CN112111200A - Preparation method of high-temperature-resistant water-based heat-conducting anticorrosive paint - Google Patents
Preparation method of high-temperature-resistant water-based heat-conducting anticorrosive paint Download PDFInfo
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Abstract
The invention discloses a preparation method of a high-temperature-resistant water-based heat-conducting anticorrosive coating, which comprises the following raw materials in parts by weight: 15-35 parts of modified carbon nano particles, 5-10 parts of anticorrosive filler, 75-90 parts of waterborne fluorocarbon resin, 3-8 parts of defoaming agent, 3-5 parts of curing agent and 150 parts of deionized water; adding the modified carbon nano particles into deionized water, ultrasonically oscillating and stirring for 15min to prepare a suspension, sequentially adding the suspension, the aqueous fluorocarbon resin, the defoaming agent and the curing agent into a ball mill, and performing ball milling for 2h to prepare the high-temperature-resistant aqueous heat-conducting anticorrosive coating; the prepared modified carbon nano particles can be stacked and connected with the matrix macromolecular chain segment, so that the density is increased, and the heat conductivity of the prepared coating is improved.
Description
Technical Field
The invention belongs to the technical field of anticorrosive paint preparation, and particularly relates to a preparation method of a high-temperature-resistant water-based heat-conducting anticorrosive paint.
Background
The most of the antirust paint anticorrosive coatings used in the current market are solvent-based coatings, and the most serious defects of the coatings are environmental pollution, flammability and explosiveness, harm to human bodies and waste of a large amount of resources and energy. The existing water-based anticorrosive paint widely applied to the market comprises water-based inorganic zinc-rich and water-based epoxy paint, and the like, and the paint is applied to primer, has high requirement on substrate treatment and is fussy to construct. The water-based acrylic acid anticorrosive paint is produced by some foreign manufacturers, but has poor anticorrosive salt spray resistance and adhesive force, and the anticorrosive pigments such as iron oxide red, composite ferrotitanium powder and the like are mainly used in water-based acrylic acid anticorrosion, are not suitable for color matching, and have poor finish paint effect when being used.
The Chinese invention patent CN102702899A discloses a water-based modified pure acrylic acid anticorrosive paint, which comprises the following components in percentage by mass: 30-45% of modified acrylic emulsion, 3-5% of film-forming additive, 0.6-1.2% of dispersing agent, 0.1-1.0% of defoaming agent, 0.1-0.2% of wetting agent, 0.05-0.10% of mildew preventive, 1-2% of anti-flash rust agent, 2-5% of pigment, 15-30% of anti-rust pigment filler, 2-5% of thickening agent, 1-2.5% of salt-resistant fog agent, 8-9% of pH value adjustment and the balance of water.
Disclosure of Invention
In order to overcome the technical problems, the invention provides a preparation method of a high-temperature-resistant water-based heat-conducting anticorrosive coating.
The carbon nano tube has a small specific surface area and is easy to agglomerate, active groups such as carboxyl groups and the like can be introduced to the carbon nano tube in the acid washing process, the dispersing performance of the carbon nano tube is improved, the nano filler is prepared and can be uniformly dispersed in deionized water, step S2 is to add the nano filler into the deionized water to prepare a suspension B, sodium tripolyphosphate is added to serve as a dispersing agent, 4 mass percent of polyvinyl alcohol aqueous solution is added to serve as a thickening agent to modify the carbon nano tube, the dispersing performance of the carbon nano tube in a solvent is further enhanced, and the prepared modified carbon nano particles can be stacked and connected with a matrix macromolecule chain segment, so that the density is increased, and the heat conducting performance of the prepared coating is further improved.
The purpose of the invention can be realized by the following technical scheme:
a preparation method of a high-temperature-resistant water-based heat-conducting anticorrosive coating comprises the following steps:
firstly, weighing the following raw materials in parts by weight: 15-35 parts of modified carbon nano particles, 5-10 parts of anticorrosive filler, 75-90 parts of waterborne fluorocarbon resin, 3-8 parts of defoaming agent, 3-5 parts of curing agent and 150 parts of deionized water;
and secondly, adding the modified carbon nano particles into deionized water, carrying out ultrasonic oscillation and stirring for 15min at the rotating speed of 180-.
Further, the defoaming agent is one or two of trialkyl melamine and dimethyl siloxane which are mixed according to any proportion, and the curing agent is one or two of vinyl triamine and m-phenylenediamine which are mixed according to any proportion.
Further, the modified carbon nanoparticles are prepared by the following method:
step S1, adding carbon nanotubes into a three-neck flask filled with concentrated sulfuric acid and concentrated nitric acid, controlling the weight ratio of the concentrated sulfuric acid to the concentrated nitric acid to be 3: 1, uniformly stirring at a rotation speed of 100-120r/min for 15min, then placing the mixture into a water bath kettle at 80-90 ℃, stirring at the temperature for 30min, cooling to 30-35 ℃ after stirring, standing for 1h to prepare a suspension A, pouring the suspension A into a beaker filled with deionized water, standing for 1h, performing suction filtration, and washing a filter cake with the deionized water until the filtrate is neutral to prepare the nanofiller;
and S2, adding the nano filler prepared in the step S1 into deionized water, uniformly stirring at a speed of 240 plus 280r/min and ultrasonically dispersing for 30min to prepare a suspension B, controlling the ultrasonic power to be 50-60W, adding sodium tripolyphosphate into the suspension B, continuously stirring for 30min, dropwise adding a polyvinyl alcohol aqueous solution with the mass fraction of 4%, controlling the dropwise adding time to be 15min, heating in a water bath at 60-65 ℃, irradiating by using an infrared lamp until the solution is completely dried, and grinding to prepare the modified carbon nano particles.
Step S1, adding a carbon nano tube into a three-neck flask filled with concentrated sulfuric acid and concentrated nitric acid, removing residual catalyst and amorphous carbon impurities in the carbon nano tube in the preparation process by strong acid washing of the concentrated sulfuric acid and the concentrated nitric acid, wherein the carbon nano tube has a small specific surface area and is easy to agglomerate, active groups such as carboxyl groups can be introduced onto the carbon nano tube in the acid washing process to improve the dispersion performance of the carbon nano tube, the nano filler can be uniformly dispersed in deionized water, step S2, the nano filler is added into the deionized water to prepare a suspension B, sodium tripolyphosphate is added as a dispersing agent, a polyvinyl alcohol aqueous solution with the mass fraction of 4% is added as a thickening agent to modify the carbon nano tube, the dispersion performance of the nano filler in a solvent is further enhanced, and the prepared modified carbon nano particle can be stacked and connected with a matrix macromolecular chain segment to increase the density, thereby improving the heat-conducting property of the prepared coating.
Further, in the step S1, the dosage ratio of the carbon nano tube to the concentrated sulfuric acid is controlled to be 2-3 g: 120-150mL, the mass fraction of the concentrated sulfuric acid is 75%, the mass fraction of the concentrated nitric acid is 70%, the weight ratio of the nano filler to the deionized water is controlled to be 1: 50 in the step S2, and the weight ratio of the nano filler, the sodium tripolyphosphate and the 4% polyvinyl alcohol aqueous solution is 1: 0.1-0.3: 3-5.
Further, the anti-corrosion filler is prepared by the following method:
step S11, adding beta-cyclodextrin into deionized water, stirring at a constant speed until the beta-cyclodextrin is completely dissolved, preparing a beta-cyclodextrin aqueous solution with the mass fraction of 50%, adding clove essential oil into an ethanol aqueous solution with the volume fraction of 10%, stirring at a constant speed for 15min to prepare a mixed solution a, dropwise adding the mixed solution a into the beta-cyclodextrin aqueous solution with the mass fraction of 50%, controlling the dropwise adding time to be 30min, heating in a water bath at 45-50 ℃ and stirring magnetically for 30min, refrigerating and standing at 2-5 ℃ after stirring for 20h, performing suction filtration, washing a filter cake with absolute ethyl alcohol and deionized water for three times respectively, and then drying at 50-60 ℃ to constant weight to prepare a first product;
step S12, adding magnesium nitrate and aluminum nitrate into a beaker filled with deionized water, uniformly stirring, adding sodium hydroxide, heating in a water bath at 35-40 ℃ and magnetically stirring, then transferring into a three-neck flask, introducing nitrogen gas during the adding process, stirring at a rotating speed of 400r/min, completely adding, crystallizing at 70 ℃ for 20 hours, performing suction filtration, washing with deionized water at 45 ℃ for three times, and performing vacuum drying at 100 ℃ for 4 hours to obtain a second product;
step S13, adding sodium p-styrene sulfonate into deionized water, stirring at a constant speed for 10min, adding a second product, controlling the weight ratio of the sodium p-styrene sulfonate to the second product to be 1: 15, heating in a water bath at 35-40 ℃, stirring at a constant speed for 2h, filtering, washing with deionized water three times, drying at 70 ℃ for 40h to obtain a third product, and mixing the first product and the third product according to the weight ratio of 0.3-0.5: 1 to obtain the anticorrosive filler.
The clove essential oil is a natural bacteriostatic agent, but the clove essential oil has pungent smell, and the coating prepared by using the clove essential oil as an antibacterial agent has pungent smell, so that in the step S11, a beta-cyclodextrin aqueous solution is prepared firstly, then the clove essential oil is dissolved in an ethanol aqueous solution, and then a microcapsule-shaped intermediate with the beta-cyclodextrin as a wall material and the clove essential oil as a core material is prepared by mixing; in the step S12, a second product is prepared from raw materials such as magnesium nitrate and aluminum nitrate, the second product has active groups such as hydroxyl groups and the like, the surface energy is large, the surface structure of the second product is unstable, hydrogen bonds are easy to generate to form agglomeration, the second product is an inorganic material, the compatibility is poor when the second product is mixed with a matrix material, and the second product cannot be uniformly dispersed in the matrix, so that S13 modifies the second product through sodium styrene sulfonate to organize the surface of the second product, the surface is passivated, the agglomeration phenomenon can be prevented, styrene sulfonate ions can enter between filler layers in the modification process, the interlayer spacing of the styrene sulfonate ions is increased, the filler is not easy to agglomerate, and then the first product and the third product are mixed according to the weight ratio of 0.3-0.5: 1 to prepare the anticorrosive filler.
Further, in step S11, the weight ratio of the clove essential oil to the 10% ethanol aqueous solution is controlled to be 1: 10-15, the weight ratio of the mixed solution a to the 50% beta-cyclodextrin aqueous solution is controlled to be 1: 5-8, and the weight ratio of the magnesium nitrate, the aluminum nitrate and the sodium hydroxide is controlled to be 2: 1 in step S12.
The invention has the beneficial effects that:
(1) the invention relates to a high-temperature-resistant water-based heat-conducting anticorrosive coating which is prepared from modified carbon nano-particles, anticorrosive fillers, water-based fluorocarbon resin and other raw materials, wherein in the preparation process of the modified carbon nano-particles, in step S1, a carbon nano-tube is firstly added into a three-neck flask filled with concentrated sulfuric acid and concentrated nitric acid, the catalyst and amorphous carbon impurities remained in the preparation process of the carbon nano-tube are removed under the washing of strong acid of the concentrated sulfuric acid and the concentrated nitric acid, the carbon nano-tube has small specific surface area and is easy to agglomerate, active groups such as carboxyl and the like can be introduced on the carbon nano-tube in the acid washing process to improve the dispersing performance of the carbon nano-tube, so as to prepare the nano-fillers which can be uniformly dispersed in deionized water, in step S2, the nano-fillers are added into the deionized water to prepare a suspension B, the carbon nano-tube is modified, the dispersion performance of the carbon nano-tube in a solvent is further enhanced, and the prepared modified carbon nano-particles can be stacked and lapped with the matrix macromolecular chain segment, so that the density is increased, and the heat-conducting property of the prepared coating is further improved.
(2) The invention also prepares an anti-corrosion filler, and the clove essential oil is a natural bacteriostatic agent in the preparation process, but the clove essential oil has pungent smell, and the coating prepared by using the clove essential oil as an antibacterial agent has pungent smell, so that a beta-cyclodextrin water solution is prepared in step S11, then the clove essential oil is dissolved in an ethanol water solution, and then a microcapsule-shaped intermediate with the beta-cyclodextrin as a wall material and the clove essential oil as a core material is prepared by mixing; in the step S12, a second product is prepared from raw materials such as magnesium nitrate and aluminum nitrate, the second product has active groups such as hydroxyl groups and the like, the surface energy is large, the surface structure of the second product is unstable, hydrogen bonds are easy to generate to form agglomeration, the second product is an inorganic material, the compatibility is poor when the second product is mixed with a matrix material, and the second product cannot be uniformly dispersed in the matrix, so that S13 modifies the second product through sodium styrene sulfonate to organize the surface of the second product, the surface is passivated, the agglomeration phenomenon can be prevented, styrene sulfonate ions can enter between filler layers in the modification process, the interlayer spacing of the styrene sulfonate ions is increased, the filler is not easy to agglomerate, and then the first product and the third product are mixed according to the weight ratio of 0.3-0.5: 1 to prepare the anticorrosive filler.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
A preparation method of a high-temperature-resistant water-based heat-conducting anticorrosive coating comprises the following steps:
firstly, weighing the following raw materials in parts by weight: 15 parts of modified carbon nanoparticles, 5 parts of anticorrosive filler, 75 parts of waterborne fluorocarbon resin, 3 parts of dimethyl siloxane, 3 parts of vinyl triamine and 150 parts of deionized water;
and secondly, adding the modified carbon nano particles into deionized water, carrying out ultrasonic oscillation, stirring for 15min at the rotating speed of 180r/min to prepare a suspension, sequentially adding the suspension, the aqueous fluorocarbon resin, the dimethyl siloxane and the vinyl triamine into a ball mill, and carrying out ball milling for 2h at the rotating speed of 480r/min to prepare the high-temperature-resistant aqueous heat-conducting anticorrosive coating.
The modified carbon nanoparticles are prepared by the following method:
step S1, adding carbon nanotubes into a three-neck flask filled with concentrated sulfuric acid and concentrated nitric acid, controlling the weight ratio of the concentrated sulfuric acid to the concentrated nitric acid to be 3: 1, uniformly stirring at a rotating speed of 100r/min for 15min, then placing the mixture into a water bath kettle at 80 ℃, stirring at the temperature for 30min, cooling to 30 ℃ after stirring, standing for 1h to prepare a suspension A, pouring the suspension A into a beaker filled with deionized water, standing for 1h, performing suction filtration, washing a filter cake with the deionized water until the filtrate is neutral to prepare the nano filler, controlling the using amount ratio of the carbon nanotubes to the concentrated sulfuric acid to be 2 g: 120mL, controlling the mass fraction of the concentrated sulfuric acid to be 75%, and controlling the mass fraction of the concentrated nitric acid to be 70%;
and S2, adding the nano filler prepared in the step S1 into deionized water, uniformly stirring at a speed of 240r/min and ultrasonically dispersing for 30min to prepare a suspension B, controlling the ultrasonic power to be 50W, adding sodium tripolyphosphate into the suspension B, continuously stirring for 30min, then dropwise adding a polyvinyl alcohol aqueous solution with the mass fraction of 4%, controlling the dropwise adding time to be 15min, heating in a water bath at 60 ℃, irradiating by using an infrared lamp until the mixture is completely dried, and grinding to prepare the modified carbon nano particles, wherein the weight ratio of the nano filler to the deionized water is controlled to be 1: 50, and the weight ratio of the nano filler to the sodium tripolyphosphate to the polyvinyl alcohol aqueous solution with the mass fraction of 4% is 1: 0.1: 3.
The anti-corrosion filler is prepared by the following method:
step S11, adding beta-cyclodextrin into deionized water, stirring at a constant speed until the beta-cyclodextrin is completely dissolved, preparing a beta-cyclodextrin aqueous solution with the mass fraction of 50%, adding clove essential oil into an ethanol aqueous solution with the volume fraction of 10%, stirring at a constant speed for 15min to prepare a mixed solution a, dropwise adding the mixed solution a into the beta-cyclodextrin aqueous solution with the mass fraction of 50%, controlling the dropwise adding time to be 30min, heating in a 45 ℃ water bath, magnetically stirring for 30min, standing at 2 ℃ after stirring for 20h, performing suction filtration, washing a filter cake with absolute ethyl alcohol and deionized water for three times respectively, drying at 50 ℃ to constant weight to prepare a first product, controlling the weight ratio of the clove essential oil to the 10% ethanol aqueous solution to be 1: 10, and controlling the weight ratio of the mixed solution a to the 50% beta-cyclodextrin aqueous solution to be 1: 5;
step S12, adding magnesium nitrate and aluminum nitrate into a beaker filled with deionized water, uniformly stirring, adding sodium hydroxide, heating in a water bath at 35 ℃ and magnetically stirring, then transferring into a three-neck flask, introducing nitrogen gas during the adding process, stirring at a rotating speed of 400r/min, completely adding, crystallizing at 70 ℃ for 20 hours, performing suction filtration, washing with deionized water at 45 ℃ for three times, and performing vacuum drying at 100 ℃ for 4 hours to obtain a second product, wherein the weight ratio of the magnesium nitrate to the aluminum nitrate to the sodium hydroxide is controlled to be 2: 1;
and step S13, adding sodium p-styrene sulfonate into deionized water, stirring at a constant speed for 10min, adding a second product, controlling the weight ratio of the sodium p-styrene sulfonate to the second product to be 1: 15, heating in a water bath at 35 ℃, stirring at a constant speed for 2h, filtering, washing with deionized water three times, drying at 70 ℃ for 40h to obtain a third product, and mixing the first product and the third product according to the weight ratio of 0.3: 1 to obtain the anticorrosive filler.
Example 2
A preparation method of a high-temperature-resistant water-based heat-conducting anticorrosive coating comprises the following steps:
firstly, weighing the following raw materials in parts by weight: 20 parts of modified carbon nanoparticles, 6 parts of anticorrosive filler, 80 parts of waterborne fluorocarbon resin, 5 parts of dimethyl siloxane, 4 parts of vinyl triamine and 160 parts of deionized water;
and secondly, adding the modified carbon nano particles into deionized water, carrying out ultrasonic oscillation, stirring for 15min at the rotating speed of 180r/min to prepare a suspension, sequentially adding the suspension, the aqueous fluorocarbon resin, the dimethyl siloxane and the vinyl triamine into a ball mill, and carrying out ball milling for 2h at the rotating speed of 480r/min to prepare the high-temperature-resistant aqueous heat-conducting anticorrosive coating.
The modified carbon nanoparticles are prepared by the following method:
step S1, adding carbon nanotubes into a three-neck flask filled with concentrated sulfuric acid and concentrated nitric acid, controlling the weight ratio of the concentrated sulfuric acid to the concentrated nitric acid to be 3: 1, uniformly stirring at a rotating speed of 100r/min for 15min, then placing the mixture into a water bath kettle at 80 ℃, stirring at the temperature for 30min, cooling to 30 ℃ after stirring, standing for 1h to prepare a suspension A, pouring the suspension A into a beaker filled with deionized water, standing for 1h, performing suction filtration, washing a filter cake with the deionized water until the filtrate is neutral to prepare the nano filler, controlling the using amount ratio of the carbon nanotubes to the concentrated sulfuric acid to be 2 g: 120mL, controlling the mass fraction of the concentrated sulfuric acid to be 75%, and controlling the mass fraction of the concentrated nitric acid to be 70%;
and S2, adding the nano filler prepared in the step S1 into deionized water, uniformly stirring at a speed of 240r/min and ultrasonically dispersing for 30min to prepare a suspension B, controlling the ultrasonic power to be 50W, adding sodium tripolyphosphate into the suspension B, continuously stirring for 30min, then dropwise adding a polyvinyl alcohol aqueous solution with the mass fraction of 4%, controlling the dropwise adding time to be 15min, heating in a water bath at 60 ℃, irradiating by using an infrared lamp until the mixture is completely dried, and grinding to prepare the modified carbon nano particles, wherein the weight ratio of the nano filler to the deionized water is controlled to be 1: 50, and the weight ratio of the nano filler to the sodium tripolyphosphate to the polyvinyl alcohol aqueous solution with the mass fraction of 4% is 1: 0.1: 3.
The anti-corrosion filler is prepared by the following method:
step S11, adding beta-cyclodextrin into deionized water, stirring at a constant speed until the beta-cyclodextrin is completely dissolved, preparing a beta-cyclodextrin aqueous solution with the mass fraction of 50%, adding clove essential oil into an ethanol aqueous solution with the volume fraction of 10%, stirring at a constant speed for 15min to prepare a mixed solution a, dropwise adding the mixed solution a into the beta-cyclodextrin aqueous solution with the mass fraction of 50%, controlling the dropwise adding time to be 30min, heating in a 45 ℃ water bath, magnetically stirring for 30min, standing at 2 ℃ after stirring for 20h, performing suction filtration, washing a filter cake with absolute ethyl alcohol and deionized water for three times respectively, drying at 50 ℃ to constant weight to prepare a first product, controlling the weight ratio of the clove essential oil to the 10% ethanol aqueous solution to be 1: 10, and controlling the weight ratio of the mixed solution a to the 50% beta-cyclodextrin aqueous solution to be 1: 5;
step S12, adding magnesium nitrate and aluminum nitrate into a beaker filled with deionized water, uniformly stirring, adding sodium hydroxide, heating in a water bath at 35 ℃ and magnetically stirring, then transferring into a three-neck flask, introducing nitrogen gas during the adding process, stirring at a rotating speed of 400r/min, completely adding, crystallizing at 70 ℃ for 20 hours, performing suction filtration, washing with deionized water at 45 ℃ for three times, and performing vacuum drying at 100 ℃ for 4 hours to obtain a second product, wherein the weight ratio of the magnesium nitrate to the aluminum nitrate to the sodium hydroxide is controlled to be 2: 1;
and step S13, adding sodium p-styrene sulfonate into deionized water, stirring at a constant speed for 10min, adding a second product, controlling the weight ratio of the sodium p-styrene sulfonate to the second product to be 1: 15, heating in a water bath at 35 ℃, stirring at a constant speed for 2h, filtering, washing with deionized water three times, drying at 70 ℃ for 40h to obtain a third product, and mixing the first product and the third product according to the weight ratio of 0.3: 1 to obtain the anticorrosive filler.
Example 3
A preparation method of a high-temperature-resistant water-based heat-conducting anticorrosive coating comprises the following steps:
firstly, weighing the following raw materials in parts by weight: 30 parts of modified carbon nanoparticles, 8 parts of anticorrosive filler, 85 parts of waterborne fluorocarbon resin, 6 parts of dimethyl siloxane, 4 parts of vinyl triamine and 180 parts of deionized water;
and secondly, adding the modified carbon nano particles into deionized water, carrying out ultrasonic oscillation, stirring for 15min at the rotating speed of 180r/min to prepare a suspension, sequentially adding the suspension, the aqueous fluorocarbon resin, the dimethyl siloxane and the vinyl triamine into a ball mill, and carrying out ball milling for 2h at the rotating speed of 480r/min to prepare the high-temperature-resistant aqueous heat-conducting anticorrosive coating.
The modified carbon nanoparticles are prepared by the following method:
step S1, adding carbon nanotubes into a three-neck flask filled with concentrated sulfuric acid and concentrated nitric acid, controlling the weight ratio of the concentrated sulfuric acid to the concentrated nitric acid to be 3: 1, uniformly stirring at a rotating speed of 100r/min for 15min, then placing the mixture into a water bath kettle at 80 ℃, stirring at the temperature for 30min, cooling to 30 ℃ after stirring, standing for 1h to prepare a suspension A, pouring the suspension A into a beaker filled with deionized water, standing for 1h, performing suction filtration, washing a filter cake with the deionized water until the filtrate is neutral to prepare the nano filler, controlling the using amount ratio of the carbon nanotubes to the concentrated sulfuric acid to be 2 g: 120mL, controlling the mass fraction of the concentrated sulfuric acid to be 75%, and controlling the mass fraction of the concentrated nitric acid to be 70%;
and S2, adding the nano filler prepared in the step S1 into deionized water, uniformly stirring at a speed of 240r/min and ultrasonically dispersing for 30min to prepare a suspension B, controlling the ultrasonic power to be 50W, adding sodium tripolyphosphate into the suspension B, continuously stirring for 30min, then dropwise adding a polyvinyl alcohol aqueous solution with the mass fraction of 4%, controlling the dropwise adding time to be 15min, heating in a water bath at 60 ℃, irradiating by using an infrared lamp until the mixture is completely dried, and grinding to prepare the modified carbon nano particles, wherein the weight ratio of the nano filler to the deionized water is controlled to be 1: 50, and the weight ratio of the nano filler to the sodium tripolyphosphate to the polyvinyl alcohol aqueous solution with the mass fraction of 4% is 1: 0.1: 3.
The anti-corrosion filler is prepared by the following method:
step S11, adding beta-cyclodextrin into deionized water, stirring at a constant speed until the beta-cyclodextrin is completely dissolved, preparing a beta-cyclodextrin aqueous solution with the mass fraction of 50%, adding clove essential oil into an ethanol aqueous solution with the volume fraction of 10%, stirring at a constant speed for 15min to prepare a mixed solution a, dropwise adding the mixed solution a into the beta-cyclodextrin aqueous solution with the mass fraction of 50%, controlling the dropwise adding time to be 30min, heating in a 45 ℃ water bath, magnetically stirring for 30min, standing at 2 ℃ after stirring for 20h, performing suction filtration, washing a filter cake with absolute ethyl alcohol and deionized water for three times respectively, drying at 50 ℃ to constant weight to prepare a first product, controlling the weight ratio of the clove essential oil to the 10% ethanol aqueous solution to be 1: 10, and controlling the weight ratio of the mixed solution a to the 50% beta-cyclodextrin aqueous solution to be 1: 5;
step S12, adding magnesium nitrate and aluminum nitrate into a beaker filled with deionized water, uniformly stirring, adding sodium hydroxide, heating in a water bath at 35 ℃ and magnetically stirring, then transferring into a three-neck flask, introducing nitrogen gas during the adding process, stirring at a rotating speed of 400r/min, completely adding, crystallizing at 70 ℃ for 20 hours, performing suction filtration, washing with deionized water at 45 ℃ for three times, and performing vacuum drying at 100 ℃ for 4 hours to obtain a second product, wherein the weight ratio of the magnesium nitrate to the aluminum nitrate to the sodium hydroxide is controlled to be 2: 1;
and step S13, adding sodium p-styrene sulfonate into deionized water, stirring at a constant speed for 10min, adding a second product, controlling the weight ratio of the sodium p-styrene sulfonate to the second product to be 1: 15, heating in a water bath at 35 ℃, stirring at a constant speed for 2h, filtering, washing with deionized water three times, drying at 70 ℃ for 40h to obtain a third product, and mixing the first product and the third product according to the weight ratio of 0.3: 1 to obtain the anticorrosive filler.
Example 4
A preparation method of a high-temperature-resistant water-based heat-conducting anticorrosive coating comprises the following steps:
firstly, weighing the following raw materials in parts by weight: 35 parts of modified carbon nanoparticles, 10 parts of anticorrosive filler, 90 parts of waterborne fluorocarbon resin, 8 parts of dimethyl siloxane, 5 parts of vinyl triamine and 200 parts of deionized water;
and secondly, adding the modified carbon nano particles into deionized water, carrying out ultrasonic oscillation, stirring for 15min at the rotating speed of 180r/min to prepare a suspension, sequentially adding the suspension, the aqueous fluorocarbon resin, the dimethyl siloxane and the vinyl triamine into a ball mill, and carrying out ball milling for 2h at the rotating speed of 480r/min to prepare the high-temperature-resistant aqueous heat-conducting anticorrosive coating.
The modified carbon nanoparticles are prepared by the following method:
step S1, adding carbon nanotubes into a three-neck flask filled with concentrated sulfuric acid and concentrated nitric acid, controlling the weight ratio of the concentrated sulfuric acid to the concentrated nitric acid to be 3: 1, uniformly stirring at a rotating speed of 100r/min for 15min, then placing the mixture into a water bath kettle at 80 ℃, stirring at the temperature for 30min, cooling to 30 ℃ after stirring, standing for 1h to prepare a suspension A, pouring the suspension A into a beaker filled with deionized water, standing for 1h, performing suction filtration, washing a filter cake with the deionized water until the filtrate is neutral to prepare the nano filler, controlling the using amount ratio of the carbon nanotubes to the concentrated sulfuric acid to be 2 g: 120mL, controlling the mass fraction of the concentrated sulfuric acid to be 75%, and controlling the mass fraction of the concentrated nitric acid to be 70%;
and S2, adding the nano filler prepared in the step S1 into deionized water, uniformly stirring at a speed of 240r/min and ultrasonically dispersing for 30min to prepare a suspension B, controlling the ultrasonic power to be 50W, adding sodium tripolyphosphate into the suspension B, continuously stirring for 30min, then dropwise adding a polyvinyl alcohol aqueous solution with the mass fraction of 4%, controlling the dropwise adding time to be 15min, heating in a water bath at 60 ℃, irradiating by using an infrared lamp until the mixture is completely dried, and grinding to prepare the modified carbon nano particles, wherein the weight ratio of the nano filler to the deionized water is controlled to be 1: 50, and the weight ratio of the nano filler to the sodium tripolyphosphate to the polyvinyl alcohol aqueous solution with the mass fraction of 4% is 1: 0.1: 3.
The anti-corrosion filler is prepared by the following method:
step S11, adding beta-cyclodextrin into deionized water, stirring at a constant speed until the beta-cyclodextrin is completely dissolved, preparing a beta-cyclodextrin aqueous solution with the mass fraction of 50%, adding clove essential oil into an ethanol aqueous solution with the volume fraction of 10%, stirring at a constant speed for 15min to prepare a mixed solution a, dropwise adding the mixed solution a into the beta-cyclodextrin aqueous solution with the mass fraction of 50%, controlling the dropwise adding time to be 30min, heating in a 45 ℃ water bath, magnetically stirring for 30min, standing at 2 ℃ after stirring for 20h, performing suction filtration, washing a filter cake with absolute ethyl alcohol and deionized water for three times respectively, drying at 50 ℃ to constant weight to prepare a first product, controlling the weight ratio of the clove essential oil to the 10% ethanol aqueous solution to be 1: 10, and controlling the weight ratio of the mixed solution a to the 50% beta-cyclodextrin aqueous solution to be 1: 5;
step S12, adding magnesium nitrate and aluminum nitrate into a beaker filled with deionized water, uniformly stirring, adding sodium hydroxide, heating in a water bath at 35 ℃ and magnetically stirring, then transferring into a three-neck flask, introducing nitrogen gas during the adding process, stirring at a rotating speed of 400r/min, completely adding, crystallizing at 70 ℃ for 20 hours, performing suction filtration, washing with deionized water at 45 ℃ for three times, and performing vacuum drying at 100 ℃ for 4 hours to obtain a second product, wherein the weight ratio of the magnesium nitrate to the aluminum nitrate to the sodium hydroxide is controlled to be 2: 1;
and step S13, adding sodium p-styrene sulfonate into deionized water, stirring at a constant speed for 10min, adding a second product, controlling the weight ratio of the sodium p-styrene sulfonate to the second product to be 1: 15, heating in a water bath at 35 ℃, stirring at a constant speed for 2h, filtering, washing with deionized water three times, drying at 70 ℃ for 40h to obtain a third product, and mixing the first product and the third product according to the weight ratio of 0.3: 1 to obtain the anticorrosive filler.
Comparative example 1
This comparative example compares to example 1 with carbon nanotubes instead of modified carbon nanoparticles.
Comparative example 2
In comparison with example 1, no corrosion inhibiting filler was added in this comparative example.
Comparative example 3
The comparative example is a high-temperature-resistant water-based heat-conducting anticorrosive coating in the market.
The corrosion preventing properties and the heat conducting properties of examples 1 to 4 and comparative examples 1 to 3 were measured, and the results are shown in the following table:
as can be seen from the table above, the bacteriostatic rates of the examples 1-4 for Escherichia coli are 99.7-99.9%, the bacteriostatic rate for Staphylococcus aureus is 99.5-99.8%, the thermal conductivities are excellent, the bacteriostatic rates of the comparative examples 1-3 for Escherichia coli are 33.2-98.3%, the bacteriostatic rate for Staphylococcus aureus is 34.8-98.1%, and the thermal conductivities are good; therefore, in step S2, the nanofiller is added to deionized water to prepare a suspension B, sodium tripolyphosphate is added as a dispersant, and a 4% by mass aqueous solution of polyvinyl alcohol is added as a thickener to modify the carbon nanotubes, thereby further enhancing the dispersibility of the carbon nanotubes in the solvent.
In the description herein, references to the description of "one embodiment," "an example," "a specific example" or the like are intended to mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The foregoing is illustrative and explanatory only and is not intended to be exhaustive or to limit the invention to the precise embodiments described, and various modifications, additions, and substitutions may be made by those skilled in the art without departing from the scope of the invention or exceeding the scope of the claims.
Claims (6)
1. The preparation method of the high-temperature-resistant water-based heat-conducting anticorrosive paint is characterized by comprising the following steps of:
firstly, weighing the following raw materials in parts by weight: 15-35 parts of modified carbon nano particles, 5-10 parts of anticorrosive filler, 75-90 parts of waterborne fluorocarbon resin, 3-8 parts of defoaming agent, 3-5 parts of curing agent and 150 parts of deionized water;
and secondly, adding the modified carbon nano particles into deionized water, carrying out ultrasonic oscillation and stirring for 15min at the rotating speed of 180-.
2. The method for preparing a high temperature resistant water-based heat-conducting anticorrosive coating according to claim 1, wherein the defoaming agent is one or two of trialkyl melamine and dimethyl siloxane, and the curing agent is one or two of vinyl triamine and m-phenylenediamine, and the mixture ratio is arbitrary.
3. The preparation method of the high-temperature-resistant water-based heat-conducting anticorrosive coating according to claim 1, wherein the modified carbon nanoparticles are prepared by the following method:
step S1, adding carbon nanotubes into a three-neck flask filled with concentrated sulfuric acid and concentrated nitric acid, controlling the weight ratio of the concentrated sulfuric acid to the concentrated nitric acid to be 3: 1, uniformly stirring at a rotation speed of 100-120r/min for 15min, then placing the mixture into a water bath kettle at 80-90 ℃, stirring at the temperature for 30min, cooling to 30-35 ℃ after stirring, standing for 1h to prepare a suspension A, pouring the suspension A into a beaker filled with deionized water, standing for 1h, performing suction filtration, and washing a filter cake with the deionized water until the filtrate is neutral to prepare the nanofiller;
and S2, adding the nano filler prepared in the step S1 into deionized water, uniformly stirring at a speed of 240 plus 280r/min and ultrasonically dispersing for 30min to prepare a suspension B, controlling the ultrasonic power to be 50-60W, adding sodium tripolyphosphate into the suspension B, continuously stirring for 30min, dropwise adding a polyvinyl alcohol aqueous solution with the mass fraction of 4%, controlling the dropwise adding time to be 15min, heating in a water bath at 60-65 ℃, irradiating by using an infrared lamp until the solution is completely dried, and grinding to prepare the modified carbon nano particles.
4. The preparation method of the high temperature resistant water-based heat-conducting anticorrosive coating as claimed in claim 3, wherein the amount ratio of the carbon nanotubes to the concentrated sulfuric acid is controlled to be 2-3 g: 120-150mL in the step S1, the mass fraction of the concentrated sulfuric acid is 75%, the mass fraction of the concentrated nitric acid is 70%, the weight ratio of the nanofiller to the deionized water is controlled to be 1: 50 in the step S2, and the weight ratio of the nanofiller, the sodium tripolyphosphate and the 4% polyvinyl alcohol aqueous solution is 1: 0.1-0.3: 3-5.
5. The preparation method of the high-temperature-resistant water-based heat-conducting anticorrosive coating according to claim 1, characterized in that the anticorrosive filler is prepared by the following method:
step S11, adding beta-cyclodextrin into deionized water, stirring at a constant speed until the beta-cyclodextrin is completely dissolved, preparing a beta-cyclodextrin aqueous solution with the mass fraction of 50%, adding clove essential oil into an ethanol aqueous solution with the volume fraction of 10%, stirring at a constant speed for 15min to prepare a mixed solution a, dropwise adding the mixed solution a into the beta-cyclodextrin aqueous solution with the mass fraction of 50%, controlling the dropwise adding time to be 30min, heating in a water bath at 45-50 ℃ and stirring magnetically for 30min, refrigerating and standing at 2-5 ℃ after stirring for 20h, performing suction filtration, washing a filter cake with absolute ethyl alcohol and deionized water for three times respectively, and then drying at 50-60 ℃ to constant weight to prepare a first product;
step S12, adding magnesium nitrate and aluminum nitrate into a beaker filled with deionized water, uniformly stirring, adding sodium hydroxide, heating in a water bath at 35-40 ℃ and magnetically stirring, then transferring into a three-neck flask, introducing nitrogen gas during the adding process, stirring at a rotating speed of 400r/min, completely adding, crystallizing at 70 ℃ for 20 hours, performing suction filtration, washing with deionized water at 45 ℃ for three times, and performing vacuum drying at 100 ℃ for 4 hours to obtain a second product;
step S13, adding sodium p-styrene sulfonate into deionized water, stirring at a constant speed for 10min, adding a second product, controlling the weight ratio of the sodium p-styrene sulfonate to the second product to be 1: 15, heating in a water bath at 35-40 ℃, stirring at a constant speed for 2h, filtering, washing with deionized water three times, drying at 70 ℃ for 40h to obtain a third product, and mixing the first product and the third product according to the weight ratio of 0.3-0.5: 1 to obtain the anticorrosive filler.
6. The preparation method of the high temperature resistant water-based heat-conducting anticorrosive coating as claimed in claim 5, wherein the weight ratio of the clove essential oil to the 10% ethanol aqueous solution is controlled to be 1: 10-15 in step S11, the weight ratio of the mixed solution a to the 50% β -cyclodextrin aqueous solution is 1: 5-8, and the weight ratio of the magnesium nitrate, the aluminum nitrate and the sodium hydroxide is controlled to be 2: 1 in step S12.
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