CN114517046A - Water-based epoxy coating based on divalent zinc ion modified graphene oxide and preparation method thereof - Google Patents
Water-based epoxy coating based on divalent zinc ion modified graphene oxide and preparation method thereof Download PDFInfo
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- CN114517046A CN114517046A CN202210196191.8A CN202210196191A CN114517046A CN 114517046 A CN114517046 A CN 114517046A CN 202210196191 A CN202210196191 A CN 202210196191A CN 114517046 A CN114517046 A CN 114517046A
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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
- 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 water-based epoxy coating based on divalent zinc ion modified graphene oxide and a preparation method thereof, belonging to the field of corrosion-resistant coating materials. According to the method, the pH value of a solution is regulated, zinc nitrate hexahydrate is selected as a precursor, so that the load of divalent zinc ions on graphene oxide is realized, and the modified graphene oxide filler is obtained; the filler is added into water-based epoxy and a curing agent to be mixed, and a GO @ Zn (II)/WEC coating is obtained after curing. In 3.5 wt% NaCl solution, compared with a blank waterborne epoxy coating WEC, the GO @ Zn (II)/WEC coating has the advantages that the corrosion resistance is improved by more than 2.6 times, the corrosion current density is obviously reduced, and the chlorine ion corrosion resistance of the coating is greatly enhanced. The method is simple and easy to operate, the graphene oxide loaded with divalent zinc ions improves the dispersibility of the graphene oxide in the waterborne epoxy coating, and the corrosion resistance of the waterborne epoxy coating in a seawater environment is obviously improved.
Description
Technical Field
The invention relates to the technical field of corrosion-resistant coating materials, in particular to a water-based epoxy coating based on divalent zinc ion modified graphene oxide and a preparation method thereof.
Background
Metal structures, such as steel reinforcement in concrete, which are in service for long periods in marine environments, can be contaminated with corrosive ions (e.g., Cl)-、SO4 2-、H2O, etc.) to cause severe electrochemical corrosion, which leads to the reduction of the structural strength of the ocean engineering, the shortening of the service life and huge economic loss.
The coating of the environment-friendly water-based epoxy resin coating is one of effective methods for coping with the corrosion of the steel bar in the concrete. However, WEC itself is less dense, and generates a large number of microscopic defects such as voids and fine lines during the construction and application processes, providing diffusion channels for corrosive components, so that the physical barrier properties of the coating are not ideal. The problem of coating compactness can be solved by adding fillers, and a plurality of fillers based on graphene oxide modification are invented and published at present. However, the synthesis steps are complicated, and the harsh conditions requiring high temperature and even high pressure are often present. Therefore, the development and preparation of the water-based epoxy coating with simplicity and remarkable effect can improve the WEC compactness and further enhance the corrosion protection performance of the coating, and the water-based epoxy coating is a bottleneck problem to be broken through urgently in the epoxy coating industry.
Disclosure of Invention
Aiming at the problems that the aqueous epoxy coating adopted by the prior art is poor in compactness and cannot effectively prevent corrosive media from diffusing to a metal substrate, and the coating cannot spontaneously generate a repairing function at a corroded part after being damaged so as to block a corrosion process, the invention provides the aqueous epoxy coating based on the divalent zinc ion modified graphene oxide and the preparation method thereof, and the anticorrosive coating with excellent anticorrosive performance and better anticorrosive effect is prepared.
In order to realize the purpose, the technical scheme adopted by the invention is as follows:
an anticorrosive waterborne epoxy coating based on divalent zinc ion modified graphene oxide, which is prepared from waterborne epoxy resin, a curing agent and a filler, wherein: the filler is based on zinc nitrate hexahydrate modified graphene oxide, and the filler contains divalent zinc ions.
In the raw materials of the water-based epoxy coating, the filler accounts for 0.07-0.11 wt% (preferably 0.07-0.09 wt.%), and the weight ratio of the water-based epoxy resin to the curing agent is 3: 10-6: 10.
the curing agent is an aliphatic amine curing agent.
According to the method, firstly, zinc nitrate hexahydrate and graphene oxide are subjected to electrostatic self-assembly to obtain a filler, then the filler and a curing agent are added into aqueous epoxy resin according to a proportion, and the aqueous epoxy resin is uniformly mixed and coated on a low-alloy steel substrate to obtain the aqueous epoxy coating.
The preparation process of the filler GO @ Zn (II) comprises the following steps:
(1) adding 5-15 ml of graphene oxide solution (GO) with the concentration of 1.0-2.5mg/ml into 100-180 ml of deionized water, and performing ultrasonic dispersion for 10-20 minutes;
(2) Slowly dripping 0.1mol/L NaOH solution into the graphene oxide solution subjected to ultrasonic dispersion treatment in the step (1), and adjusting the pH of the solution to 7.5-9;
(3) adding 250-350 mg of zinc nitrate hexahydrate Zn (NO) into the solution with the pH value adjusted in the step (2)3)2·6H2O, magnetically stirring for 1-1.5 hours at 500-800 rpm to fully react;
(4) and (4) washing the reaction product obtained in the step (3) by using deionized water, wherein the rotating speed of a centrifugal machine is 10000r/min, the centrifugal time is 3min, and the obtained solid material is the filler after the centrifugal product is dried in an oven.
The preparation process of the water-based epoxy coating comprises the following specific steps:
uniformly dispersing the filler in deionized water, adding the filler into a mixed solution (3: 10-6: 10) of water-based epoxy resin and a curing agent, stirring, and standing for 15-30 minutes to ensure that bubbles in the mixed solution escape sufficiently to obtain a coating mixed solution; and uniformly coating the prepared coating mixed solution on the surface of a low-alloy steel substrate which is polished with No. 2000 abrasive paper step by using a fine and soft brush pen, and standing at room temperature for curing for 8-12 h to obtain the water-based epoxy coating.
The invention has the following advantages:
1. the graphene oxide composite filler GO @ Zn (II) modified based on zinc nitrate hexahydrate is prepared by a coprecipitation method at normal temperature, the process is simple and easy to operate, and the precursor is low in cost.
2. In the filler, because the Graphene Oxide (GO) is loaded with divalent zinc ions, the divalent zinc ions stored on the surface of GO can react with corrosion products to generate Zn (OH) rich when a substrate is corroded2The protective film layer plays a role in protecting a corrosion area through a corrosion inhibitor reaction mechanism, and improves the corrosion resistance and the self-repairing function of the coating. In addition, the graphene oxide has good physical shielding performance and generates a synergistic effect with divalent zinc ions, so that the water-based epoxy coating has excellent corrosion resistance.
3. In 3.5 wt% NaCl solution, compared with a blank waterborne epoxy coating WEC, the GO @ Zn (II)/WEC coating has the advantages that the corrosion resistance is improved by more than 2.6 times, the corrosion current density is obviously reduced, and the capability of the coating for resisting chloride ion corrosion is greatly enhanced. The method is simple and easy to operate, the graphene oxide loaded with divalent zinc ions improves the dispersibility of the graphene oxide in the waterborne epoxy coating, and the corrosion resistance of the waterborne epoxy coating in a seawater environment is obviously improved.
Drawings
Fig. 1 is a modified graphene oxide filler based on zinc nitrate hexahydrate in example 1; wherein: (a) SEM picture; (b) EDX diagram.
Figure 2 is an infrared absorption spectrum FTIR of unmodified graphene oxide and the graphene oxide filler modified based on zinc nitrate hexahydrate in example 1.
Fig. 3 is an open circuit potential OCP of 0.08 wt.% addition of a graphene oxide filler modified based on zinc nitrate hexahydrate aqueous epoxy coating GO @ zn (ii)/WEC in example 1, 0.08 wt.% addition of a graphene oxide aqueous epoxy coating GO/WEC in comparative example 2, and an aqueous epoxy coating WEC in comparative example 1 soaked in a 3.5 wt.% NaCl solution for 0.5 h.
FIG. 4 is an AC impedance plot after 0.08 wt.% addition of a graphene oxide filler modified based on zinc nitrate hexahydrate, aqueous epoxy coating GO @ Zn (II)/WEC in example 1, 0.08 wt.% addition of a graphene oxide aqueous epoxy coating GO/WEC in comparative example 2, and an aqueous epoxy coating WEC in comparative example 1 soaked in a 3.5 wt.% NaCl solution for 0.5 h; wherein: (a) a Nyquist plot; (b) bode diagram.
Fig. 5 is a steady state polarization curve after soaking 0.08 wt.% of the graphene oxide filler modified based on zinc nitrate hexahydrate aqueous epoxy coating GO @ zn (ii)/WEC in example 1, 0.08 wt.% of the graphene oxide aqueous epoxy coating GO/WEC in comparative example 2, and the aqueous epoxy coating WEC in comparative example 1 in 3.5 wt.% NaCl solution for 1 h.
Detailed Description
The invention is further illustrated below with reference to specific embodiments. It is to be understood that the present invention is not limited to the following embodiments, which are regarded as conventional methods unless otherwise specified. The materials are commercially available from the open literature unless otherwise specified.
The invention provides an anticorrosive paint based on zinc nitrate hexahydrate modified graphene and a preparation method thereof, wherein the method comprises the following steps: adding zinc nitrate hexahydrate and graphene oxide into water, and reacting at normal temperature after uniform dispersion to obtain modified graphene; and dispersing the modified graphene into deionized water, adding the deionized water into a mixed solution of resin and a curing agent, and uniformly dispersing to obtain a coating mixed solution based on the divalent zinc ion modified graphene oxide. And coating the coating mixed solution on the surface of the metal substrate, and curing at normal temperature to form a film to obtain the metal anticorrosive coating.
Preferably, the addition amount of the modified graphene oxide in the coating is 0.07 wt% to 0.11 wt%.
Preferably, the divalent zinc ion precursor in the preparation process of the modified graphene oxide is zinc nitrate hexahydrate.
When the coating is prepared, when the filler is dispersed in deionized water, the ratio of the total weight of the waterborne epoxy and the curing agent to the deionized water is (1.5-2.5 g): 1 mL.
The invention comprehensively utilizes the film forming effect of divalent zinc ions and the shielding function of graphene oxide, prepares the composite filler by an electrostatic self-assembly method, and further constructs a novel strong corrosion-resistant self-repairing waterborne epoxy coating-GO @ Zn (II)/WEC.
The curing agents in the following examples and comparative examples are aliphatic amine-based curing agents.
Comparative example 1:
this example is WEC coating preparation, procedure is as follows:
1ml of deionized water, 0.761g of waterborne epoxy and 1.369 of curing agent are mixed and stirred for 10 minutes for mixing, the mixture is kept stand for 20 minutes to discharge bubbles mixed in the stirring, then the mixture is coated on the surface of the polished 20SiMn steel by a brush pen, and the mixture is solidified for 8 hours at room temperature to obtain the WEC coating.
Comparative example 2:
this example is the GO/WEC coating preparation, the procedure is as follows:
and adding 0.761g of water-based epoxy and 1.369 curing agent into 1.25mL of graphene oxide solution with the concentration of 2mg/mL, stirring for 10 minutes, standing for 20 minutes, coating the surface of the polished 20SiMn steel by using a brush pen, and solidifying for 8 hours at room temperature to obtain the GO/WEC coating.
Example 1:
this example is a GO @ Zn (II)/WEC coating preparation, as follows:
and adding 10ml of 2mg/ml GO solution into 100ml of deionized water, performing ultrasonic dispersion for 15min, and dropwise adding 0.1mol/L NaOH solution to adjust the pH value of the GO solution to 8.0. 150mg Zn (NO) was added3)2·6H2O, stirring at 560rmp for 1h at room temperature. And after the reaction is finished, ultrasonically cleaning the mixture by using deionized water for 10 minutes, centrifugally separating the mixture for 3 minutes at 10000r/min by using a centrifugal machine, and repeatedly cleaning the mixture for 3 times to obtain the GO @ Zn (II) filler.
2.5mg of the GO @ Zn (II) filler obtained above is put into 1ml of deionized water, and after 15min of ultrasonic dispersion, the filler is mixed with 2.13g of mixed liquid of waterborne epoxy and curing agent (the weight ratio of the waterborne epoxy to the curing agent in the mixed liquid is 5: 9) to be uniformly stirred and kept stand for 20 min. Coating the surface of the polished 20SiMn steel by using a brush pen, and solidifying for 8 hours at room temperature to obtain GO @ Zn (II)/WEC.
Example 2:
this example is a GO @ Zn (II)/WEC coating preparation, as follows:
adding 15ml of GO solution with the concentration of 2mg/ml into 100ml of deionized water, performing ultrasonic dispersion for 15min, and dropwise adding 0.1mol/L NaOH solution to adjust the pH value of the GO solution to 8.5. Adding 200mg Zn (NO)3)2·6H2O, stirring at room temperature for 1h at 800 rmp. And after the reaction is finished, ultrasonically cleaning the mixture by using deionized water for 10 minutes, centrifugally separating the mixture for 3 minutes at 10000r/min by using a centrifugal machine, and repeatedly cleaning the mixture for 3 times to obtain the GO @ Zn (II) filler.
2.0mg of the GO @ Zn (II) filler obtained above is put into 1ml of deionized water, and after ultrasonic dispersion for 15min, the filler is mixed with 3g of mixed liquid of water-based epoxy and curing agent (the weight ratio of the water-based epoxy to the curing agent in the mixed liquid is 5: 10), and the mixture is stirred uniformly and stands for 20 min. Coating the polished 20SiMn steel surface by a brush pen, and solidifying for 8h at room temperature to obtain GO @ Zn (II)/WEC.
As shown in fig. 1(a), which is an SEM image of the modified graphene oxide filler used in the present invention, it can be seen that the lamellar graphene oxide in the present invention contains a large amount of lamellar solid substances due to zn (ii) supported on the surface thereof.
EDS data in FIG. 1(b) shows that GO @ Zn (II) filler contains Zn element but NO N element, illustrating NO in the precursor3 2-Is cleaned, and Zn (II) realizes the modification of GO through reaction.
Fig. 2 is a TEM image of modified graphene oxide, in which it is clearly seen that nanoparticles, zn (ii), formed as shown in fig. 1a, are mostly concentrated at 30nm in diameter, and the wrinkled and translucent material is graphene oxide.
FIG. 3 is an infrared absorption spectrum of GO @ Zn (II) filler synthesized in example 1 of this technology, indicating that GO @ Zn (II) has Zn (OH) which is not present in GO originally2Peak (2850 cm)-1,1920cm-1) Zn (II) from the precursor; while the C-H peak in the GO molecule (1220 cm)-1) Disappearance in the synthesized GO @ Zn (II) filler proves that the Zn (II) product is grafted on GO molecules by replacing H protons of C-H at GO edges to realize the modification of GO.
FIG. 4 shows the open circuit potential OCP of three coatings, comparative example 1WEC, comparative example 2GO/WEC and example 1GO @ Zn (II)/WEC, immersed in a 3.5 wt.% solution for 30 minutes, indicating that the WEC potential is stable at around-0.22V, while the GO/WEC coating is stable at around-0.28V and the GO @ Zn (II)/WEC at-0.164V. As the potential is more negative and the corrosion tendency is larger, the GO added with WEC can not improve the corrosion resistance but increase the corrosion tendency, and the GO @ Zn (II)/WEC synthesized by the invention can reduce the corrosion resistance tendency of the coating.
FIG. 4(a) Nyquist plot of the higher impedance spectrum radius of the WEC in comparative example 1 than the GO/WEC coating in comparative example 2, but significantly less than the GO @ Zn (II)/WEC of example 1, and FIG. 4(b) Bode plot shows that the lowest frequency impedance of the WEC coating is 2.1X 105Ω.cm2GO/WEC coating of 0.88X 105Ω.cm2GO @ Zn (II)/WEC coatings of up to 4.5X 105Ω.cm2The method shows that the GO filler is added into the waterborne epoxy coating to reduce the corrosion resistance of the coating, and the modified graphene oxide coating synthesized by the method greatly improves the chlorine ion corrosion resistance of the waterborne epoxy coating.
The potentiodynamic polarization curve in FIG. 5 shows that the corrosion current density of the WEC coating after 1h soaking in a 3.5 wt.% solution is about 2X 10-7A.cm-2Less than 4X 10 of GO/WEC coatings-7A.cm-2Much greater than GO @ Zn (II)/WEC coatings of 9X 10- 8A.cm-2The modified graphene oxide synthesized by the method can obviously enhance the corrosion resistance of the waterborne epoxy coating and can generate a better protection effect on a matrix.
Claims (9)
1. A waterborne epoxy coating based on divalent zinc ion modified graphene oxide is characterized in that: the water-based epoxy coating consists of water-based epoxy resin, a curing agent and a filler, wherein: the filler is divalent zinc ion modified graphene oxide.
2. The waterborne epoxy coating based on divalent zinc ion-modified graphene oxide according to claim 1, wherein: in the waterborne epoxy coating, the filler accounts for 0.07-0.11 wt%, and the weight ratio of the waterborne epoxy resin to the curing agent is 3: 10-6: 10.
3. the divalent zinc ion modified graphene oxide based waterborne epoxy coating according to claim 1, wherein: the curing agent is aliphatic amine curing agent.
4. The method for preparing the waterborne epoxy coating based on the divalent zinc ion modified graphene oxide according to claim 1, wherein the method comprises the following steps: the method comprises the steps of firstly, carrying out electrostatic self-assembly on zinc nitrate hexahydrate and graphene oxide to obtain a filler, then adding the filler and a curing agent into waterborne epoxy resin according to a proportion, uniformly mixing, and then coating on a low-alloy steel substrate to obtain the waterborne epoxy coating.
5. The method for preparing the waterborne epoxy coating based on the divalent zinc ion modified graphene oxide according to claim 4, wherein: the preparation process of the filler GO @ Zn (II) comprises the following steps:
(1) adding 5-15 ml of graphene oxide solution (GO) with the concentration of 1.0-2.5mg/ml into 100-180 ml of deionized water, and performing ultrasonic dispersion for 10-20 minutes;
(2) Slowly dripping a NaOH solution into the graphene oxide solution subjected to ultrasonic dispersion treatment in the step (1), and adjusting the pH of the solution to 7.5-9;
(3) adding 250-350 mg of zinc nitrate hexahydrate Zn (NO) into the solution with the pH value adjusted in the step (2)3)2·6H2O, fully reacting under the stirring condition;
(4) and (4) washing the reaction product obtained in the step (3) by using deionized water, and drying the product in an oven after centrifugation to obtain the solid material, namely the filler.
6. The method for preparing the waterborne epoxy coating based on the divalent zinc ion modified graphene oxide according to claim 5, wherein the method comprises the following steps: in the step (1), the concentration of the NaOH solution is 0.1 mol/L.
7. The zinc alloy according to claim 5, which is based on divalent zincThe preparation method of the water-based epoxy coating of the ion-modified graphene oxide is characterized by comprising the following steps: in the step (3), Zn (NO) is added into the solution3)2·6H2And after O, magnetically stirring for 1-1.5 h at a magnetic stirring speed of 500-800 rpm.
8. The method for preparing the waterborne epoxy coating based on the divalent zinc ion modified graphene oxide according to claim 5, wherein the method comprises the following steps: in the step (4), when deionized water is adopted for washing, the rotating speed of a centrifugal machine is 10000r/min, and the centrifugal time is 3 min.
9. The method for preparing the waterborne epoxy coating based on the divalent zinc ion modified graphene oxide according to claim 4, wherein: the preparation process of the water-based epoxy coating is as follows:
Uniformly dispersing the filler in deionized water, adding the filler into a mixed solution of waterborne epoxy resin and a curing agent, stirring (wherein the ratio of waterborne epoxy to the curing agent is 3: 10-6: 10), standing for 15-30 minutes to ensure that bubbles in the mixed solution escape sufficiently, and thus obtaining a coating mixed solution; and uniformly coating the prepared coating mixed solution on the surface of a low-alloy steel substrate which is polished with No. 2000 abrasive paper step by using a fine and soft brush pen, and standing at room temperature for curing for 8-12 hours to obtain the water-based epoxy coating.
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