CN111548704B - Composite anticorrosive coating based on interface regulation and control and preparation method and application thereof - Google Patents
Composite anticorrosive coating based on interface regulation and control and preparation method and application thereof Download PDFInfo
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- CN111548704B CN111548704B CN202010475071.2A CN202010475071A CN111548704B CN 111548704 B CN111548704 B CN 111548704B CN 202010475071 A CN202010475071 A CN 202010475071A CN 111548704 B CN111548704 B CN 111548704B
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D163/00—Coating compositions based on epoxy resins; Coating compositions based on derivatives of epoxy resins
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
- C08G73/02—Polyamines
- C08G73/026—Wholly aromatic polyamines
- C08G73/0266—Polyanilines or derivatives thereof
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
- C08K3/042—Graphene or derivatives, e.g. graphene oxides
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/08—Anti-corrosive paints
Abstract
The invention discloses a composite anticorrosive coating based on interface regulation and control as well as a preparation method and application thereof, wherein the method comprises the following steps: adding an aniline monomer into a graphene oxide solution, and dropwise adding an oxidant under the condition of ice-water bath stirring to prepare a polyaniline-graphene oxide composite material; adding the polyaniline-graphene oxide composite material into aqueous epoxy resin to obtain a composite coating, and coating the composite coating to form a film to obtain the composite anticorrosive coating. According to the invention, based on the regulation and control of polyaniline and graphene oxide structures, the correlation between the structure and the performance of the polyaniline-graphene oxide composite material is determined, the PANI-GO composite coating with stable dispersity is prepared, and on the basis, the controllable preparation of the high-efficiency anti-corrosion GO-based composite coating and the high-efficiency protection of a metal matrix are realized.
Description
Technical Field
The invention relates to the field of metal corrosion prevention, in particular to a composite corrosion-resistant coating based on interface regulation and control as well as a preparation method and application thereof.
Background
Marine preservation is linked to national safety and marine economic development. Currently, the most widely used marine corrosion protection is by organic coatings. After long-term service, fillers such as chromate, metal oxide and the like in the organic coating can release heavy metal ions, so that the environment is harmed. For this reason, researchers have developed various high-performance, environmentally friendly fillers to improve the performance of organic coatings. The graphene/graphene oxide (G/GO) has strong barrier property and high chemical stability, can form a labyrinth effect in an organic coating after being uniformly dispersed, and is an anticorrosive filler with great potential. However, the G/GO composite coating meets new challenges, which make it difficult to popularize and apply the G/GO composite coating commercially: the strong acting force between G/GO layers can cause the G/GO layers to form agglomeration defects in the organic coating, so that the coating is rapidly failed; after long-term service, the micro-battery can form a corrosion micro-battery with metal, and G/GO can be used as a cathode phase to accelerate metal corrosion.
Therefore, the method has very important practical significance and strategic significance for solving the neck clamping problem in the application of the G/GO composite coating.
Disclosure of Invention
In view of the defects of the prior art, the invention aims to provide a composite anticorrosive coating based on interface regulation and control, and a preparation method and application thereof, and aims to solve the problem that the existing anticorrosive coating has poor anticorrosive effect on a metal substrate.
The technical scheme of the invention is as follows:
a preparation method of a composite anticorrosive coating based on interface regulation comprises the following steps:
applying a first voltage to an initial graphite paper electrode in a first sulfuric acid solution to obtain flexible graphite paper;
applying a second voltage to the flexible graphite paper electrode in a second sulfuric acid solution to obtain a graphene oxide solution;
adding an aniline monomer into the graphene oxide solution, and dropwise adding an oxidant under the condition of ice-water bath stirring to obtain a polyaniline-graphene oxide composite material;
respectively determining the structure, components and grafting ratio of the polyaniline-graphene oxide composite material by XPS, Raman and FTIR analysis means, evaluating the dispersion stability of different polyaniline-graphene oxide composite materials by a precipitation experiment, and determining reaction conditions by selecting the polyaniline-graphene oxide composite material with the best dispersion stability;
adding the polyaniline-graphene oxide composite material with the best dispersion stability into aqueous epoxy resin to obtain a composite coating, and coating the composite coating to form a film to obtain the composite anticorrosive coating.
The preparation method of the composite anticorrosive coating based on interface regulation and control comprises the following steps of enabling the concentration of the first sulfuric acid solution to be more than 95% and enabling the first voltage to be 8-12V.
The preparation method of the composite anticorrosive coating based on interface regulation and control comprises the steps of preparing a first sulfuric acid solution, preparing a second sulfuric acid solution, and controlling the concentration of the second sulfuric acid solution to be 30% -70% and controlling the second voltage to be 4-8V.
The preparation method of the composite anticorrosive coating based on interface regulation and control comprises the step of preparing the aniline monomer, wherein the concentration of the aniline monomer is 1-3 mol/L.
The preparation method of the composite anticorrosive coating based on interface regulation and control comprises the step of preparing the composite anticorrosive coating based on interface regulation and control, wherein the mass ratio of the aniline monomer to the oxidant is 1:3-3: 1.
The preparation method of the composite anticorrosive coating based on interface regulation and control is characterized in that the oxidant is (NH)4)2SO4Or FeCl3One kind of (1).
The preparation method of the composite anticorrosive coating based on interface regulation and control comprises the following step of preparing the polyaniline-graphene oxide composite material, wherein the polyaniline-graphene oxide composite material accounts for 1-10% of the composite anticorrosive coating by weight.
The preparation method of the composite anticorrosive coating based on interface regulation and control comprises the step of preparing the composite anticorrosive coating, wherein the thickness of the composite anticorrosive coating is 20-100 micrometers.
The invention discloses a composite anticorrosive coating based on interface regulation, which is prepared by the preparation method of the composite anticorrosive coating based on interface regulation.
The invention discloses application of a composite anticorrosive coating based on interface regulation, wherein the composite anticorrosive coating based on interface regulation is used for metal corrosion prevention.
Has the advantages that: the invention provides a preparation method of a composite anticorrosive coating based on interface regulation, which is based on the structural regulation of Polyaniline (PANI) and Graphene Oxide (GO), determines the correlation between the structure and the performance of a polyaniline-graphene oxide composite material, and prepares a PANI-GO composite coating with stable dispersibility; on the basis, controllable preparation of the high-efficiency anticorrosive GO-based composite coating and high-efficiency protection of a metal matrix are realized.
Drawings
Fig. 1 is a flowchart of a preferred embodiment of a method for preparing a composite anticorrosive coating based on interface regulation according to the present invention.
Fig. 2 is a graph of the dispersion stability results of the PANI-GO composite prepared in example 1 of the present invention and the PANI prepared in comparative example 1 at different time periods, wherein the left side of the graph is PANI and the right side is the PANI-GO composite.
FIG. 3 is a Nyquist plot of the PANI-GO/WEP coatings prepared in example 1 of the present invention versus the PANI/WEP coatings prepared in comparative example 1 and the WEP coatings prepared in comparative example 2 after 10 days of service in 3.5% NaCl solution.
FIG. 4 is a graph of Bode after 10 days of service in 3.5% NaCl solution of the PANI-GO/WEP coatings prepared in example 1 of the present invention versus the PANI/WEP coatings prepared in comparative example 1 and the WEP coatings prepared in comparative example 2.
Detailed Description
The invention provides a composite anticorrosive coating based on interface regulation and control as well as a preparation method and application thereof, and the invention is further described in detail below in order to make the purpose, technical scheme and effect of the invention clearer and clearer. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The organic coating is the most widely applied mode of active marine corrosion prevention, and graphene/graphene oxide (G/GO) has strong barrier property and high chemical stability and is widely applied to organic coating fillers to enhance the protective performance of the coating. However, strong van der waals forces between G/GO layers can cause them to agglomerate within the organic coating, resulting in a reduction in coating performance; the potential of the G/GO is positive, and the G/GO and metal form a corrosion micro-battery after a long-term service corrosion medium enters the micro-battery, so that metal corrosion is accelerated; the two restrict the application and development of the G/GO-based composite coating in the practical environment.
Based on the problems in the prior art, the invention provides a preparation method of a composite anticorrosive coating based on interface regulation, as shown in fig. 1, the preparation method comprises the following steps:
s10, applying a first voltage to the initial graphite paper electrode in a first sulfuric acid solution to obtain flexible graphite paper;
s20, applying a second voltage to the flexible graphite paper electrode in a second sulfuric acid solution to obtain a graphene oxide solution;
s30, adding an aniline monomer into the graphene oxide solution, and dropwise adding an oxidant under the condition of ice-water bath stirring to obtain a polyaniline-graphene oxide composite material;
s40, respectively determining the structure, the components and the grafting ratio of the polyaniline-graphene oxide composite material by XPS, Raman and FTIR analysis means, evaluating the dispersion stability of different polyaniline-graphene oxide composite materials through a precipitation experiment, and determining the reaction conditions by selecting the polyaniline-graphene oxide composite material with the best dispersion stability;
s50, adding the polyaniline-graphene oxide composite material with the best dispersion stability into aqueous epoxy resin to obtain a composite coating, and coating the composite coating to form a film to obtain the composite anticorrosive coating.
In the embodiment, structural regulation and control of a polyaniline-graphene oxide composite (PANI-GO) material are used as research focuses to prepare the high-performance GO-based anticorrosive coating, and good dispersion stability of the PANI-GO material is a premise for ensuring excellent metal protection performance of a composite anticorrosive coating (PANI-GO/water-based epoxy coating) and realizing a PANI-GO synergistic protection effect. In the embodiment, the PANI and GO can form pi-pi interaction or the PANI can improve the dispersity of GO by covalent grafting with a specific functional group on the surface of GO, and the PANI can also wrap the GO to avoid galvanic corrosion between the PANI and metal; also the conductivity of GO may facilitate passivation of the metal by PANI. Therefore, the structure of GO, the type, number and proportion of GO surface functional groups directly affect the grafting rate of GO with PANI and the performance of the resulting PANI-GO composite, and further affect the performance of the composite anticorrosive coating.
Therefore, in the embodiment, the PANI-GO composite material is prepared by in-situ chemical polymerization of PANI on the surface of GO, then the grafting types of the two are determined by adopting FTIR, XPS and Raman chemical structure analysis means, the structure of GO is regulated and controlled, GO with different hydroxyl, epoxy and carboxyl contents or proportions is obtained, different PANI-GO composite materials are prepared by in-situ chemical polymerization of the PANI on the surface of GO under different reaction conditions, the relationship between the GO structure/reaction condition and modified GO performance is determined by analyzing the components, the structure and the performance of the composite materials, the bonding theory of the two is established, and the controllable preparation of the PANI-GO composite material and the GO-based composite coating is realized.
In some embodiments, the starting graphite is treated in a first sulfuric acid solutionApplying a first voltage to the paper electrode to obtain flexible graphite paper; and applying a second voltage to the flexible graphite paper electrode in a second sulfuric acid solution to obtain a graphene oxide solution. In the embodiment, a two-step method is adopted to electrochemically strip graphite paper to prepare graphene oxide. Specifically, to ensure H2SO4Intercalation is carried out in the initial graphite paper, the concentration of the first sulfuric acid solution is more than 95 percent, and the first voltage is 8-12V; in order to realize the oxidation and stripping of the intercalated graphite paper, the concentration of the first sulfuric acid solution is 30-70%, and the second voltage is 4-8V. For example, a voltage of 10V is applied to a graphite paper electrode in a sulfuric acid solution with a concentration of 98% to complete intercalation of graphite paper, and then a voltage of 5V is applied to a flexible graphite paper electrode in a sulfuric acid solution with a concentration of 50% to complete oxidation and stripping of GO, so that graphene oxide is obtained. In this embodiment, GO with different numbers or ratios of functional groups can be obtained by controlling the concentration of the second sulfuric acid solution, and the higher the concentration of the second sulfuric acid solution is, the higher the carboxyl content of the generated GO is.
In some embodiments, aniline monomer with the concentration of 1-3mol/L is added into the graphene oxide solution, the mixture is uniformly stirred, and then under the conditions of ice water bath and stirring, the oxidant is added dropwise, so that the PANI-GO composite material is prepared in situ. In this embodiment, if the concentration of the aniline monomer is too low (less than 1mol/L), the polymerization efficiency of the aniline monomer is too low; if the concentration of the aniline monomer is too high (greater than 3mol/L), then depolymerization of the aniline monomer may occur.
In some embodiments, the mass ratio of the aniline monomer to the oxidizing agent is from 1:3 to 3: 1. In this embodiment, if the ratio of the aniline monomer is too low, the non-conductive polyaniline in a fully oxidized state is generated; if the ratio of the aniline monomer is too high, the oxidation degree of the product polyaniline is insufficient. In this embodiment, the oxidant is (NH)4)2SO4Or FeCl3But is not limited thereto.
In some embodiments, the structure, composition and grafting ratio of the PANI-GO composite material are determined by using analysis means such as XPS, Raman, FTIR and the like, and the dispersion stability of the PANI-GO composite material prepared under different conditions is evaluated by a precipitation experiment, wherein the PANI-GO composite material with the best dispersion stability is the optimal reaction condition and the PANI-GO structural component.
In some embodiments, the PANI-GO composite material is added into a water-based epoxy resin, a certain amount of distilled water is added to dilute the epoxy resin, the mixture is uniformly stirred and subjected to ultrasonic treatment for a period of time, a water-based epoxy resin curing agent is added to the mixture and is manually and uniformly stirred to prepare a composite coating, and the composite coating is coated on a metal surface to prepare a PANI-GO/WEP coating, namely a composite anticorrosive coating. In this embodiment, in the composite anticorrosive coating, the weight ratio of the polyaniline-graphene oxide composite material is 1-10%. If the content of the PANI-GO composite material is lower than 1%, bubbles can appear in the prepared composite anticorrosive coating, and if the content of the PANI-GO composite material is too high, agglomeration of the PANI-GO composite material can be caused, so that the metal anticorrosive effect of the composite anticorrosive coating is influenced.
In some embodiments, the composite corrosion protective coating has a thickness of 20 to 100 micrometers.
In some embodiments, the metal is one of carbon steel, stainless steel, or an aluminum alloy, but is not limited thereto.
In some embodiments, the invention further provides a composite anticorrosive coating based on interface regulation, and the composite anticorrosive coating is prepared by the preparation method of the composite anticorrosive coating based on interface regulation.
In some embodiments, the invention further provides application of the composite anticorrosive coating based on interface regulation, and the composite anticorrosive coating based on interface regulation is used for metal corrosion prevention.
The preparation method of the composite anticorrosive coating based on interface regulation and the metal anticorrosive performance thereof are further explained by the following specific examples:
example 1
1) And applying 10V voltage in 98% concentrated H2SO4 solution to react for 20 min. Then transferring the anode and the anode into 8% concentrated H2SO4 solution, applying voltage of 5V, and reacting for 1 minute to obtain GO sulfuric acid solution;
2) diluting the sulfuric acid concentration in the sulfuric acid solution of GO to 1mol/L by adopting a semipermeable membrane to obtain a mixed solution;
3) and adding aniline monomer into the mixed solution, and stirring until the white precipitate is completely dissolved. And then dropwise adding an ammonium persulfate solution under the ice-water bath condition, and stirring for reacting for 24 hours to obtain a PANI-GO mixed solution. And the sulfuric acid in the solution is removed to pH > 5 by adopting a semipermeable membrane;
4) measuring a certain amount of the PANI-GO mixed solution prepared in the step (3), filling the mixed solution into a sample bottle, standing for a period of time, and evaluating the dispersion stability, wherein the result is shown in figure 2;
5) connecting a copper wire to the surface of Q235, encapsulating by epoxy resin, and preparing a metal electrode. Grinding the surface of Q235 carbon steel of the electrode to 1000# by using metallographic abrasive paper, then sequentially removing oil and cleaning by using deionized water and absolute ethyl alcohol, and drying by using an air duct;
6) and (3) weighing 5g of waterborne epoxy resin, adding the mixed solution prepared in the step (3) with equal mass, stirring uniformly, adding the waterborne epoxy resin curing agent, and mixing uniformly. Coating the surface of the Q235 carbon steel electrode treated in the step (5) with a brush to prepare a coated electrode;
7) and (3) placing the PANI-GO/WEP metal electrode prepared in the step (6) in a 3.5% NaCl solution for service, and monitoring the EIS after the electrode is placed in service for 10 days by adopting an electrochemical workstation, wherein the results are shown in fig. 3 and fig. 4.
Comparative example 1
Compared with example 1, PANI prepared by chemical oxidative polymerization directly using 1mol/L sulfuric acid solution has the dispersion stability results shown in FIG. 2. And a coated electrode was prepared in the same manner as in example 1, the prepared PANI/WEP metal electrode was used in a 3.5% NaCl solution, and an EIS after 10 days of service was monitored and tested using an electrochemical workstation, with the results shown in fig. 3 and 4.
Comparative example 2
Coating water-based epoxy resin on the surface of a treated Q235 carbon steel electrode to obtain a WEP coated electrode, serving the WEP coated electrode in a 3.5% NaCl solution, monitoring EIS after 10 days of service by using an electrochemical workstation, and testing the EIS, wherein the results are shown in fig. 3 and 4.
As can be seen from FIG. 2, the PANI-GO has no obvious change after standing for 10 days, and the PANI is layered, which shows that the PANI-GO has better dispersion stability in an aqueous solution.
As can be seen from figures 3 and 4, after the coating is in service for 10 days, the capacitive arc radius and the low-frequency impedance mode value of the prepared PANI-GO/WEP coating are larger than those of the PANI/WEP coating and the WEP coating, and the PANI-GO/WEP coating has better anti-corrosion protection performance on Q235 carbon steel.
In summary, the invention provides a preparation method of a composite anticorrosive coating based on interface regulation, which is based on Polyaniline (PANI) and Graphene Oxide (GO) structure regulation, so that the correlation between the structure and the performance of a polyaniline-graphene oxide composite material is determined, and the PANI-GO composite coating with stable dispersibility is prepared. On the basis, controllable preparation of the high-efficiency anticorrosive GO-based composite coating and high-efficiency protection of a metal matrix are realized.
It is to be understood that the invention is not limited to the examples described above, but that modifications and variations may be effected thereto by those of ordinary skill in the art in light of the foregoing description, and that all such modifications and variations are intended to be within the scope of the invention as defined by the appended claims.
Claims (8)
1. A preparation method of a composite anticorrosive coating based on interface regulation is characterized by comprising the following steps:
applying a first voltage to an initial graphite paper electrode in a first sulfuric acid solution to obtain flexible graphite paper;
applying a second voltage to the flexible graphite paper electrode in a second sulfuric acid solution to obtain a graphene oxide solution;
adding an aniline monomer into the graphene oxide solution, and dropwise adding an oxidant under the condition of ice-water bath stirring to obtain a polyaniline-graphene oxide composite material;
respectively determining the structure, components and grafting rate of the polyaniline-graphene oxide composite material by XPS, Raman and FTIR analysis means, evaluating the dispersion stability of different polyaniline-graphene oxide composite materials by a precipitation experiment, and determining reaction conditions by selecting the polyaniline-graphene oxide composite material with the best dispersion stability;
adding the polyaniline-graphene oxide composite material with the best dispersion stability into aqueous epoxy resin to obtain a composite coating, and coating the composite coating to form a film to obtain the composite anticorrosive coating;
the concentration of the first sulfuric acid solution is more than 95%, and the first voltage is 8-12V; the concentration of the second sulfuric acid solution is 30-70%, and the second voltage is 4-8V.
2. The preparation method of the composite anticorrosive coating based on interfacial modulation according to claim 1, wherein the concentration of the aniline monomer is 1 to 3 mol/L.
3. The preparation method of the composite anticorrosive coating based on interface regulation and control according to claim 1, characterized in that the mass ratio of the aniline monomer to the oxidant is 1:3-3: 1.
4. The method for preparing the composite anticorrosive coating based on interface regulation and control of claim 3, wherein the oxidant is (NH)4)2SO4Or FeCl3One kind of (1).
5. The preparation method of the composite anticorrosive coating based on interface regulation and control according to claim 1, characterized in that the weight percentage of the polyaniline-graphene oxide composite material in the composite anticorrosive coating is 1-10%.
6. The method for preparing the composite anticorrosive coating based on the interface regulation and control according to claim 1, wherein the thickness of the composite anticorrosive coating is 20 to 100 micrometers.
7. The composite anticorrosive coating based on interface regulation is characterized by being prepared by the preparation method of the composite anticorrosive coating based on interface regulation according to any one of claims 1 to 6.
8. The application of the composite anticorrosive coating based on interface regulation is characterized in that the composite anticorrosive coating based on interface regulation in claim 7 is used for metal corrosion prevention.
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