CN111253782A - Modified anticorrosive hydrotalcite, water-based intelligent anticorrosive paint, preparation method and coating - Google Patents
Modified anticorrosive hydrotalcite, water-based intelligent anticorrosive paint, preparation method and coating Download PDFInfo
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Abstract
The invention discloses modified anticorrosive hydrotalcite, a water-based intelligent anticorrosive coating, a preparation method and a coating, wherein the preparation method of the modified anticorrosive hydrotalcite comprises the following steps: dripping a mixed solution of a metal nitrate solution, sodium hydroxide and sodium tripolyphosphate into deionized water, stirring and centrifuging to obtain anticorrosive hydrotalcite; and adding the anticorrosive hydrotalcite and dopamine into a buffer solution, stirring and centrifuging to obtain the modified anticorrosive hydrotalcite. According to the invention, the corrosion resistance is improved by utilizing the capability of the tripolyphosphate ions to passivate metal to form a protective film and the lamellar blocking effect of the hydrotalcite, the coating made of the modified corrosion-resistant hydrotalcite is coated on the surface of steel, and when the steel is corroded to generate metal cations, the catechol group on the dopamine and the metal cations can form a cross-linked network structure, so that the coating is adsorbed on the surface of a steel matrix, and the effects of automatic protection and intelligent corrosion prevention are achieved.
Description
Technical Field
The invention relates to modified anticorrosive hydrotalcite, a water-based intelligent anticorrosive coating, a preparation method and a coating, and belongs to the technical field of coating preparation.
Background
Metal materials are widely used in many fields such as automobile production, ship manufacturing, electric wires, and building construction because of their good ductility, electrical conductivity, and mechanical properties. Among them, steel is a basic structural material, known as "industrial skeleton", and it is seen that steel materials are incomparable in industry. However, since the corrosion of steel materials rapidly degrades the properties of steel materials in all respects, corrosion prevention work of steel materials is essential.
In the aspect of corrosion protection, a method for changing the structure or components in the metal, an electrochemical protection method, a corrosion inhibitor adding method, an anticorrosive paint covering protection method and the like are adopted, wherein the anticorrosive paint covering protection method has the lowest cost and the highest efficiency. Most of the traditional anticorrosive coatings are organic solvent type, and volatile organic solvents can pollute air. Thus, water-borne coatings tend to dominate the future coating market.
Compared with organic solvent-based coatings, the water-based coatings are more environment-friendly, but the corrosion resistance of the coatings is deteriorated after the water-based coatings are water-based, and at present, in order to solve the problem, some corrosion-resistant materials are often added to be filled in the coatings to increase the corrosion resistance of the coatings. However, most of the traditional anticorrosive fillers are inorganic substances, so that the traditional anticorrosive fillers are difficult to achieve a good dispersion effect in the coating after water-based coating, cannot effectively cover the surface of a steel substrate, and do not greatly improve the anticorrosive capacity of the water-based coating. Therefore, a new utilization approach is needed to improve the corrosion resistance of the water-based paint.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides modified anticorrosive hydrotalcite, a water-based intelligent anticorrosive paint, a preparation method and a coating, and aims to solve the technical problem of poor anticorrosive capability of the water-based paint in the prior art.
In order to achieve the above purpose, an embodiment of the present invention provides a modified anticorrosive hydrotalcite, which is prepared from the following raw materials in parts by weight: 20-40 parts of anticorrosive hydrotalcite, 5-10 parts of dopamine and 30-60 parts of tris-HCl buffer solution with the pH value of 8-9.
In order to achieve the above object, an embodiment of the present invention further provides a preparation method of a modified anticorrosive hydrotalcite, where the preparation method of the modified anticorrosive hydrotalcite includes:
dripping a mixed solution of a metal nitrate solution, sodium hydroxide and sodium tripolyphosphate into deionized water, stirring and centrifuging to obtain anticorrosive hydrotalcite;
and adding the anticorrosive hydrotalcite and dopamine into a trihydroxymethyl aminomethane buffer solution, stirring and centrifuging to obtain the modified anticorrosive hydrotalcite.
Preferably, the modified anticorrosive hydrotalcite is obtained by adding the anticorrosive hydrotalcite and dopamine into a tris buffer solution, stirring and centrifuging the mixture, and specifically comprises the following steps:
weighing 20-40 parts of the anticorrosive hydrotalcite and 5-10 parts of dopamine, adding the anticorrosive hydrotalcite and the dopamine into 30-60 parts of tris (hydroxymethyl) aminomethane buffer solution with the pH value of 8-9, and mechanically stirring for 12-24 hours at the stirring speed of 500-1000 rpm to obtain a first stirring product;
and weighing 500 parts of 300-2000 parts of water to centrifuge and wash the first stirring product, wherein the centrifugation time is 3-5 times, and the centrifugation speed is 1000-2000 rpm, so as to obtain the modified anticorrosive hydrotalcite.
Preferably, the method comprises the following steps of dropping a mixed solution of a metal nitrate solution, sodium hydroxide and sodium tripolyphosphate into deionized water, stirring and centrifuging to obtain the anticorrosive hydrotalcite, and specifically comprises the following steps:
dissolving magnesium nitrate hexahydrate and aluminum nitrate nonahydrate in deionized water to obtain a metal nitrate solution;
dissolving sodium hydroxide and sodium tripolyphosphate in deionized water to obtain a mixed solution of the sodium hydroxide and the sodium tripolyphosphate;
dripping the metal nitrate solution and the mixed solution of sodium hydroxide and sodium tripolyphosphate into deionized water to obtain an alkaline mixture;
and sequentially stirring, crystallizing, centrifuging, washing and drying the alkaline mixture to obtain the anticorrosive hydrotalcite.
Preferably, before dissolving magnesium nitrate hexahydrate and aluminum nitrate nonahydrate in deionized water to obtain a metal nitrate solution, the method further comprises:
the deionized water was boiled and cooled to 25-30 ℃.
In order to achieve the above purpose, an embodiment of the present invention further provides a water-based intelligent anticorrosive paint, which is prepared from the following raw materials in parts by weight: 1 part of curing agent solution and 3-4 parts of aqueous anticorrosive paint mother liquor.
In order to achieve the above object, an embodiment of the present invention further provides a preparation method of the water-based intelligent anticorrosive paint, where the preparation method of the water-based intelligent anticorrosive paint includes:
adding the modified anticorrosive hydrotalcite into a water-based epoxy resin solution, stirring and vibrating to obtain a water-based anticorrosive paint mother solution;
and mixing the aqueous anticorrosive paint mother liquor with a curing agent to obtain the aqueous intelligent anticorrosive paint.
Preferably, the modified anticorrosive hydrotalcite is added into a water-based epoxy resin solution to be stirred and vibrated, so as to obtain a water-based anticorrosive paint mother liquor, and the method specifically comprises the following steps:
mixing 100-120 parts of deionized water and 150-200 parts of aqueous epoxy resin according to the parts by weight to obtain an aqueous epoxy resin solution;
weighing 10-20 parts of modified anticorrosive hydrotalcite, adding the modified anticorrosive hydrotalcite into the aqueous epoxy resin solution, and performing electromagnetic stirring for 10-30 minutes at a stirring speed of 50-100 rpm to obtain a second stirring product;
and vibrating the second stirring product by an ultrasonic oscillator for 10-30 minutes at a vibration power of 40-50 watts to obtain the mother solution of the water-based anticorrosive paint.
Preferably, the aqueous intelligent anticorrosive coating is obtained by mixing the aqueous anticorrosive coating mother liquor and a curing agent, and specifically comprises:
weighing 30-50 parts by weight of curing agent and 50-80 parts by weight of deionized water, mechanically stirring for 10-20 minutes at a stirring speed of 100 and 200 revolutions per minute, and obtaining a curing agent solution after stirring;
and (3) mixing the curing agent solution with the aqueous anticorrosive paint mother liquor according to the proportion of 1 (3-4) to obtain the aqueous intelligent anticorrosive paint.
In order to achieve the above purpose, the embodiment of the present invention further provides an anticorrosion coating, which is obtained by coating and curing the above water-based intelligent anticorrosion coating.
Compared with the prior art, the method has the following advantages:
according to the invention, the anticorrosion capability is improved by utilizing the capability of passivating metal to form a protective film by tripolyphosphate ions and the sheet layer blocking effect of the hydrotalcite insertion layer material, and the anticorrosion hydrotalcite can be better distributed in the coating by utilizing the polyhydroxy structure of polydopamine, so that the dispersibility of the anticorrosion hydrotalcite is improved. And when steel is corroded to generate metal cations and corrosion anions, catechol groups on the polydopamine and the metal cations can form a cross-linked network structure, so that the modified anticorrosive hydrotalcite is adsorbed on the surface of the steel matrix to achieve the effects of automatic protection and intelligent corrosion prevention, and the corrosion anions can be replaced between layers to weaken the cathode reaction of the corrosion reaction, thereby achieving the double corrosion prevention effect and avoiding the metal matrix from being further corroded.
Drawings
In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the drawings needed to be used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without creative efforts.
FIG. 1 is a schematic flow chart of a preparation method of modified anticorrosive hydrotalcite according to the present invention;
FIG. 2 is a schematic flow chart of a preparation method of the water-based intelligent anticorrosive paint;
FIG. 3 is a corrosion prevention schematic diagram of a preparation method of the water-based intelligent anticorrosive paint;
FIG. 4 is a graph of the AC impedance of various coatings of the present invention after 800 hours of salt spray testing.
Detailed Description
The present invention will be described in detail below with reference to specific embodiments and examples, and the advantages and various effects of the present invention will be more clearly apparent therefrom. It will be understood by those skilled in the art that these specific embodiments and examples are for the purpose of illustrating the invention and are not to be construed as limiting the invention.
Throughout the specification, unless otherwise specifically noted, terms used herein should be understood as having meanings as commonly used in the art. Accordingly, unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. If there is a conflict, the present specification will control.
Unless otherwise specifically stated, various raw materials, reagents, instruments, equipment and the like used in the present invention are commercially available or can be prepared by existing methods.
The embodiment of the invention provides modified anticorrosive hydrotalcite which is prepared from the following raw materials in parts by weight: 20-40 parts of anticorrosive hydrotalcite, 5-10 parts of dopamine and 30-60 parts of tris-HCl buffer solution with the pH value of 8-9. The polydopamine is grown on the surface of the anticorrosive hydrotalcite, and the polyhydroxy structure of the polydopamine is utilized to enable the anticorrosive hydrotalcite to be better distributed in the coating, so that the modified anticorrosive hydrotalcite is obtained, and the dispersibility of the anticorrosive hydrotalcite is improved.
Referring to fig. 1, an embodiment of the present invention provides a method for preparing modified anticorrosive hydrotalcite, specifically including:
step S10: and (3) dripping the mixed solution of the metal nitrate solution, the sodium hydroxide and the sodium tripolyphosphate into deionized water, stirring and centrifuging to obtain the anticorrosive hydrotalcite.
Layered Double Hydroxide (L)DH) is a generic name for Hydrotalcite (HT) and Hydrotalcite-Like Compounds (HTLCs), and a series of supramolecular materials intercalated and assembled from these Compounds are called Hydrotalcite-Like intercalation materials (LDHs). The LDHs have unique layered structure, are excellent anion exchange materials consisting of mixed metal hydroxide layers with positive and negative charges, and have higher metal dispersibility. LDHs, particularly heat-activated LDHs, are excellent corrosion protection materials because their positively charged layered structure is very susceptible to intercalation of different anions, such as Sulfate (SO)4 2-) Chlorine ion (CL)-) And the like, common corrosion anions. And the layered structure of the hydrotalcite intercalation material LDHs can fill up the pore channel defect caused by the cured waterborne epoxy resin, and improve the barrier property of the resin, thereby improving the corrosion resistance of the coating.
Sodium tripolyphosphate is a class of amorphous water-soluble linear polyphosphates, is commonly used in food as a water retention agent, a quality modifier, a pH regulator or a metal chelating agent, and tripolyphosphate ions in the sodium tripolyphosphate can be chelated with metal ions to form a passivation film, so the sodium tripolyphosphate can be used as a metal corrosion inhibitor.
Thus, this example uses tripolyphosphate (P)3O10 5-) And intercalating LDHs to prepare the anticorrosive hydrotalcite with stronger anticorrosive capability. Specifically, a mixed solution of a metal nitrate solution, sodium hydroxide and sodium tripolyphosphate is dripped into deionized water to be stirred and centrifuged, the metal nitrate and the sodium hydroxide generate LDHs, and the tripolyphosphate radical is intercalated into the LDHs, so that the anticorrosive hydrotalcite is obtained, and the anticorrosive hydrotalcite improves the anticorrosive capacity by utilizing the capability of the tripolyphosphate radical ions to passivate metal magnesium and aluminum to form a protective film and the lamellar blocking effect of the LDHs.
Further, the step S10 specifically includes:
dissolving magnesium nitrate hexahydrate and aluminum nitrate nonahydrate in deionized water to obtain a metal nitrate solution;
dissolving sodium hydroxide and sodium tripolyphosphate in deionized water to obtain a mixed solution of the sodium hydroxide and the sodium tripolyphosphate;
dripping the metal nitrate solution and the mixed solution of sodium hydroxide and sodium tripolyphosphate into deionized water to obtain an alkaline mixture;
and sequentially stirring, crystallizing, centrifuging, washing and drying the alkaline mixture to obtain the anticorrosive hydrotalcite.
In a specific implementation, magnesium nitrate hexahydrate (Mg (NO) is selected3)2·6H2O) and aluminum nitrate nonahydrate (Al (NO)3)3·9H2O) preparing metal nitrate solution by mixing 5-10 parts of Mg (NO) by weight3)2·6H2O and 5-10 parts of Al (NO)3)3·9H2Dissolving O in 50-100 parts of deionized water, and forming a metal nitrate solution at room temperature under an inert atmosphere, wherein the content ratio of magnesium to aluminum in the metal nitrate solution is Mg: al ═ 2: (0.5-1). At room temperature under inert atmosphere, 3-5 parts of sodium hydroxide (NaOH) and 5-10 parts of sodium tripolyphosphate (Na)5P3O10) Dissolving in 50-100 parts of deionized water to prepare a mixed solution of sodium hydroxide and sodium tripolyphosphate. Then, a mixed solution of a metal nitrate solution, sodium hydroxide and sodium tripolyphosphate was simultaneously dropped into a beaker containing 100-150 parts of deionized water until the pH of the final mixture was adjusted to 9-10, to obtain an alkaline mixture. Stirring the alkaline mixture at 300-400 rpm and 70-80 ℃ for 7-9 hours to obtain white paste, transferring the white paste into a reaction kettle, and crystallizing at 70-80 ℃ for 24-48 hours. Forming a brown precipitate after crystallization, collecting the brown precipitate by centrifugation, and taking a water/ethanol mixture, wherein the volume ratio of water to ethanol is 4: (1-2), washing the brown precipitate three to five times by using the water/ethanol mixture, washing 100 parts of the brown precipitate for each time, and drying the washed product in an oven at the temperature of between 55 and 65 ℃ overnight to obtain the anticorrosive hydrotalcite.
Further, before dissolving magnesium nitrate hexahydrate and aluminum nitrate nonahydrate in deionized water to obtain a metal nitrate solution, the method further comprises: boiling deionized water, and cooling to 25-30 deg.C to remove dissolved carbon dioxide in the deionized water to avoid carbonate radical to tripolyphosphate (P)3O10 5-) Intercalated LDHs have an effect.
Step S20: and adding the anticorrosive hydrotalcite and dopamine into a trihydroxymethyl aminomethane buffer solution, stirring and centrifuging to obtain the modified anticorrosive hydrotalcite.
The Polydopamine (PDA) can be coated on the surfaces of various matrixes by auto-oxidation polymerization of the polydopamine (DA) under an alkaline condition to form an anticorrosive coating, and the coating has the advantages of good stability, strong water dispersibility, excellent biocompatibility and capability of being generated at normal temperature. And the polydopamine micro/nanosphere contains a large amount of amino and phenolic hydroxyl groups and other groups, and the amino and phenolic hydroxyl groups can be combined with metal ions.
Further, the step S20 specifically includes:
weighing 20-40 parts of the anticorrosive hydrotalcite and 5-10 parts of dopamine, adding the anticorrosive hydrotalcite and the dopamine into 30-60 parts of tris (hydroxymethyl) aminomethane buffer solution with the pH value of 8-9, and mechanically stirring to obtain a first stirring product;
and weighing 500 parts of 300-one water to centrifuge and wash the first stirring product to obtain the modified anticorrosive hydrotalcite.
Further, the stirring time of the mechanical stirring is 12-24 hours, and the stirring speed is 500-1000 rpm; the centrifugation times is 3-5 times, and the centrifugation speed is 1000-.
In the specific implementation, according to the parts by weight, 20-40 parts of the anticorrosive hydrotalcite is weighed and added into 30-60 parts of tris buffer solution (tris-HCl buffer solution) with the pH value of 8-9, 5-10 parts of dopamine is weighed and immediately added into the buffer solution, mechanical stirring is carried out for 12-24 hours under the dark and dark conditions, the stirring speed is 500-.
In the embodiment, by utilizing the characteristic of polymerization of dopamine in an alkaline environment, the anticorrosive hydrotalcite and dopamine are added into a tris buffer solution for stirring and centrifugation, so that dopamine forms a polydopamine film on the surface of the anticorrosive hydrotalcite, the modified anticorrosive hydrotalcite is obtained, the polydopamine grows on the surface of the anticorrosive hydrotalcite, the polyhydroxy structure of the polydopamine is utilized to enable the anticorrosive hydrotalcite to be better distributed in a coating, and the dispersibility of the anticorrosive hydrotalcite is improved. And when steel is corroded to generate metal cations and corrosion anions, the catechol group on the polydopamine and the metal cations can form a cross-linked network structure, so that the modified anticorrosive hydrotalcite is adsorbed on the surface of the steel matrix, and the effects of automatic protection and intelligent corrosion prevention are achieved. And corrosion anions can be replaced between layers, so that the cathode reaction of the corrosion reaction is weakened, the double corrosion prevention effect is achieved, and the metal matrix is prevented from being further corroded.
The embodiment of the invention also provides a water-based intelligent anticorrosive paint which is prepared from the following raw materials in parts by weight: 1 part of curing agent solution and 3-4 parts of aqueous anticorrosive paint mother liquor.
Referring to fig. 2, an embodiment of the present invention further provides a preparation method of a water-based intelligent anticorrosive paint, where the preparation method of the water-based intelligent anticorrosive paint includes:
step S30: and adding the modified anticorrosive hydrotalcite into a water-based epoxy resin solution, and stirring and vibrating to obtain a water-based anticorrosive paint mother solution.
The water-based epoxy resin is a raw material for preparing the water-based epoxy resin coating, and the water-based epoxy resin coating has the advantages of strong adaptability, good environmental protection performance, low price, no odor, non-flammability, good operability and the like, so that the modified anticorrosive hydrotalcite is added into a water-based epoxy resin solution to be stirred and vibrated to obtain a water-based anticorrosive coating mother solution for subsequent preparation of the water-based intelligent anticorrosive coating.
Further, the step S30 specifically includes:
mixing 100-120 parts of deionized water and 150-200 parts of aqueous epoxy resin according to the parts by weight to obtain an aqueous epoxy resin solution;
weighing 10-20 parts of the modified anticorrosive hydrotalcite, adding the modified anticorrosive hydrotalcite into the aqueous epoxy resin solution, and performing electromagnetic stirring to obtain a second stirring product;
and vibrating the second stirring product through an ultrasonic oscillator to obtain the water-based anticorrosive paint mother liquor.
Further, the stirring time of the electromagnetic stirring is 10-30 minutes, and the stirring speed is 50-100 revolutions per minute; the vibration time is 10-30 minutes, and the vibration power is 40-50 watts.
Further, the water-based epoxy resin is Ar555 epoxy resin, E51 epoxy emulsion or E44 epoxy emulsion.
In the concrete implementation, 10-20 parts of modified anticorrosive hydrotalcite is weighed according to parts by weight and added into 100-120 parts of deionized water and 150-200 parts of waterborne epoxy resin, electromagnetic stirring is adopted for 10-30 minutes, the stirring speed is 50-100 rpm, an ultrasonic oscillator is adopted for vibrating for 10-30 minutes after stirring, and the power is 40-50 watts, so that the waterborne anticorrosive coating mother solution is prepared.
Step S40: and mixing the aqueous anticorrosive paint mother liquor with a curing agent to obtain the aqueous intelligent anticorrosive paint.
Curing agents, also known as hardeners, curing agents or setting agents, are a class of substances or mixtures that enhance or control the curing reaction. This embodiment will aqueous anticorrosive paint mother liquor mixes with curing agent, obtains the aqueous intelligent anticorrosive paint of solidification, the curing agent is indispensable, otherwise aqueous epoxy in the aqueous anticorrosive paint mother liquor can not solidify. The curing agent is H228B, W650 or W651.
Further, the step S40 specifically includes:
weighing 30-50 parts by weight of curing agent and 50-80 parts by weight of deionized water, mechanically stirring for 10-20 minutes at a stirring speed of 100 and 200 revolutions per minute, and obtaining a curing agent solution after stirring;
and (3) mixing the curing agent solution with the aqueous anticorrosive paint mother liquor according to the proportion of 1 (3-4) to obtain the aqueous intelligent anticorrosive paint.
Referring to fig. 3, fig. 3 is an anticorrosion principle diagram of a preparation method of the aqueous intelligent anticorrosive coating, the aqueous intelligent anticorrosive coating prepared in the embodiment is coated on the surface of a metal substrate, tripolyphosphate ions exist between anticorrosive hydrotalcite layers, and by utilizing the characteristic that dopamine is polymerized in an alkaline environment, the anticorrosive hydrotalcite and dopamine are added into a tris (hydroxymethyl) aminomethane buffer solution to be stirred and centrifuged, so that dopamine forms a poly-dopamine film on the surface of the anticorrosive hydrotalcite, a modified anticorrosive hydrotalcite is obtained, and the anticorrosive hydrotalcite can be better distributed in the coating by utilizing the polyhydroxy structure of the poly-dopamine, so that the dispersibility of the anticorrosive hydrotalcite is improved. When steel is corroded to generate metal cations and corrosion anions, the catechol group on the polydopamine and the metal cations can form a cross-linked network structure, so that the modified anticorrosive hydrotalcite is adsorbed on the surface of the steel matrix, and the effects of automatic protection and intelligent corrosion prevention are achieved. And corrosion anions can be replaced between layers, so that the cathode reaction of the corrosion reaction is weakened, the double corrosion prevention effect is achieved, and the metal matrix is prevented from being further corroded.
In this embodiment, the anticorrosive hydrotalcite is obtained by dropping a mixed solution of a metal nitrate solution, sodium hydroxide and sodium tripolyphosphate into deionized water, stirring and centrifuging; adding the anticorrosive hydrotalcite and dopamine into a trihydroxymethyl aminomethane buffer solution, stirring and centrifuging to obtain modified anticorrosive hydrotalcite; adding the modified anticorrosive hydrotalcite into a water-based epoxy resin solution, and stirring and vibrating to obtain a water-based anticorrosive paint mother solution; and mixing the aqueous anticorrosive paint mother liquor with a curing agent to obtain the aqueous intelligent anticorrosive paint. According to the embodiment, the corrosion resistance is improved by utilizing the capability of the tripolyphosphate ions to passivate metal to form a protective film and the lamellar blocking effect of the hydrotalcite, and when steel is corroded to generate metal cations, the phenol groups on the dopamine and the metal cations can form a cross-linked network structure, so that the coating is adsorbed on the surface of a steel matrix, and the effects of automatic protection and intelligent corrosion prevention are achieved.
The embodiment of the invention also provides an anticorrosive coating which is obtained by coating and curing the water-based intelligent anticorrosive coating. The anticorrosive coating improves the anticorrosive capability by utilizing the capability of a tripolyphosphate ion to passivate metal to form a protective film and the lamellar blocking effect of hydrotalcite, and when steel is corroded to generate metal cations, the phenolic group on dopamine and the metal cations can form a cross-linked network structure, so that the coating is adsorbed on the surface of a steel matrix, and the effects of automatic protection and intelligent corrosion prevention are achieved.
In order to clearly understand the objects, technical solutions and advantages of the present invention, the present invention will be further described in detail with reference to the following embodiments. The specific examples described herein relate to specific data only to illustrate the present invention and are not intended to limit the invention.
Example 1
(1) Preparation of anticorrosive hydrotalcite: the deionized water was boiled and cooled to 25 ℃. According to the parts by weight, 10 parts of Mg (NO)3)2·6H2O and 5 parts of Al (NO)3)3·9H2Dissolving O in 50 parts of deionized water, and forming a metal nitrate solution at room temperature under an inert atmosphere, wherein the content ratio of magnesium to aluminum in the metal nitrate solution is Mg: al ═ 2: 1. at room temperature under an inert atmosphere, 3 parts NaOH and 5 parts Na5P3O10And dissolved in 50 parts of deionized water to prepare a mixed solution of sodium hydroxide and sodium tripolyphosphate. Then, a mixed solution of a metal nitrate solution, sodium hydroxide and sodium tripolyphosphate was simultaneously dropped into a beaker containing 100 parts of deionized water until the pH of the final mixture was adjusted to 9.5, to obtain an alkaline mixture. The alkaline mixture was stirred at 350 rpm and 75 ℃ for 8 hours to give a white paste, which was transferred to a reaction vessel and crystallized at 75 ℃ for 24 hours. After crystallization, a brown precipitate is formed, collected by centrifugation and then taken out of a water/ethanol mixture, wherein the volume ratio of water to ethanol is 4: washing the brown precipitate three times with 100 parts of the water/ethanol mixture each time, and drying the washed product in an oven at 55 ℃ overnight to obtain the anticorrosive hydrotalcite.
(2) Preparing modified anticorrosive hydrotalcite: weighing 20 parts by weight of the anticorrosive hydrotalcite, adding the anticorrosive hydrotalcite into 30 parts by weight of tris-HCl buffer solution with the pH value of 8.5, weighing 5 parts by weight of dopamine, immediately adding the dopamine into the buffer solution, mechanically stirring for 12 hours under dark and dark conditions at the stirring speed of 500 rpm, centrifugally washing with 300 parts of water after stirring is finished, centrifuging for 3 times, 10 minutes each time, and rotating at the rotating speed of 1000 rpm, and finally preparing the modified anticorrosive hydrotalcite.
(3) Preparing the water-based intelligent anticorrosive paint: weighing 10 parts of modified anticorrosive hydrotalcite according to parts by weight, adding the modified anticorrosive hydrotalcite into 100 parts of deionized water and 150 parts of Ar555 epoxy resin, electromagnetically stirring for 10 minutes at the stirring speed of 50 rpm, and vibrating for 10 minutes by using an ultrasonic oscillator after stirring at the power of 40 watts to prepare the aqueous anticorrosive paint mother liquor. Weighing 30 parts of H228B curing agent and 50 parts of deionized water, mechanically stirring for 10 minutes at a stirring speed of 100 rpm to obtain a curing agent solution after stirring; and mixing the curing agent solution with the aqueous anticorrosive paint mother liquor according to the proportion of 1:4 to obtain the aqueous intelligent anticorrosive paint.
Example 2
(1) Preparation of anticorrosive hydrotalcite: the deionized water was boiled and cooled to 25 ℃. According to the parts by weight, 10 parts of Mg (NO)3)2·6H2O and 5 parts of Al (NO)3)3·9H2Dissolving O in 80 parts of deionized water, and forming a metal nitrate solution at room temperature under an inert atmosphere, wherein the content ratio of magnesium to aluminum in the metal nitrate solution is Mg: al ═ 2: 1. at room temperature under an inert atmosphere, 3 parts NaOH and 5 parts Na5P3O10And dissolved in 80 parts of deionized water to prepare a mixed solution of sodium hydroxide and sodium tripolyphosphate. Then, a mixed solution of a metal nitrate solution, sodium hydroxide and sodium tripolyphosphate was simultaneously added dropwise to a beaker containing 120 parts of deionized water until the pH of the final mixture was adjusted to 9.5, resulting in an alkaline mixture. The alkaline mixture was stirred at 350 rpm and 75 ℃ for 8 hours to give a white paste, which was transferred to a reaction vessel and crystallized at 70 ℃ for 36 hours. After crystallization, a brown precipitate is formed, collected by centrifugation and then taken out of a water/ethanol mixture, wherein the volume ratio of water to ethanol is 2: washing the brown precipitate four times with 150 parts of the water/ethanol mixture each time, and drying the washed product in an oven at 60 ℃ overnight to obtain the anticorrosive hydrotalcite.
(2) Preparing modified anticorrosive hydrotalcite: weighing 30 parts by weight of the anticorrosive hydrotalcite, adding the anticorrosive hydrotalcite into 40 parts by weight of tris-HCl buffer solution with the pH value of 8.5, weighing 8 parts by weight of dopamine, immediately adding the dopamine into the buffer solution, mechanically stirring for 18 hours under dark and dark conditions at the stirring speed of 800 rpm, centrifugally washing with 400 parts by weight of water after stirring is finished, centrifuging for 4 times, 15 minutes each time, and rotating at the rotating speed of 1500 rpm, and finally preparing the modified anticorrosive hydrotalcite.
(3) Preparing the water-based intelligent anticorrosive paint: weighing 15 parts of modified anticorrosive hydrotalcite by weight, adding the modified anticorrosive hydrotalcite into 100 parts of deionized water and 180 parts of E51 epoxy emulsion, electromagnetically stirring for 20 minutes at a stirring speed of 80 rpm, and vibrating for 20 minutes by using an ultrasonic oscillator after stirring at a power of 45 watts to obtain the aqueous anticorrosive paint mother liquor. Weighing 40 parts of W650 curing agent and 60 parts of deionized water, mechanically stirring for 15 minutes at a stirring speed of 150 rpm to obtain a curing agent solution after stirring; and mixing the curing agent solution with the aqueous anticorrosive paint mother liquor according to the proportion of 1:3 to obtain the aqueous intelligent anticorrosive paint.
Example 3
(1) Preparation of anticorrosive hydrotalcite: the deionized water was boiled and cooled to 30 ℃. According to the parts by weight, 10 parts of Mg (NO)3)2·6H2O and 5 parts of Al (NO)3)3·9H2Dissolving O in 100 parts of deionized water, and forming a metal nitrate solution at room temperature under an inert atmosphere, wherein the content ratio of magnesium to aluminum in the metal nitrate solution is Mg: al ═ 2: 1. 5 parts of NaOH and 10 parts of Na are added at room temperature under an inert atmosphere5P3O10Dissolved in 100 parts of deionized water to prepare a mixed solution of sodium hydroxide and sodium tripolyphosphate. Then, a mixed solution of a metal nitrate solution, sodium hydroxide and sodium tripolyphosphate was simultaneously added dropwise to a beaker containing 150 parts of deionized water until the pH of the final mixture was adjusted to 9-10, to obtain an alkaline mixture. The alkaline mixture was stirred at 400 rpm and 80 ℃ for 9 hours to give a white paste, which was transferred to a reaction vessel and crystallized at 80 ℃ for 48 hours. After crystallization, a brown precipitate is formed, which is collected by centrifugation and then taken from a water/ethanol mixture, wherein water and ethanolThe volume ratio of the alcohol is 4: 1, washing the brown precipitate three to five times with 200 parts of each water/ethanol mixture, and drying the washed product in an oven at 65 ℃ overnight to obtain the anticorrosive hydrotalcite.
(2) Preparing modified anticorrosive hydrotalcite: weighing 40 parts by weight of the anticorrosive hydrotalcite, adding the anticorrosive hydrotalcite into 60 parts by weight of tris-HCl buffer solution with the pH value of 8.5, weighing 10 parts by weight of dopamine, immediately adding the dopamine into the buffer solution, mechanically stirring for 24 hours under dark and dark conditions at the stirring speed of 1000 rpm, centrifugally washing with 500 parts by weight of water after stirring is finished, centrifuging for 5 times, each time for 20 minutes at the rotating speed of 2000 rpm, and finally preparing the modified anticorrosive hydrotalcite.
(3) Preparing the water-based intelligent anticorrosive paint: weighing 20 parts of modified anticorrosive hydrotalcite by weight, adding the modified anticorrosive hydrotalcite into 120 parts of deionized water and 200 parts of E44 epoxy emulsion, electromagnetically stirring for 30 minutes at a stirring speed of 100 revolutions per minute, and vibrating for 30 minutes by using an ultrasonic oscillator after stirring at a power of 50 watts to obtain the aqueous anticorrosive paint mother liquor. Weighing 50 parts of W651 curing agent and 80 parts of deionized water, mechanically stirring for 20 minutes at a stirring speed of 200 rpm to obtain a curing agent solution after stirring is finished; and mixing the curing agent solution with the aqueous anticorrosive paint mother liquor according to the proportion of 1:3 to obtain the aqueous intelligent anticorrosive paint.
Comparative example 1
(1) Preparation of the water-based epoxy resin coating: adding 100 parts of deionized water and 150 parts of Ar555 epoxy resin into a beaker, electromagnetically stirring for 10 minutes at the stirring speed of 50 rpm, and vibrating for 10 minutes by using an ultrasonic oscillator after stirring at the power of 40W to prepare a mother solution of the water-based epoxy resin coating; and (3) mechanically stirring 30 parts of H228B curing agent and 50 parts of deionized water for 10 minutes at the stirring speed of 100 rpm, and mixing the mixture with the aqueous epoxy resin coating mother liquor according to the proportion of 1:4 to prepare the aqueous epoxy resin coating.
(2) Preparing the water-based anticorrosive paint: mixing 10 parts of Mg (NO)3)2·6H2O and 5 parts of Al (NO)3)3·9H2Dissolving O in 50 portions of deionized water to form metal nitric acid at room temperature under inert atmosphereAnd the content ratio of magnesium to aluminum in the metal nitrate solution is Mg: al ═ 2: 1. a mixed solution of sodium hydroxide and sodium tripolyphosphate was prepared by dissolving 3 parts NaOH and 5 parts Na5P3O10 in 50 parts deionized water at room temperature under an inert atmosphere (deionized water was boiled to remove dissolved carbon dioxide and kept at 25 ℃ for use). Then, a mixed solution of a metal nitrate solution, sodium hydroxide and sodium tripolyphosphate was simultaneously dropped into a beaker containing 100 parts of deionized water until the pH of the final mixture was adjusted to 9.5, to obtain an alkaline mixture. The basic mixture was stirred at 70-80 ℃ for 7 hours at 300 rpm to give a white paste which was transferred to a reaction vessel and crystallized at 70 ℃ for 24 hours. After crystallization, a brown precipitate is formed, collected by centrifugation and then taken out of a water/ethanol mixture, wherein the volume ratio of water to ethanol is 4: washing the brown precipitate three to five times with 100 parts of each water/ethanol mixture, and drying the washed product in an oven at 55 ℃ overnight to obtain the anticorrosive hydrotalcite. Adding 10 parts of anticorrosive hydrotalcite into 1000 parts of deionized water and 150 parts of Ar555 waterborne epoxy resin, electromagnetically stirring for 10 minutes at the stirring speed of 50 rpm, and vibrating for 10 minutes by using an ultrasonic oscillator after stirring at the power of 40 watts to prepare the mother solution of the waterborne anticorrosive paint. And (3) mechanically stirring 30 parts of H228B curing agent and 50 parts of deionized water for 10 minutes at a stirring speed of 100 rpm, and mixing the mixture with the mother solution of the water-based anticorrosive paint according to a ratio of 1:4 to prepare the water-based anticorrosive paint.
(3) The prepared water-based epoxy resin coating, water-based anticorrosive coating and water-based intelligent anticorrosive coating are respectively subjected to film forming on a steel sheet substrate, the adhesion is detected according to GB1720-1979, and the corrosion resistance of 3 resin films is detected through salt spray.
| Group of | Water-based epoxy resin coating | Water-based anticorrosive paint | Water-based intelligent anticorrosive paint |
| Adhesion (MPa) | 7.05 | 7.52 | 8.72 |
TABLE 1 test results of adhesion after film formation of the coating
Table 1 shows the adhesion detection results of the water-based epoxy resin coating, the water-based anticorrosive coating and the water-based intelligent anticorrosive coating after film formation, and the adhesion performance of the water-based epoxy resin coating after film formation is the lowest and is only 7.05 MPa. The adhesion performance of the aqueous anticorrosive coating added with the anticorrosive hydrotalcite after film formation is improved, which is attributed to the magnesium-aluminum oxide in the anticorrosive hydrotalcite, so that the coating has better adsorption when being coated on a metal matrix, thereby increasing the adhesion performance of the coating. The adhesion performance of the water-based intelligent anticorrosive coating after film formation is highest because dopamine on the surface of the anticorrosive hydrotalcite has a large number of active groups, and can form a network structure with a metal matrix, so that a coating is more tightly combined with metal, and the adhesion performance of the coating is greatly improved.
Referring to fig. 4, fig. 4 is an ac impedance graph of various paints after 800 hours of salt spray test, in which a square point a, a circular point b, and a triangular point c represent impedances of the aqueous epoxy resin paint, the aqueous anticorrosive paint, and the aqueous smart anticorrosive paint, respectively. It can be seen that the impedance of group a is lowest and weber impedance appears compared to groups b and c, indicating that the coating has broken down the coating by current in the ac impedance test, and the coating loses its protective effect, thus indicating that group a, to which no filler has been added, has no corrosion protection. The impedance value of the group b is obviously improved due to the action of the anti-corrosion hydrotalcite, namely the lamellar structure of the hydrotalcite increases the barrier property so as to improve the anti-corrosion capability, the passivation effect of tripolyphosphate radical ions on metal generates a protective film to protect a metal anode so as to improve the anti-corrosion capability, and the interlayer ion exchange capability of the hydrotalcite can adsorb corrosion anions, reduce the occurrence of cathode corrosion reaction and further improve the anti-corrosion capability of a coating. The impedance value of the group c is the highest because the modified anticorrosive hydrotalcite has higher dispersion performance in the coating, can form a network structure with iron ions and is adsorbed on the metal surface, once corrosion occurs, the iron ions appear, and the modified anticorrosive hydrotalcite can immediately play a role, so that the intelligent corrosion prevention effect is achieved.
Finally, it should also be noted that the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
While preferred embodiments of the present invention have been described, additional variations and modifications in those embodiments may occur to those skilled in the art once they learn of the basic inventive concepts. Therefore, it is intended that the appended claims be interpreted as including preferred embodiments and all such alterations and modifications as fall within the scope of the invention.
It will be apparent to those skilled in the art that various changes and modifications may be made in the present invention without departing from the spirit and scope of the invention. Thus, if such modifications and variations of the present invention fall within the scope of the claims of the present invention and their equivalents, the present invention is also intended to include such modifications and variations.
Claims (10)
1. The modified anticorrosive hydrotalcite is characterized by being prepared from the following raw materials in parts by weight: 20-40 parts of anticorrosive hydrotalcite, 5-10 parts of dopamine and 30-60 parts of tris-HCl buffer solution with the pH value of 8-9.
2. The preparation method of the modified anticorrosive hydrotalcite is characterized by comprising the following steps:
dripping a mixed solution of a metal nitrate solution, sodium hydroxide and sodium tripolyphosphate into deionized water, stirring and centrifuging to obtain anticorrosive hydrotalcite;
and adding the anticorrosive hydrotalcite and dopamine into a trihydroxymethyl aminomethane buffer solution, stirring and centrifuging to obtain the modified anticorrosive hydrotalcite.
3. The preparation method according to claim 2, wherein the modified anticorrosive hydrotalcite is obtained by adding the anticorrosive hydrotalcite and dopamine into tris buffer solution, stirring and centrifuging, and specifically comprises:
weighing 20-40 parts of the anticorrosive hydrotalcite and 5-10 parts of dopamine, adding the anticorrosive hydrotalcite and the dopamine into 30-60 parts of tris (hydroxymethyl) aminomethane buffer solution with the pH value of 8-9, and mechanically stirring for 12-24 hours at the stirring speed of 500-1000 rpm to obtain a first stirring product;
and weighing 500 parts of 300-2000 parts of water to centrifuge and wash the first stirring product, wherein the centrifugation time is 3-5 times, and the centrifugation speed is 1000-2000 rpm, so as to obtain the modified anticorrosive hydrotalcite.
4. The preparation method according to claim 3, wherein the mixed solution of the metal nitrate solution, the sodium hydroxide and the sodium tripolyphosphate is dropped into deionized water to be stirred and centrifuged to obtain the anticorrosive hydrotalcite, and the preparation method specifically comprises the following steps:
dissolving magnesium nitrate hexahydrate and aluminum nitrate nonahydrate in deionized water to obtain a metal nitrate solution;
dissolving sodium hydroxide and sodium tripolyphosphate in deionized water to obtain a mixed solution of the sodium hydroxide and the sodium tripolyphosphate;
dripping the metal nitrate solution and the mixed solution of sodium hydroxide and sodium tripolyphosphate into deionized water to obtain an alkaline mixture;
and sequentially stirring, crystallizing, centrifuging, washing and drying the alkaline mixture to obtain the anticorrosive hydrotalcite.
5. The method of claim 4, wherein prior to dissolving the magnesium nitrate hexahydrate and the aluminum nitrate nonahydrate in deionized water to provide the metal nitrate solution, the method further comprises:
the deionized water was boiled and cooled to 25-30 ℃.
6. The water-based intelligent anticorrosive paint is characterized by being prepared from the following raw materials in parts by weight: 1 part of curing agent solution and 3-4 parts of aqueous anticorrosive paint mother liquor.
7. A preparation method of a water-based intelligent anticorrosive paint is characterized by comprising the following steps:
adding the modified anticorrosive hydrotalcite into a water-based epoxy resin solution, stirring and vibrating to obtain a water-based anticorrosive paint mother solution;
and mixing the aqueous anticorrosive paint mother liquor with a curing agent to obtain the aqueous intelligent anticorrosive paint.
8. The preparation method of claim 7, wherein the modified anticorrosive hydrotalcite is added into the aqueous epoxy resin solution to be stirred and vibrated to obtain the aqueous anticorrosive paint mother liquor, and the preparation method specifically comprises the following steps:
mixing 100-120 parts of deionized water and 150-200 parts of aqueous epoxy resin according to the parts by weight to obtain an aqueous epoxy resin solution;
weighing 10-20 parts of modified anticorrosive hydrotalcite, adding the modified anticorrosive hydrotalcite into the aqueous epoxy resin solution, and performing electromagnetic stirring for 10-30 minutes at a stirring speed of 50-100 rpm to obtain a second stirring product;
and vibrating the second stirring product by an ultrasonic oscillator for 10-30 minutes at a vibration power of 40-50 watts to obtain the mother solution of the water-based anticorrosive paint.
9. The preparation method of claim 8, wherein the mixing of the aqueous anticorrosive paint mother liquor and the curing agent to obtain the aqueous intelligent anticorrosive paint specifically comprises:
weighing 30-50 parts by weight of curing agent and 50-80 parts by weight of deionized water, mechanically stirring for 10-20 minutes at a stirring speed of 100 and 200 revolutions per minute, and obtaining a curing agent solution after stirring;
and (3) mixing the curing agent solution with the aqueous anticorrosive paint mother liquor according to the proportion of 1 (3-4) to obtain the aqueous intelligent anticorrosive paint.
10. An anti-corrosion coating is characterized in that the anti-corrosion coating is obtained by coating and curing the water-based intelligent anti-corrosion coating according to claim 6.
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