CN109909131B - Preparation method of graphene-based steel anticorrosive coating - Google Patents
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Abstract
The invention discloses a preparation method of a graphene-based steel anticorrosive coating, and relates to a preparation method of a graphene-based anticorrosive coating with excellent isolation and barrier effects on aggressive media. The invention aims to effectively solve the problem that the anticorrosion effect of the anticorrosion coating of the built steel structure is poor in the high-salinity seawater environment. According to the invention, the steel surface is subjected to oil and rust removal and polishing treatment, then the polished steel surface is coated with a layer of epoxy resin coating by using the underwater cured epoxy resin, and then the silane coupling agent, the silane coupling agent water-based graphene composite layer and the oily graphene layer are adopted for transition process, so that the anticorrosive coating with excellent anticorrosive performance, which can be applied in tidal zones, splash zones and high-humidity environments, is obtained, and the effects of increasing the self-corrosion potential by 100mV and reducing the corrosion current density by 1 order of magnitude can be realized by using the single-pass graphene-based steel anticorrosive coating. The invention can be applied to the field of civil engineering.
Description
Technical Field
The invention relates to a preparation method of a graphene-based steel anticorrosive coating.
Background
In the present and future development time, steel structures have played an extremely important role as an important structural form in the field of building construction and civil engineering, while their corrosion resistance is also critical in determining their service life. In recent years, China has been built up on a large scale of cross-sea bridges, steel structures for the sea and coastal infrastructures, the demand of steel for military ships and naval vessels is increased obviously, and the quantity of steel which cannot be used due to corrosion and scrapping of the steel is increased, so that huge national economic loss is caused. In steel and reinforced concrete structures in coastal environments, the contact of corrosion factors such as chloride ions, water molecules, oxygen molecules and the like with the surface of a steel substrate is the most main reason for causing corrosion and reducing the durability of the steel substrate. The steel is corroded by natural corrosion factors, such as oxygen and water. Therefore, the research on the corrosion resistance and durability of the steel under the action of the coastal high-salinity seawater corrosion environment is always a hot spot at home and abroad. However, the prior heavy anti-corrosive paint has poor using effect on a high-salinity seawater steel structure, and is not suitable for the field construction of the anti-corrosive paint of the built steel structure because most of the prior heavy anti-corrosive paint needs to be constructed under the condition of drying the surface of the steel structure.
Disclosure of Invention
The invention aims to solve the problem that an anticorrosive coating of a steel structure is poor in anticorrosive effect in a high-salinity seawater environment, and provides a preparation method of a graphene-based steel anticorrosive coating.
The preparation method of the graphene-based steel anticorrosive coating is carried out according to the following steps:
the method comprises the following steps: carrying out oil and rust removal treatment on the surface of the steel, and then polishing the surface of the steel to be bright by using a polishing machine;
step two: coating a layer of underwater curing epoxy resin coating with the thickness of 10-30 mu m on the surface of the polished steel, and then solidifying and forming;
step three: diluting a silane coupling agent by using distilled water, wherein the volume concentration of the diluted silane coupling agent is 10-20%, and the dilution time is 10-20min, and then putting the diluted silane coupling agent into a constant-temperature water bath kettle at 25-50 ℃ for later use;
step four: ultrasonically dispersing the aqueous graphene solution for 15-30 min for later use;
step five: mixing the silane coupling agent diluted in the third step and the water-based graphene dispersed in the fourth step according to the volume ratio of 1:1, and stirring to obtain a black uniform mixed solution for later use;
step six: putting the steel obtained in the step two into the mixed solution obtained in the step five, soaking for 15-30 min, taking out, and putting into a drying oven at 80-100 ℃ for drying for 2-4 h for later use;
step seven: and C, coating a layer of uniform oily graphene with the thickness of 10-20 microns on the coating obtained in the step six, and then drying the coating in a drying oven at the temperature of 80-100 ℃ for 2-4 hours to finish the coating of the graphene-based steel anticorrosive coating.
The Kh550 silane coupling agent and the water-based graphene are mixed to obtain a uniformly dispersed mixture, so that a transition layer tightly combined with the underwater cured epoxy resin is formed; oily graphene with different polarity from a seawater environment is used as a surface layer, so that the spreading of an environmental medium on the surface of the coating is reduced; the water-based graphene and the oily graphene coating act together, so that the shielding effect of the coating on an aggressive medium is enhanced, and the anticorrosion effect of the graphene anticorrosion coating can be further improved by increasing the number of coating tracks of the underwater cured epoxy resin/silane coupling agent water-based graphene coating.
The invention has the following advantages: the invention carries out oil and rust removal and polishing treatment on the surface of steel, then uses water-based cured epoxy resin to coat a layer of epoxy resin coating on the polished surface of the steel, and then adopts a silane coupling agent, a silane coupling agent water-based graphene composite layer and an oily graphene layer transition process to obtain an anticorrosive coating which can be applied in tidal areas, splash areas and high-humidity environments and has excellent anticorrosive performance, thereby being capable of being constructed on site aiming at the constructed steel structure.
The graphene-based coating process can solve the problem that the graphene-based coating is not good enough in adhesion on the surface of steel, and the problem that graphene only forms van der Waals force and poor hydrogen bonding force on the bonding surface of the steel substrate directly, so that reliable covalent bonds and chemical bonds are formed, and the stable bonding force between the graphene-based coating and the steel substrate is increased. Compared with the traditional process, the method can solve the problem of surface moisture of the steel structure matrix caused by water fluctuation and tide in the ocean tide area, can stably cure the steel structure matrix on the surface of an underwater environment by using the underwater curing epoxy resin, and can prevent factors such as underwater chloride ions, oxygen molecules in air, water molecules and the like which accelerate the corrosion of the steel matrix from reaching the surface of the base material to play a certain protection role. The heavy anti-corrosion coating doped with graphene in the current market mostly utilizes the dispersibility and the barrier property of a graphene sheet layer to increase the path of a corrosion medium factor to reach the surface of a base material, but the barrier property of the graphene sheet layer is not utilized, the graphene-based coating process of the three-layer composite transition coating provided by the invention can enable the graphene sheet layer to cover the surface of a steel block base material, and utilizes the barrier property of the graphene sheet layer to isolate the corrosion medium factor, so that the corrosion resistance of steel can be greatly increased, and the effects of improving the self-corrosion potential by 100mV and reducing the corrosion current density by 1 order of magnitude can be realized by a single graphene-based steel anti-corrosion coating. Obviously, the anticorrosive effect can be further obviously improved by the plurality of graphene-based steel anticorrosive coatings.
The invention obviously improves the corrosion resistance of steel, and can be constructed in a high-humidity environment to obtain the corrosion-resistant coating with excellent performance for coastal, cross-sea bridges, tunnels and other projects, no matter the structures are built or newly built.
Drawings
FIG. 1 is a graphene-based steel corrosion-resistant coating;
FIG. 2 is a surface appearance of a steel test piece 10h in a salt spray test of a steel test piece without an anticorrosive coating;
FIG. 3 is a surface morphology of a steel test piece in 10h of the salt spray test of the steel test piece in comparative test 1;
FIG. 4 is a surface topography of a steel test piece in 10h of the salt spray test of the steel test piece in test 1;
FIG. 5 is a scanning electron microscope of the anticorrosive coating of single-pass graphene-based steel prepared in test 1;
FIG. 6 is a scanning electron microscope of the three graphene-based steel anticorrosive coatings of comparative test 2;
FIG. 7 is Tafel polarization curves for a steel test piece without an anti-corrosion coating and a steel test piece with a graphene-based steel anti-corrosion coating in test 1; wherein a is a steel test piece without an anti-corrosion coating, and b is a steel test piece with a graphene-based steel anti-corrosion coating in test 1;
FIG. 8 shows the effect of the scribing test with the graphene-based steel anticorrosive coating in test 1.
Detailed Description
The first embodiment is as follows: the preparation method of the graphene-based steel anticorrosive coating is carried out according to the following steps:
the method comprises the following steps: carrying out oil and rust removal treatment on the surface of the steel, and then polishing the surface of the steel to be bright by using a polishing machine;
step two: coating a layer of underwater curing epoxy resin coating with the thickness of 10-30 mu m on the surface of the polished steel, and then solidifying and forming;
step three: diluting a silane coupling agent by using distilled water, wherein the volume concentration of the diluted silane coupling agent is 10-20%, and the dilution time is 10-20min, and then putting the diluted silane coupling agent into a constant-temperature water bath kettle at 25-50 ℃ for later use;
step four: ultrasonically dispersing the aqueous graphene solution for 15-30 min for later use;
step five: mixing the silane coupling agent diluted in the third step and the water-based graphene dispersed in the fourth step according to the volume ratio of 1:1, and stirring to obtain a black uniform mixed solution for later use;
step six: putting the steel obtained in the step two into the mixed solution obtained in the step five, soaking for 15-30 min, taking out, and putting into a drying oven at 80-100 ℃ for drying for 2-4 h for later use;
step seven: and C, coating a layer of uniform oily graphene with the thickness of 10-20 microns on the coating obtained in the step six, and then drying the coating in a drying oven at the temperature of 80-100 ℃ for 2-4 hours to finish the coating of the graphene-based steel anticorrosive coating.
This embodiment has the following advantages: according to the embodiment, the steel surface is subjected to oil and rust removal and polishing treatment, then the polished steel surface is coated with a layer of epoxy resin coating by using the underwater curing epoxy resin, and then the anticorrosion coating which can be applied to tidal zones, splash zones and high-humidity environments and has excellent anticorrosion performance is obtained by adopting the silane coupling agent, the silane coupling agent aqueous graphene composite layer and the oily graphene layer transition process.
The graphene-based coating process described in the embodiment can solve the problem that the graphene-based coating is not well adhered to the surface of the steel material, and the problem that graphene directly forms only van der waals force and poor hydrogen bonding force on the bonding surface of the steel material substrate, so that reliable covalent bonds and chemical bonds are formed, and the stable bonding force between the graphene-based coating and the steel material substrate is increased. Compared with the traditional process, the method can solve the problem of surface moisture of the steel structure matrix caused by water fluctuation and tide in the ocean tide area, can stably cure the steel structure matrix on the surface of an underwater environment by using the underwater curing epoxy resin, and can prevent factors such as underwater chloride ions, oxygen molecules in air, water molecules and the like which accelerate the corrosion of the steel matrix from reaching the surface of the base material to play a certain protection role. The graphene-doped heavy anti-corrosion coating and the like in the current market mostly utilize the dispersibility and the barrier property of a graphene sheet layer to increase the path of a corrosion medium factor to reach the surface of a base material, but the barrier property of the graphene sheet layer is not utilized, the graphene-based coating process of the three-layer composite transition coating provided by the invention can enable the graphene sheet layer to cover the surface of a steel block base material, and isolate the corrosion medium factor by utilizing the barrier property of the graphene sheet layer, so that the steel anti-corrosion performance is greatly improved, and the effects of improving the self-corrosion potential by 100mV and reducing the corrosion current density by 1 order of magnitude can be realized by a single graphene-based steel anti-corrosion coating. Obviously, the anticorrosive effect can be further obviously improved by the plurality of graphene-based steel anticorrosive coatings.
The embodiment obviously improves the corrosion resistance of steel, and can be used for construction in a high-humidity environment to obtain a corrosion-resistant coating with excellent performance for coastal, cross-sea bridges, tunnels and other projects, no matter the structures are built or newly built.
The second embodiment is as follows: the first difference between the present embodiment and the specific embodiment is: the underwater curing epoxy resin is prepared from a component A and a component B according to the mass ratio of 100 (20-35), wherein the component A is epoxy resin, and the component B is an underwater curing agent. The rest is the same as the first embodiment.
The third concrete implementation mode: the present embodiment differs from the first or second embodiment in that: the underwater curing epoxy resin is prepared from a component A and a component B according to the mass ratio of 100: 21. The others are the same as in the first or second embodiment.
The fourth concrete implementation mode: the difference between this embodiment mode and one of the first to third embodiment modes is: the component A is bisphenol F epoxy resin, bisphenol A epoxy resin, novolac epoxy resin or o-cresol epoxy resin. The rest is the same as one of the first to third embodiments.
The fifth concrete implementation mode: the difference between this embodiment and one of the first to fourth embodiments is: the component B is polyamide curing agent, aliphatic amine curing agent or phenolic amine curing agent. The rest is the same as one of the first to fourth embodiments.
The sixth specific implementation mode: the difference between this embodiment and one of the first to fifth embodiments is: the method for removing oil and rust on the surface of steel comprises the following steps: adopting absorbent cotton to dip and analyze pure alcohol, and wiping the surface of the steel until no floating rust trace exists; then, the steel is ultrasonically cleaned for 10min by deionized water. The rest is the same as one of the first to fifth embodiments.
The seventh embodiment: the difference between this embodiment and one of the first to sixth embodiments is: the silane coupling agent is Kh550 silane coupling agent. The rest is the same as one of the first to sixth embodiments.
The specific implementation mode is eight: the present embodiment differs from one of the first to seventh embodiments in that: and step four, performing ultrasonic dispersion under the conditions of 150-200W and 40 kHz. The rest is the same as one of the first to seventh embodiments.
The specific implementation method nine: the present embodiment differs from the first to eighth embodiments in that: and the drying in the sixth step and the seventh step is drying for 2-4 h in a drying oven at the temperature of 80-100 ℃. The rest is the same as the first to eighth embodiments.
The following examples were used to demonstrate the beneficial effects of the present invention:
test 1: the preparation method of the graphene-based steel anticorrosive coating comprises the following steps:
the method comprises the following steps: processing 3c x 2cm3Steel test piece, test piece tableCarrying out oil and rust removal treatment on the surface, and then polishing the surface to be bright by using a polishing machine to expose the fresh surface of the steel;
step two: coating a layer of epoxy resin coating with the thickness of 15 mu m on the surface of the test piece, and then solidifying and forming the test piece;
step three: diluting a Kh550 silane coupling agent by using distilled water, wherein the volume concentration of the diluted silane coupling agent is 20%, and then putting the diluted silane coupling agent into a constant-temperature water bath kettle at 25 ℃ for later use;
step four: dispersing the aqueous graphene solution for later use by ultrasonic dispersion of 180W and 40kHz for 15min, wherein the aqueous graphene solution is a commercialized product from Nanjing Xiancheng nanometer material science and technology Limited;
step five: mixing the Kh550 silane coupling agent obtained in the step three and the water-based graphene dispersed in the step four according to the volume ratio of 1:1, and stirring to obtain a black uniform mixed solution for later use;
step six: placing the test piece obtained in the step two into the mixed solution obtained in the step five, soaking for 25min, taking out, and placing into a drying oven at 80 ℃ for drying for 2h for later use;
step seven: and (3) coating a layer of uniform oily graphene with the thickness of 15 mu m on the surface of the test piece obtained in the sixth step, and drying the test piece in a drying box at the temperature of 80 ℃ for 2 hours to finally obtain the graphene-based steel anticorrosive coating shown in the figure 1, wherein the oily graphene is a commercial product purchased from Nanjing Xiancheng nanometer material science and technology Limited company.
By adopting the first embodiment of the invention, the underwater cured epoxy resin/silane coupling agent and aqueous graphene composite/oily graphene three-layer graphene-based anticorrosive coating shown in fig. 1 is prepared on the surface of a steel test piece. As can be seen from FIG. 1, the method of the present invention can obtain a dense graphene-based anticorrosive coating on the surface of steel.
For the effect of contrast anticorrosive coating, this experiment has set up the contrast test:
comparative experiment 1 was carried out as follows:
the method comprises the following steps: processing 3c x 2cm3The surface of the steel test piece is subjected to oil and rust removal treatment, and then the surface is polished to be bright by a polishing machine, so that the fresh surface of the steel is exposed;
step two: coating a layer of epoxy resin coating with the thickness of 15 mu m on the surface of the test piece, and then solidifying and forming the test piece;
step three: diluting a Kh550 silane coupling agent by using distilled water, wherein the volume concentration of the diluted silane coupling agent is 20%, and then putting the diluted silane coupling agent into a constant-temperature water bath kettle at 25 ℃ for later use;
step four: dispersing the aqueous graphene solution for later use by ultrasonic dispersion of 180W and 40kHz for 15min, wherein the aqueous graphene solution is a commercialized product from Nanjing Xiancheng nanometer material science and technology Limited;
step five: mixing the Kh550 silane coupling agent obtained in the step three and the water-based graphene dispersed in the step four according to the volume ratio of 1:1, and stirring to obtain a black uniform mixed solution for later use;
step six: and (4) placing the test piece obtained in the step two into the mixed solution obtained in the step five, soaking for 25min, taking out, and placing into a drying oven at 80 ℃ for drying for 2h to obtain the test piece coated with two layers of water-based graphene coatings.
Comparative experiment 2 was carried out as follows:
the method comprises the following steps: processing 3c x 2cm3The surface of the steel test piece is subjected to oil and rust removal treatment, and then the surface is polished to be bright by a polishing machine, so that the fresh surface of the steel is exposed;
step two: coating a layer of epoxy resin coating with the thickness of 15 mu m on the surface of the test piece, and then solidifying and forming the test piece;
step three: diluting a Kh550 silane coupling agent by using distilled water, wherein the volume concentration of the diluted silane coupling agent is 20%, and then putting the diluted silane coupling agent into a constant-temperature water bath kettle at 25 ℃ for later use;
step four: dispersing the aqueous graphene solution for later use by using ultrasonic of 150-plus-200W and 40kHz for 15min, wherein the aqueous graphene solution is a commercialized product purchased from Nanjing Xiancheng nanometer material science and technology Limited;
step five: mixing the Kh550 silane coupling agent obtained in the step three and the water-based graphene dispersed in the step four according to the volume ratio of 1:1, and stirring to obtain a black uniform mixed solution for later use;
step six: placing the test piece obtained in the step two into the mixed solution obtained in the step five, soaking for 25min, taking out, and placing into a drying oven at 80 ℃ for drying for 2h for later use;
step seven: coating a layer of uniform oily graphene with the thickness of 15 mu m on the surface of the test piece obtained in the sixth step, and drying the test piece in a drying box at the temperature of 80 ℃ for 2 hours;
step eight: repeating the operation of the second step to the seventh step twice to obtain the test piece coated with the three graphene-based steel anticorrosive coatings.
The underwater curing epoxy resin in the test 1 and the comparative tests 1 and 2 is prepared from a component A and a component B according to the mass ratio of 100:21, wherein the component A is bisphenol A epoxy resin, and the component B is aliphatic amine curing agent.
Tests 1, comparative tests 1 and comparative tests 2 were carried out according to the GBT10125-2012 salt spray test standard, and fig. 2-4 show the surface topography of three steel test pieces under the action of 10h salt spray. The corrosion-free coated steel test piece shown in fig. 2 was corroded more severely by the electrochemical corrosion action of the salt spray. The test pieces of comparative test 1 shown in fig. 3 resulted in overall failure of the coating due to hydrolysis by the salt spray. The steel test piece of the underwater curing epoxy resin/silane coupling agent and aqueous graphene composite/oily graphene three-layer graphene-based anticorrosive coating prepared by the test 1 shown in fig. 4 has good coating surface integrity, no local damage and excellent anticorrosive performance.
In order to further inspect the surface state of the graphene anticorrosive coating, the surfaces of the single-pass graphene-based steel anticorrosive coating prepared in the test 1 and the three-pass graphene-based steel anticorrosive coating prepared in the comparative test 2 were observed by using an electronic scanning electron microscope, and the results are shown in fig. 5 and 6. As can be seen from fig. 5 and 6, the graphene anti-corrosion coating prepared by the single process and the three processes has no obvious wrinkle phenomenon on the surface of the coating, which indicates that the anti-corrosion coating has been flattened and tightly overlapped, and can effectively prevent erosion particles from entering.
The corrosion protection effect of the graphene anti-corrosion coating is tested and compared by adopting a potentiodynamic scanning method, and the result is shown in fig. 7. As shown in fig. 7, the single-pass graphene-based steel anticorrosive coating prepared in test 1 can achieve the effects of increasing the self-corrosion potential by 100mV and reducing the corrosion current density by 1 order of magnitude.
In order to examine the performance of the graphene anticorrosive coating more fully, a scribing test is performed on the single-pass graphene-based steel anticorrosive coating prepared in the test 1, and the result is shown in fig. 8. Compared with the ASTM D3359 coating adhesion standard, the adhesion of the graphene anticorrosive coating to steel reaches the highest 5B grade.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (8)
1. A preparation method of a graphene-based steel anticorrosive coating is characterized by comprising the following steps:
the method comprises the following steps: carrying out oil and rust removal treatment on the surface of the steel, and then polishing the surface of the steel to be bright by using a polishing machine;
step two: coating a layer of underwater curing epoxy resin coating with the thickness of 10-30 mu m on the surface of the polished steel, and then solidifying and forming;
step three: diluting a silane coupling agent by using distilled water, wherein the volume concentration of the diluted silane coupling agent is 10-20%, and the dilution time is 10-20min, and then putting the diluted silane coupling agent into a constant-temperature water bath kettle at 25-50 ℃ for later use;
step four: ultrasonically dispersing the aqueous graphene solution for 15-30 min for later use;
step five: mixing the silane coupling agent diluted in the third step and the water-based graphene dispersed in the fourth step according to the volume ratio of 1:1, and stirring to obtain a black uniform mixed solution for later use;
step six: putting the steel obtained in the step two into the mixed solution obtained in the step five, soaking for 15-30 min, taking out, and putting into a drying oven at 80-100 ℃ for drying for 2-4 h for later use;
step seven: and C, coating a layer of uniform oily graphene with the thickness of 10-20 microns on the coating obtained in the step six, and then drying the coating in a drying oven at the temperature of 80-100 ℃ for 2-4 hours to finish the coating of the graphene-based steel anticorrosive coating.
2. The preparation method of the graphene-based steel anticorrosive coating according to claim 1, wherein the underwater curing epoxy resin is prepared from a component A and a component B according to a mass ratio of 100 (20-35), wherein the component A is epoxy resin, and the component B is an underwater curing agent.
3. The preparation method of the graphene-based steel anticorrosive coating according to claim 1, wherein the underwater curing epoxy resin is prepared from a component A and a component B according to a mass ratio of 100: 21.
4. The method for preparing the graphene-based steel anticorrosive coating according to claim 2 or 3, wherein the component A is bisphenol F epoxy resin, bisphenol A epoxy resin or novolac epoxy resin.
5. The method for preparing graphene-based steel anticorrosive coating according to claim 2 or 3, wherein the component B is polyamide curing agent, aliphatic amine curing agent or phenolic amine curing agent.
6. The preparation method of the graphene-based steel anticorrosive coating according to claim 1, characterized in that the method for oil and rust removal treatment of the steel surface comprises the following steps: adopting absorbent cotton to dip and analyze pure alcohol, and wiping the surface of the steel until no floating rust trace exists; then, the steel is ultrasonically cleaned for 10min by deionized water.
7. The method for preparing graphene-based steel anticorrosive coating according to claim 1, wherein the silane coupling agent is Kh550 silane coupling agent.
8. The preparation method of the graphene-based steel anticorrosive coating according to claim 1, wherein the step four is ultrasonic dispersion under the conditions of 150-200W and 40 kHz.
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