Patents
Super-hydrophobic rGO-Ag-modified epoxy resin anticorrosive paint and preparation method thereof Download PDFInfo
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Abstract
The invention relates to the technical field of epoxy resin materials, and discloses an anticorrosive coating of super-hydrophobic rGO-Ag-modified epoxy resin, which comprises the following formula raw materials: modified graphene oxide, polyaniline-coated Ag and nano SiO2-epoxy resin composite, curing agent, dispersant. The super-hydrophobic rGO-Ag-modified epoxy resinModified nano SiO2The micro-nano mastoid structure is formed on the surface of the epoxy resin coating, the contact angle of the coating and water is increased, the rolling angle is reduced, the epoxy resin coating has good super-hydrophobic performance, the heptadecafluorodecyltriethoxysilane modified graphene oxide improves the compatibility of the graphene oxide and the epoxy resin, the graphene oxide is filled in the pores inside the epoxy resin, the barrier performance of the epoxy resin is improved, the permeation rate of corrosive media is reduced, the polyaniline coats the nano silver, the corrosion current of metal is reduced, and the electrochemical corrosion resistance and the biological corrosion resistance of the coating are enhanced.
Description
Technical Field
The invention relates to the technical field of epoxy resin materials, in particular to an anticorrosive paint of super-hydrophobic rGO-Ag-modified epoxy resin and a preparation method thereof.
Background
The metal corrosion is caused by the damage to the metal under the chemical or electrochemical action of the surrounding medium and the combined action of physical or biological factors, the metal corrosion can be divided into chemical corrosion and electrochemical corrosion, the corrosion caused by the chemical action of the metal in dry gas and non-electrolyte solution is called as chemical corrosion, the product of the chemical corrosion exists on the surface of the metal, no current is generated in the corrosion process, the electrochemical corrosion refers to the damage caused by the electrochemical action generated between the metal and the electrolyte solution, it is characterized in that current is generated in the corrosion process, metal in the electrolyte solution is ionized under the action of water molecules, when the binding capacity of the metal ions and water molecules is greater than that of the metal ions and electrons thereof, the upper part of the metal ions is released from the metal surface into the electrolyte, and electrochemical corrosion is formed.
The epoxy resin is a polymer containing more than two epoxy groups in the molecule, is a thermosetting resin, the epoxy group has good chemical activity, the compound containing active hydrogen can open the ring, solidify and crosslink to generate a network structure, the main varieties of the epoxy resin comprise high temperature resistant glue, conductive glue, sealing glue, civil construction glue and the like, and the epoxy resin is widely applied to the fields of civil construction, electronic and electrical appliances, aerospace and aviation and the like, however, the prior epoxy resin material has poor corrosion resistance, and the epoxy resin is modified by adding the corrosion resistant material, however, the anticorrosive materials such as graphene, inorganic zinc, silver and the like are poor in dispersibility and compatibility in the epoxy resin, and are easy to agglomerate and agglomerate, so that the performance of the epoxy resin for blocking water molecules and oxygen is reduced, the anticorrosive new performance of the epoxy resin is influenced, and the materials are corroded.
Technical problem to be solved
Aiming at the defects of the prior art, the invention provides an anticorrosive coating of super-hydrophobic rGO-Ag-modified epoxy resin and a preparation method thereof, which solve the problem of low anticorrosive property of the epoxy resin and solve the problems of poor dispersibility and compatibility of inorganic materials in the epoxy resin.
(II) technical scheme
In order to achieve the purpose, the invention provides the following technical scheme: an ultra-hydrophobic rGO-Ag-modified epoxy resin anticorrosive paint comprises the following formula raw materials in parts by weight: 3-6 parts of modified graphene oxide, 15-22 parts of polyaniline-coated Ag, 67-80 parts of nano SiO2-epoxy resin composite material, 1-3 parts of curing agent and 1-2 parts of dispersing agent.
Preferably, the curing agent is N-dodecyl succinic anhydride.
Preferably, the dispersant is BYK-163.
Preferably, the nano SiO2The preparation method of the epoxy resin composite material can comprise the following steps:
(1) adding ethanol solvent into the reaction bottle, wherein the mass ratio of the ethanol solvent to the nano SiO is 8-12:12And silane coupling agent dodecyl trimethoxy silane, placing the reaction bottle in an ultrasonic disperser, performing ultrasonic dispersion treatment at 40-50 ℃ for 1-2h, placing the reaction bottle in a constant-temperature water bath kettle, heating to 75-85 ℃, stirring at constant speed for 2-3h, concentrating the solution under reduced pressure to remove the solvent, washing the solid product with distilled water, and fully drying to obtain the modified nano SiO2。
(2) Adding bisphenol A epoxy resin, glycidyl methacrylate and a catalyst dibutyltin dilaurate into a reaction bottle, placing the reaction bottle into an oil bath pot, heating to 125-135 ℃, stirring at constant speed, slowly dropwise adding hydroxyl-terminated polydimethylsiloxane, stirring at constant speed for reacting for 6-10h, cooling to 80-90 ℃, adding modified nano SiO into the solution2Stirring at constant speed for 5-8h to obtain nano SiO2-an epoxy resin composite.
Preferably, the bisphenol A epoxy resin, glycidyl methacrylate, dibutyltin dilaurate, hydroxyl-terminated polydimethylsiloxane and modified nano SiO2The mass ratio of the five components is 80-110:40-45:1:65-75: 60-90.
Preferably, the oil bath pot is including the pot body, and the right side at pot body top is provided with the operation panel, and the bath has been seted up at the top of the pot body and the left side that is located the operation panel, and the interior diapire fixedly connected with heating ring of bath, the inside fixedly connected with baffle of bath, even through-hole has been seted up at the top of baffle, and the apron has been placed to the opening part of bath, and the front of operation panel sets up display and main switch, and the operation panel sets up to the inclined plane, and apron top fixed mounting has the handle, and it all adopts.
Preferably, the preparation method of the modified graphene oxide comprises the following steps:
(1) adding ethanol solvent, graphene oxide and silane coupling agent heptadecafluorodecyltriethoxysilane into a reaction bottle, placing the reaction bottle into an ultrasonic dispersion instrument, carrying out ultrasonic dispersion treatment at 40-50 ℃ for 1-3h, placing the reaction bottle into a constant-temperature water bath kettle, heating to 75-85 ℃, stirring at a constant speed for reaction for 10-15h, carrying out reduced pressure concentration on the solution to remove the solvent, washing the solid product with distilled water, and fully drying to prepare the modified graphene oxide.
Preferably, the mass ratio of the graphene oxide to the silane coupling agent heptadecafluorodecyltriethoxysilane is 18-25: 1.
Preferably, the preparation method of the polyaniline-coated Ag comprises the following steps:
(1) adding hydrochloric acid solution with the substance amount concentration of 0.1-0.15mol/L into a reaction bottle, adding simple substance nano silver and aniline, placing the reaction bottle into an ultrasonic dispersion instrument, carrying out ultrasonic dispersion treatment for 1-2h, placing the reaction bottle into a low-temperature cooling instrument, stirring the solution at a constant speed and adding an initiator potassium persulfate at the temperature of-5-0 ℃, reacting for 8-12h, standing for 2-3h, filtering the solution to remove a solvent, washing a solid product by using distilled water and diethyl ether until the solid product is neutral, and fully drying to prepare the polyaniline-coated nano Ag.
Preferably, the molar ratio of the elementary nano silver to the substances of aniline and potassium persulfate is 0.2-0.4:1.1-1.3: 1.
Preferably, the super-hydrophobic rGO-Ag-modified epoxy resin anticorrosive paint
(1) Adding toluene solvent and 67-80 parts of nano SiO into a reaction bottle2The preparation method comprises the following steps of (1) preparing an epoxy resin composite material, 3-6 parts of modified graphene oxide, 15-22 parts of polyaniline-coated Ag and 1-2 parts of a dispersant BYK-163, controlling the solid-liquid ratio of a solution to be 75-90%, placing a reaction bottle in an ultrasonic dispersion instrument, carrying out ultrasonic dispersion treatment for 1-2h at the temperature of 60-80 ℃, adding 1-3 parts of curing agent N-dodecyl succinic anhydride, and stirring at a constant speed for 4-6h to prepare the super-hydrophobic rGO-Ag-modified epoxy resin anticorrosive paint.
(III) advantageous technical effects
Compared with the prior art, the invention has the following beneficial technical effects:
the super-hydrophobic rGO-Ag-modified epoxy resin anticorrosive paint uses a hydrophobic long alkyl chain silane coupling agent dodecyl trimethoxy silane to graft and modify nano SiO2Nano SiO2The micro-nano mastoid structure is formed on the surface of the epoxy resin coating, so that the contact angle of the coating and water is increased, the rolling angle is reduced, the epoxy resin coating has good super-hydrophobic performance, the adhesion of water molecules on the surface of the coating is reduced, and the corrosion process is inhibited.
According to the super-hydrophobic rGO-Ag-modified epoxy resin anticorrosive paint, the silane coupling agent heptadecafluorodecyltriethoxysilane modified graphene oxide with extremely strong hydrophobicity is used, so that the compatibility of the graphene oxide and the epoxy resin is improved, meanwhile, the graphene oxide is filled into pores inside the epoxy resin to form a microscopic zigzag path, the blocking performance of the epoxy resin is improved, the permeation of water molecules and oxygen is inhibited, the permeation rate of corrosive media is reduced, and the anticorrosive performance of an epoxy resin coating is enhanced.
According to the super-hydrophobic rGO-Ag-modified epoxy resin anticorrosive coating, polyaniline is formed on the surface of nano-silver by using an in-situ polymerization method, the polyaniline has good anticorrosive performance, the corrosion current of metal is reduced, oxidation reaction is carried out on the polyaniline and oxygen, and the permeation of oxygen is inhibited, so that the anticorrosive performance of the epoxy resin is greatly enhanced, hydrogen bonds are formed between imino groups of the polyaniline and ether bonds of the epoxy resin, the polyaniline and the epoxy resin are mixed and dissolved, the compatibility and the dispersibility of the nano-silver in the epoxy resin are enhanced, the nano-silver has excellent sterilization and antimicrobial effects, and an epoxy resin coating has good biological corrosion resistance.
Drawings
FIG. 1 is a front view of the connection structure of the present invention;
FIG. 2 is a cross-sectional view of the connection structure of the present invention;
FIG. 3 is a top view of the connection structure of the present invention;
FIG. 4 is a schematic view of the spacer in the connection structure of the present invention.
In the figure: 1-pot body, 2-operation table, 3-bath, 4-heating ring, 5-clapboard, 6-through hole and 7-cover plate.
Detailed Description
To achieve the above object, the present invention provides the following embodiments and examples: an ultra-hydrophobic rGO-Ag-modified epoxy resin anticorrosive paint comprises the following formula raw materials in parts by weight: 3-6 parts of modified graphene oxide, 15-22 parts of polyaniline-coated Ag, 67-80 parts of nano SiO2The epoxy resin composite material comprises 1-3 parts of a curing agent and 1-2 parts of a dispersing agent, wherein the curing agent is N-dodecyl succinic anhydride, and the preferred dispersing agent is BYK-163.
Nano SiO2The preparation method of the epoxy resin composite material can comprise the following steps:
(1) adding ethanol solvent into the reaction bottle, wherein the mass ratio of the ethanol solvent to the nano SiO is 8-12:12And silane coupling agent dodecyl trimethoxy silane, placing the reaction bottle in an ultrasonic disperser, performing ultrasonic dispersion treatment at 40-50 ℃ for 1-2h, placing the reaction bottle in a constant-temperature water bath kettle, heating to 75-85 ℃, stirring at constant speed for 2-3h, concentrating the solution under reduced pressure to remove the solvent, washing the solid product with distilled water, and fully drying to obtain the modified nano SiO2。
(2) Adding bisphenol A type epoxy resin, glycidyl methacrylate and catalyst dibutyltin dilaurate into a reaction bottle, placing the reaction bottle into an oil bath pot, wherein the oil bath pot comprises a pot body, the right side of the top of the pot body is provided with an operating platform, the top of the pot body and the left side of the operating platform are provided with a bath tank, the inner bottom wall of the bath tank is fixedly connected with a heating ring, and the inside of the bath tank is provided with a heating ringA partition board is fixedly connected with the bottom, a coupling through hole is arranged at the top of the partition board, a cover plate is arranged at the opening of the bath, a display and a main switch are arranged on the front surface of an operating platform, the operating platform is arranged to be an inclined plane, a handle is fixedly arranged at the top of the cover plate, the whole body is made of stainless steel, the operating platform is heated to 125 ℃ and 135 ℃, hydroxyl-terminated polydimethylsiloxane is stirred at constant speed and slowly dripped, the reaction is stirred at constant speed for 6 to 10 hours, the temperature is reduced to 80 to 90 ℃, and modified nano SiO is added2Wherein the bisphenol A epoxy resin, glycidyl methacrylate, dibutyltin dilaurate, hydroxyl terminated polydimethylsiloxane and modified nano SiO2The mass ratio of the five components is 80-110:40-45:1:65-75:60-90, and the mixture is stirred at a constant speed for 5-8 hours to prepare the nano SiO2-an epoxy resin composite.
The preparation method of the modified graphene oxide comprises the following steps:
(1) adding ethanol solvent, graphene oxide and silane coupling agent heptadecafluorodecyltriethoxysilane in a mass ratio of 18-25:1 into a reaction bottle, placing the reaction bottle into an ultrasonic dispersion instrument, carrying out ultrasonic dispersion treatment at 40-50 ℃ for 1-3h, placing the reaction bottle into a constant-temperature water bath kettle, heating to 75-85 ℃, stirring at a constant speed for 10-15h, carrying out reduced pressure concentration on the solution to remove the solvent, washing the solid product with distilled water, and fully drying to prepare the modified graphene oxide.
The preparation method of the polyaniline-coated Ag comprises the following steps:
(1) adding hydrochloric acid solution with the mass concentration of 0.1-0.15mol/L into a reaction bottle, adding simple substance nano silver and aniline, placing the reaction bottle into an ultrasonic dispersion instrument, performing ultrasonic dispersion treatment for 1-2h, placing the reaction bottle into a low-temperature cooling instrument, stirring the solution at a constant speed and adding an initiator potassium persulfate at the temperature of-5-0 ℃, wherein the mass molar ratio of the simple substance nano silver to the aniline to the potassium persulfate is 0.2-0.4:1.1-1.3:1, reacting for 8-12h, standing for 2-3h, filtering the solution to remove the solvent, washing a solid product with distilled water and ether until the solid product is neutral, and fully drying to prepare the polyaniline-coated nano Ag.
Super-hydrophobic rGO-Ag-modified epoxy resin anticorrosive paint
(1) Adding toluene solvent and 67-80 parts of nano SiO into a reaction bottle2The preparation method comprises the following steps of (1) preparing an epoxy resin composite material, 3-6 parts of modified graphene oxide, 15-22 parts of polyaniline-coated Ag and 1-2 parts of a dispersant BYK-163, controlling the solid-liquid ratio of a solution to be 75-90%, placing a reaction bottle in an ultrasonic dispersion instrument, carrying out ultrasonic dispersion treatment for 1-2h at the temperature of 60-80 ℃, adding 1-3 parts of curing agent N-dodecyl succinic anhydride, and stirring at a constant speed for 4-6h to prepare the super-hydrophobic rGO-Ag-modified epoxy resin anticorrosive paint.
Example 1
(1) Preparation of modified Nano SiO2Component 1: adding ethanol solvent into a reaction bottle, wherein the mass ratio of the ethanol solvent to the nano SiO is 8:12And silane coupling agent dodecyl trimethoxy silane, placing the reaction bottle in an ultrasonic disperser, performing ultrasonic dispersion treatment at 40 ℃ for 1h, placing the reaction bottle in a constant-temperature water bath kettle, heating to 75 ℃, stirring at a constant speed for 2h, performing reduced pressure concentration on the solution to remove the solvent, washing the solid product with distilled water, and fully drying to obtain the modified nano SiO2And (3) component 1.
(2) Preparation of nano SiO2Epoxy resin composite 1: adding bisphenol A epoxy resin, glycidyl methacrylate and a catalyst dibutyltin dilaurate into a reaction bottle, placing the reaction bottle into an oil bath pot, wherein the oil bath pot comprises a pot body, the right side of the top of the pot body is provided with an operating platform, the top of the pot body and the left side of the operating platform are provided with a bath tank, the inner bottom wall of the bath tank is fixedly connected with a heating ring, the inside of the bath tank is fixedly connected with a clapboard, the top of the clapboard is provided with a dual through hole, a cover plate is placed at the opening of the bath tank, the front of the operating platform is provided with a display and a main switch, the operating platform is arranged to be an inclined plane, the top of the cover plate is fixedly provided with a handle, the whole body is made of stainless steel, heating is carried out to 125 ℃, uniformly stirring and slowly dripping hydroxyl terminated polydimethylsiloxane, uniformly2 Component 1, wherein bisphenol A epoxy resin, glycidyl methacrylate, dibutyltin dilaurate, hydroxyl terminated polydimethylsiloxane and modified nano SiO2The mass ratio of the five is 80:40:1:65:60, and the mixture is stirred at a constant speed5h, preparing to obtain the nano SiO2-an epoxy resin composite 1.
(3) Preparing a modified graphene oxide component 1: adding ethanol solvent, graphene oxide and silane coupling agent heptadecafluorodecyltriethoxysilane in a mass ratio of 18:1 into a reaction bottle, placing the reaction bottle into an ultrasonic dispersion instrument, carrying out ultrasonic dispersion treatment at 40 ℃ for 1h, placing the reaction bottle into a constant-temperature water bath kettle, heating to 75 ℃, stirring at a constant speed for reaction for 10h, carrying out reduced pressure concentration on the solution to remove the solvent, washing the solid product with distilled water, and fully drying to prepare the modified graphene oxide component 1.
(4) Preparing a polyaniline-coated nano Ag component 1: adding hydrochloric acid solution with the mass concentration of 0.1mol/L into a reaction bottle, adding simple substance nano silver and aniline, placing the reaction bottle into an ultrasonic dispersion instrument, performing ultrasonic dispersion treatment for 1h, placing the reaction bottle into a low-temperature cooling instrument, stirring the solution at a constant speed at 0 ℃, adding an initiator potassium persulfate, wherein the mass molar ratio of the simple substance nano silver to the aniline to the potassium persulfate is 0.2:1.1:1, reacting for 8h, standing for 2h, filtering the solution to remove the solvent, washing the solid product with distilled water and diethyl ether until the solid product is neutral, and fully drying to prepare the polyaniline-coated nano Ag component 1.
(5) Preparing an anticorrosive coating of super-hydrophobic rGO-Ag-modified epoxy resin 1: adding toluene solvent and 80 parts of nano SiO into a reaction bottle2The preparation method comprises the following steps of preparing an epoxy resin composite material 1, 3 parts of a modified graphene oxide component 1, 15 parts of a polyaniline-coated Ag component 1 and 1 part of a dispersant BYK-163, controlling the solid-liquid ratio of a solution to be 75%, placing a reaction bottle in an ultrasonic disperser, carrying out ultrasonic dispersion treatment for 1h at 60 ℃, adding 1 part of curing agent N-dodecyl succinic anhydride, and stirring at a constant speed for 4h to prepare the super-hydrophobic rGO-Ag-modified epoxy resin anticorrosive paint 1.
Example 2
(1) Preparation of modified Nano SiO2And (2) component: adding ethanol solvent into a reaction bottle, wherein the mass ratio of the ethanol solvent to the nano SiO is 8:12And silane coupling agent dodecyl trimethoxy silane, placing the reaction flask in an ultrasonic disperser, performing ultrasonic dispersion treatment at 50 deg.C for 1h, and placing the reaction flask inHeating to 75 ℃ in a constant-temperature water bath kettle, stirring at a constant speed for 2h, concentrating the solution under reduced pressure to remove the solvent, washing the solid product with distilled water, and fully drying to prepare the modified nano SiO2And (3) component 2.
(2) Preparation of nano SiO2Epoxy resin composite 2: adding bisphenol A epoxy resin, glycidyl methacrylate and a catalyst dibutyltin dilaurate into a reaction bottle, placing the reaction bottle into an oil bath pot, wherein the oil bath pot comprises a pot body, the right side of the top of the pot body is provided with an operating platform, the top of the pot body and the left side of the operating platform are provided with a bath tank, the inner bottom wall of the bath tank is fixedly connected with a heating ring, the inside of the bath tank is fixedly connected with a clapboard, the top of the clapboard is provided with a dual through hole, a cover plate is placed at the opening of the bath tank, the front of the operating platform is provided with a display and a main switch, the operating platform is arranged to be an inclined plane, the top of the cover plate is fixedly provided with a handle, the whole body is made of stainless steel, heating is carried out to 125 ℃, uniformly stirring and slowly dripping hydroxyl terminated polydimethylsiloxane, uniformly2 Component 2, wherein bisphenol A epoxy resin, glycidyl methacrylate, dibutyltin dilaurate, hydroxyl-terminated polydimethylsiloxane and modified nano SiO2The mass ratio of the five materials is 110:40:1:65:60, and the mixture is stirred at a constant speed for 5 hours to prepare the nano SiO2-an epoxy resin composite 2.
(3) Preparing a modified graphene oxide component 2: adding ethanol solvent, graphene oxide and silane coupling agent heptadecafluorodecyltriethoxysilane in a mass ratio of 25:1 into a reaction bottle, placing the reaction bottle into an ultrasonic dispersion instrument, carrying out ultrasonic dispersion treatment at 50 ℃ for 3h, placing the reaction bottle into a constant-temperature water bath kettle, heating to 75 ℃, stirring at a constant speed for reaction for 10h, carrying out reduced pressure concentration on the solution to remove the solvent, washing the solid product with distilled water, and fully drying to prepare the modified graphene oxide component 2.
(4) Preparing a polyaniline-coated nano Ag component 2: adding hydrochloric acid solution with the mass concentration of 0.1mol/L into a reaction bottle, adding simple substance nano silver and aniline, placing the reaction bottle into an ultrasonic dispersion instrument, performing ultrasonic dispersion treatment for 2 hours, placing the reaction bottle into a low-temperature cooling instrument, stirring the solution at a constant speed at-5 ℃, adding an initiator potassium persulfate, wherein the mass molar ratio of the simple substance nano silver to the aniline to the potassium persulfate is 0.4:1.3:1, reacting for 12 hours, standing for 2 hours, filtering the solution to remove the solvent, washing the solid product with distilled water and diethyl ether until the solid product is neutral, and fully drying to prepare the polyaniline-coated nano Ag component 2.
(5) Preparing an anticorrosive coating of super-hydrophobic rGO-Ag-modified epoxy resin 2: adding toluene solvent and 76 parts of nano SiO into a reaction bottle2The preparation method comprises the following steps of preparing an epoxy resin composite material 2, 4 parts of a modified graphene oxide component 2, 17.3 parts of a polyaniline-coated Ag component 2 and 1.2 parts of a dispersant BYK-163, controlling the solid-to-liquid ratio of the solution to be 75%, placing a reaction bottle in an ultrasonic disperser, carrying out ultrasonic dispersion treatment at 60 ℃ for 1h, adding 1.5 parts of curing agent N-dodecyl succinic anhydride, and stirring at a constant speed for 6h to prepare the super-hydrophobic rGO-Ag-modified epoxy resin anticorrosive paint 2.
Example 3
(1) Preparation of modified Nano SiO2And (3) component: adding ethanol solvent into a reaction bottle, wherein the mass ratio of the ethanol solvent to the nano SiO is 10:12And silane coupling agent dodecyl trimethoxy silane, placing the reaction bottle in an ultrasonic disperser, performing ultrasonic dispersion treatment at 45 ℃ for 1.5h, placing the reaction bottle in a constant-temperature water bath kettle, heating to 80 ℃, stirring at a constant speed for 2.5h, performing reduced pressure concentration on the solution to remove the solvent, washing the solid product with distilled water, and fully drying to obtain the modified nano SiO2And (3) component.
(2) Preparation of nano SiO2Epoxy resin composite 3: to adding bisphenol A type epoxy resin in the reaction bottle, glycidyl methacrylate and catalyst dibutyltin dilaurate, arrange the reaction bottle in the oil bath pot, the oil bath pot is including the pot body, the right side at pot body top is provided with the operation panel, the top of the pot body and the left side that is located the operation panel have seted up the bath, interior diapire fixedly connected with heating ring in the bath, the inside fixedly connected with baffle in bath, even through-hole has been seted up at the top of baffle, the apron has been placed to the opening part in bath, the front of operation panel sets up display and main switch, the operation panel sets up to obliqueA handle is fixedly arranged on the top of the cover plate, the whole cover plate is made of stainless steel, the mixture is heated to 130 ℃, stirred at a constant speed, slowly dripped with hydroxyl-terminated polydimethylsiloxane, stirred at a constant speed for reaction for 8 hours, the temperature is reduced to 85 ℃, and modified nano SiO is added into the solution2Component 3, wherein bisphenol A epoxy resin, glycidyl methacrylate, dibutyltin dilaurate, hydroxyl-terminated polydimethylsiloxane and modified nano SiO2The mass ratio of the five materials is 95:42:1:70:75, and the mixture is stirred at a constant speed for 6 hours to prepare the nano SiO2-an epoxy resin composite 3.
(3) Preparing a modified graphene oxide component 3: adding ethanol solvent, graphene oxide and silane coupling agent heptadecafluorodecyltriethoxysilane in a mass ratio of 22:1 into a reaction bottle, placing the reaction bottle into an ultrasonic dispersion instrument, carrying out ultrasonic dispersion treatment at 45 ℃ for 2 hours, placing the reaction bottle into a constant-temperature water bath kettle, heating to 80 ℃, stirring at a constant speed for reaction for 12 hours, carrying out reduced pressure concentration on the solution to remove the solvent, washing the solid product with distilled water, and fully drying to prepare the modified graphene oxide component 3.
(4) Preparing a polyaniline-coated nano Ag component 3: adding hydrochloric acid solution with the mass concentration of 0.12mol/L into a reaction bottle, adding simple substance nano silver and aniline, placing the reaction bottle into an ultrasonic dispersion instrument, performing ultrasonic dispersion treatment for 1.5h, placing the reaction bottle into a low-temperature cooling instrument, stirring the solution at a constant speed at-5 ℃, adding an initiator potassium persulfate, wherein the mass molar ratio of the simple substance nano silver to the aniline to the potassium persulfate is 0.3:1.2:1, reacting for 10h, standing for 2.5h, filtering the solution to remove a solvent, washing a solid product by using distilled water and diethyl ether until the solid product is neutral, and fully drying to prepare the polyaniline-coated nano Ag component 3.
(5) Preparing an anticorrosive coating of super-hydrophobic rGO-Ag-modified epoxy resin 3: adding toluene solvent and 74 parts of nano SiO into a reaction bottle 23 parts of epoxy resin composite material, 4.5 parts of modified graphene oxide component 3, 18 parts of polyaniline-coated Ag component 3 and 1.5 parts of dispersant BYK-163, wherein the solid-to-liquid ratio of the solution is controlled to be 82%, the reaction bottle is placed in an ultrasonic dispersion instrument, ultrasonic dispersion treatment is carried out for 1.5h at 70 ℃, and then 2 parts of dispersant are addedCuring agent N-dodecyl succinic anhydride, stirring at constant speed for 5h to prepare the super-hydrophobic rGO-Ag-modified epoxy resin anticorrosive paint 3.
Example 4
(1) Preparation of modified Nano SiO2And (4) component: adding ethanol solvent into a reaction bottle, wherein the mass ratio of the ethanol solvent to the nano SiO is 8:12And silane coupling agent dodecyl trimethoxy silane, placing the reaction bottle in an ultrasonic disperser, performing ultrasonic dispersion treatment at 50 ℃ for 2h, placing the reaction bottle in a constant-temperature water bath kettle, heating to 75 ℃, stirring at uniform speed for 3h, removing the solvent by concentrating the solution under reduced pressure, washing the solid product with distilled water, fully drying, and preparing the modified nano SiO2And (4) component.
(2) Preparation of nano SiO2Epoxy resin composite 4: adding bisphenol A epoxy resin, glycidyl methacrylate and a catalyst dibutyltin dilaurate into a reaction bottle, placing the reaction bottle into an oil bath pot, wherein the oil bath pot comprises a pot body, the right side of the top of the pot body is provided with an operating platform, the top of the pot body and the left side of the operating platform are provided with a bath tank, the inner bottom wall of the bath tank is fixedly connected with a heating ring, the inside of the bath tank is fixedly connected with a clapboard, the top of the clapboard is provided with a dual through hole, a cover plate is placed at the opening of the bath tank, the front of the operating platform is provided with a display and a main switch, the operating platform is arranged to be an inclined plane, the top of the cover plate is fixedly provided with a handle, the whole body is made of stainless steel, heating is carried out to 135 ℃, uniformly stirring and slowly dripping hydroxyl terminated polydimethylsiloxane, uniformly2Component 4, wherein bisphenol A epoxy resin, glycidyl methacrylate, dibutyltin dilaurate, hydroxyl-terminated polydimethylsiloxane and modified nano SiO2The mass ratio of the five materials is 110:40:1:65:60, and the mixture is stirred at a constant speed for 8 hours to prepare the nano SiO2An epoxy resin composite 4.
(3) Preparing a modified graphene oxide component 4: adding ethanol solvent, graphene oxide and silane coupling agent heptadecafluorodecyltriethoxysilane in a mass ratio of 18:1 into a reaction bottle, placing the reaction bottle into an ultrasonic dispersion instrument, carrying out ultrasonic dispersion treatment at 40 ℃ for 3h, placing the reaction bottle into a constant-temperature water bath kettle, heating to 85 ℃, stirring at a constant speed for reaction for 15h, carrying out reduced pressure concentration on the solution to remove the solvent, washing the solid product with distilled water, and fully drying to prepare the modified graphene oxide component 4.
(4) Preparing a polyaniline-coated nano Ag component 4: adding hydrochloric acid solution with the mass concentration of 0.15mol/L into a reaction bottle, adding simple substance nano silver and aniline, placing the reaction bottle into an ultrasonic dispersion instrument, performing ultrasonic dispersion treatment for 1h, placing the reaction bottle into a low-temperature cooling instrument, stirring the solution at a constant speed at 0 ℃, adding an initiator potassium persulfate, wherein the mass molar ratio of the simple substance nano silver to the aniline to the potassium persulfate is 0.4:1.1:1, reacting for 12h, standing for 2h, filtering the solution to remove the solvent, washing the solid product with distilled water and diethyl ether until the solid product is neutral, and fully drying to prepare the polyaniline-coated nano Ag component 4.
(5) Preparing an anticorrosive coating of super-hydrophobic rGO-Ag-modified epoxy resin 4: adding a toluene solvent and 71 parts of nano SiO into a reaction bottle 24 parts of epoxy resin composite material, 4.5 parts of modified graphene oxide component 4, 20.3 parts of polyaniline-coated Ag component 4 and 1.7 parts of dispersant BYK-163, wherein the solid-to-liquid ratio of the solution is controlled to be 86%, the reaction bottle is placed in an ultrasonic disperser, ultrasonic dispersion treatment is carried out for 1.5h at 70 ℃, 2.5 parts of curing agent N-dodecyl succinic anhydride is added, and stirring is carried out at constant speed for 5h to prepare the super-hydrophobic rGO-Ag-modified epoxy resin anticorrosive paint 4.
Example 5
(1) Preparation of modified Nano SiO2And (5) component: adding ethanol solvent into a reaction bottle, wherein the mass ratio of the ethanol solvent to the nano SiO is 12:12And silane coupling agent dodecyl trimethoxy silane, placing the reaction bottle in an ultrasonic disperser, performing ultrasonic dispersion treatment at 50 ℃ for 2h, placing the reaction bottle in a constant-temperature water bath kettle, heating to 85 ℃, stirring at a constant speed for 3h, performing reduced pressure concentration on the solution to remove the solvent, washing the solid product with distilled water, and fully drying to obtain the modified nano SiO2And (5) component.
(2) Preparation of nano SiO2Epoxy resin composite 5: adding bisphenol into a reaction flaskA type epoxy resin, glycidyl methacrylate and catalyst dibutyltin dilaurate, place the reaction bottle in the oil bath pot, the oil bath pot is including the pot body, the right side at pot body top is provided with the operation panel, the top of the pot body and the left side that is located the operation panel have seted up the bath, inner diapire fixedly connected with heating ring in the bath, the inside fixedly connected with baffle in the bath, even through-hole has been seted up at the top of baffle, the apron has been placed to the opening part of bath, the front of operation panel sets up display and main switch, the operation panel sets up to the inclined plane, apron top fixed mounting has the handle, it is whole to adopt the stainless steel to make, heat to 135 ℃, at the uniform velocity stirring and slowly dropwise add hydroxyl terminated polydimethylsiloxane, at the uniform velocity stirring reaction 10h, reduce the temperature to 90 ℃, to2Component 5, wherein bisphenol A epoxy resin, glycidyl methacrylate, dibutyltin dilaurate, hydroxyl-terminated polydimethylsiloxane and modified nano SiO2The mass ratio of the five materials is 110:45:1:75:90, and the mixture is stirred at a constant speed for 6 hours to prepare the nano SiO2-an epoxy resin composite 5.
(3) Preparing a modified graphene oxide component 5: adding ethanol solvent, graphene oxide and silane coupling agent heptadecafluorodecyltriethoxysilane in a mass ratio of 25:1 into a reaction bottle, placing the reaction bottle into an ultrasonic dispersion instrument, carrying out ultrasonic dispersion treatment at 50 ℃ for 3h, placing the reaction bottle into a constant-temperature water bath kettle, heating to 85 ℃, stirring at a constant speed for reaction for 15h, carrying out reduced pressure concentration on the solution to remove the solvent, washing the solid product with distilled water, and fully drying to prepare the modified graphene oxide component 5.
(4) Preparing a polyaniline-coated nano Ag component 5: adding hydrochloric acid solution with the mass concentration of 0.15mol/L into a reaction bottle, adding simple substance nano silver and aniline, placing the reaction bottle into an ultrasonic dispersion instrument, performing ultrasonic dispersion treatment for 2 hours, placing the reaction bottle into a low-temperature cooling instrument, stirring the solution at a constant speed at-5 ℃, adding an initiator potassium persulfate, wherein the mass molar ratio of the simple substance nano silver to the aniline to the potassium persulfate is 0.4:1.3:1, reacting for 12 hours, standing for 3 hours, filtering the solution to remove the solvent, washing the solid product with distilled water and diethyl ether until the solid product is neutral, and fully drying to prepare the polyaniline-coated nano Ag component 5.
(5) Preparing an anticorrosive paint of super-hydrophobic rGO-Ag-modified epoxy resin 5: adding toluene solvent and 80 parts of nano SiO into a reaction bottle 25 parts of epoxy resin composite material, 6 parts of modified graphene oxide component 5, 22 parts of polyaniline-coated Ag component 5 and 2 parts of dispersant BYK-163, controlling the solid-liquid ratio of the solution to be 90%, placing a reaction bottle in an ultrasonic disperser, performing ultrasonic dispersion treatment at 80 ℃ for 2h, adding 3 parts of curing agent N-dodecyl succinic anhydride, and stirring at a constant speed for 6h to prepare the super-hydrophobic rGO-Ag-modified epoxy resin anticorrosive paint 5.
The super-hydrophobic rGO-Ag-modified epoxy resin anticorrosive coatings in the examples 1-5 are cured into films, and the salt spray resistance of the film materials is tested by placing the films in a JYWX-020 alternating salt spray test box, wherein the test standard is GBT 2423.18-2000.
In summary, the super-hydrophobic rGO-Ag-modified epoxy resin anticorrosive paint uses the hydrophobic long alkyl chain silane coupling agent dodecyl trimethoxy silane to graft and modify nano SiO2Nano SiO2The micro-nano mastoid structure is formed on the surface of the epoxy resin coating, so that the contact angle of the coating and water is increased, the rolling angle is reduced, the epoxy resin coating has good super-hydrophobic performance, the adhesion of water molecules on the surface of the coating is reduced, and the corrosion process is inhibited.
The silane coupling agent heptadecafluorodecyltriethoxysilane modified graphene oxide with extremely strong hydrophobicity is used, so that the compatibility of the graphene oxide and epoxy resin is improved, meanwhile, the graphene oxide is filled into pores inside the epoxy resin to form a microscopic tortuous path, the barrier property of the epoxy resin is improved, the permeation of water molecules and oxygen is inhibited, the permeation rate of corrosive media is reduced, and the corrosion resistance of the epoxy resin coating is enhanced.
Polyaniline is formed on the surface of the nano-silver by using an in-situ polymerization method, the polyaniline has good corrosion resistance, the corrosion current of metal is reduced, the polyaniline and oxygen generate oxidation reaction, and the penetration of oxygen is inhibited, so that the corrosion resistance of epoxy resin is greatly enhanced, the imino group of the polyaniline and the ether bond of the epoxy resin form a hydrogen bond, the polyaniline and the epoxy resin are mixed and dissolved, the compatibility and the dispersibility of the nano-silver in the epoxy resin are enhanced, the nano-silver has excellent sterilization and antimicrobial effects, and the epoxy resin coating has good biological corrosion resistance.
Claims (11)
1. The super-hydrophobic rGO-Ag-modified epoxy resin anticorrosive paint comprises the following formula raw materials in parts by weight, and is characterized in that: 3-6 parts of modified graphene oxide, 15-22 parts of polyaniline-coated Ag, 67-80 parts of nano SiO2-epoxy resin composite material, 1-3 parts of curing agent and 1-2 parts of dispersing agent.
2. The super-hydrophobic rGO-Ag-modified epoxy resin anticorrosive paint according to claim 1, characterized in that: the curing agent is N-dodecyl succinic anhydride.
3. The super-hydrophobic rGO-Ag-modified epoxy resin anticorrosive paint according to claim 1, characterized in that: the dispersant is BYK-163.
4. The super-hydrophobic rGO-Ag-modified epoxy resin anticorrosive paint according to claim 1, characterized in that: the nano SiO2The preparation method of the epoxy resin composite material can comprise the following steps:
(1) adding nano SiO with the mass ratio of 8-12:1 into an ethanol solvent2And silane coupling agent dodecyl trimethoxy silane, performing ultrasonic dispersion treatment on the solution at 40-50 ℃ for 1-2h, heating the solution to 75-85 ℃, reacting for 2-3h, removing the solvent from the solution, washing a solid product, and drying to prepare the modified nano SiO2。
(2) To bisphenol A type epoxy resin, glycidyl methacrylate was addedEster and catalyst dibutyltin dilaurate, heating the solution to 125-135 ℃ in an oil bath, stirring at constant speed, slowly dropwise adding hydroxyl-terminated polydimethylsiloxane, reacting for 6-10h, cooling to 80-90 ℃, and adding modified nano SiO into the solution2Stirring at constant speed for 5-8h to obtain nano SiO2-an epoxy resin composite.
5. The super-hydrophobic rGO-Ag-modified epoxy resin anticorrosive paint according to claim 4, characterized in that: the bisphenol A epoxy resin, glycidyl methacrylate, dibutyltin dilaurate, hydroxyl-terminated polydimethylsiloxane and modified nano SiO2The mass ratio of the five components is 80-110:40-45:1:65-75: 60-90.
6. The super-hydrophobic rGO-Ag-modified epoxy resin anticorrosive paint according to claim 4, characterized in that: the oil bath pot is provided with operation panel (2) including the pot body (1), the right side at the pot body (1) top, bath (3) have been seted up at the top of the pot body (1) and the left side that is located operation panel (2), interior diapire fixedly connected with heating ring (4) of bath (3), inside fixedly connected with baffle (5) of bath (3), even through-hole (6) have been seted up at the top of baffle (5), apron (7) have been placed to the opening part of bath (3), and the front of operation panel (1) sets up display and main switch, and operation panel (1) sets up to the inclined plane, and apron (7) top fixed mounting has the handle, and it all adopts the stainless steel to make.
7. The super-hydrophobic rGO-Ag-modified epoxy resin anticorrosive paint according to claim 1, characterized in that: the preparation method of the modified graphene oxide comprises the following steps:
(1) adding graphene oxide and a silane coupling agent heptadecafluorodecyltriethoxysilane into an ethanol solvent, carrying out ultrasonic dispersion treatment on the solution at 40-50 ℃ for 1-3h, heating the solution to 75-85 ℃, reacting for 10-15h, removing the solvent from the solution, washing a solid product, and drying to prepare the modified graphene oxide.
8. The super-hydrophobic rGO-Ag-modified epoxy resin anticorrosive paint according to claim 7, characterized in that: the mass ratio of the graphene oxide to the silane coupling agent heptadecafluorodecyltriethoxysilane is 18-25: 1.
9. The super-hydrophobic rGO-Ag-modified epoxy resin anticorrosive paint according to claim 1, characterized in that: the preparation method of the polyaniline-coated Ag comprises the following steps:
(1) adding simple substance nano silver and aniline into hydrochloric acid solution with the mass concentration of 0.1-0.15mol/L, performing ultrasonic dispersion treatment on the solution for 1-2h, stirring the solution at a constant speed at-5-0 ℃, adding an initiator potassium persulfate, reacting for 8-12h, standing for 2-3h, removing the solvent from the solution, washing a solid product, and drying to prepare the polyaniline-coated nano Ag.
10. The super-hydrophobic rGO-Ag-modified epoxy resin anticorrosive paint according to claim 9, characterized in that: the mass molar ratio of the simple substance nano silver to the aniline to the potassium persulfate is 0.2-0.4:1.1-1.3: 1.
11. The super-hydrophobic rGO-Ag-modified epoxy resin anticorrosive paint according to claim 1, characterized in that: super-hydrophobic rGO-Ag-modified epoxy resin anticorrosive paint
(1) Adding 67-80 parts of nano SiO into toluene solvent2The preparation method comprises the following steps of (1) preparing an epoxy resin composite material, 3-6 parts of modified graphene oxide, 15-22 parts of polyaniline-coated Ag and 1-2 parts of a dispersant BYK-163, controlling the solid-liquid ratio of a solution to be 75-90%, carrying out ultrasonic dispersion treatment on the solution at 60-80 ℃ for 1-2h, adding 1-3 parts of curing agent N-dodecyl succinic anhydride, and stirring at a constant speed for 4-6h to obtain the super-hydrophobic rGO-Ag modified epoxy resin anticorrosive paint.
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