CN114015325A - Anticorrosive coating containing HATN @ graphene and preparation method thereof - Google Patents
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Abstract
The invention belongs to the technical field of anticorrosive coatings, and relates to an anticorrosive coating containing HATN @ graphene and a preparation method thereof. The technical points are as follows: the corrosion protection coating comprises: epoxy resin, HANT @ graphene, a curing agent and an auxiliary agent; wherein the mass fraction of the HANT @ graphene in the anti-corrosion coating is 0.02-0.4%. According to the anticorrosive coating containing the HATN @ graphene composite material and the preparation method thereof, provided by the invention, the HATN organic matter with the nano rod-like structure provides rich redox groups, so that the compatibility of graphene and a polymer matrix is improved, and the blocking range of a graphene sheet layer is more continuous. Besides the barrier effect of the graphene reinforced coating, the potential difference between the inside and the outside of the coating is effectively reduced, and better electrochemical protection is realized.
Description
Technical Field
The invention belongs to the technical field of anticorrosive coatings, and relates to an anticorrosive coating containing HATN @ graphene and a preparation method thereof.
Background
The problems of metal corrosion and failure are all spread in various fields of national economy, and the problems relate to the life and property safety of people, industrial and agricultural production and national defense construction. Most metal materials are corroded due to contact with corrosive environment, and the corrosion of metals is not only destructive but also wide, so that the corrosion protection of metals becomes an important problem to be solved urgently in the engineering field. Among a plurality of anticorrosion measures, the coating has the advantages of wide adaptability, simple construction, low cost, convenient maintenance and the like, and becomes an important anticorrosion means which is most widely, economically and effectively applied at present.
In the prior art, graphene is usually doped into an anti-corrosion coating, and electrochemical protection is realized through the conductive action of the graphene. However, the compatibility of graphene and organic matters is poor, the graphene is difficult to disperse in the organic matters, so that the coating is not uniform and cannot play a complete protection role; meanwhile, after the graphene is doped into an organic matter, the structural defects of the graphene sheet layer are exposed, the conductivity of the graphene is reduced, and the electrochemical protection capability of the anti-corrosion coating is reduced.
Disclosure of Invention
The invention aims to provide an anticorrosive coating containing a HATN @ graphene composite material, wherein the HATN organic matter with a nano rod-like structure provides rich redox groups, and the compatibility of graphene and a polymer matrix is improved, and simultaneously, the blocking range of a graphene sheet layer is more continuous. Besides the barrier effect of the graphene reinforced coating, the potential difference between the inside and the outside of the coating is effectively reduced, and better electrochemical protection is realized.
The technical purpose of the invention is realized by the following technical scheme:
the invention provides an anti-corrosion coating containing HANT @ graphene, which comprises the following components in part by weight: epoxy resin, HANT @ graphene, a curing agent and an auxiliary agent; wherein the mass fraction of the HANT @ graphene in the anti-corrosion coating is 0.02-0.4%. Hexaazatrinaphthalene (HATN), a phenazine derivative, is a pi-conjugated aromatic organic compound having an imino group, the abundant C ═ N active reactive group of which is capable of undergoing a redox reaction by itself to protect a substrate from oxidation. According to the invention, an organic matter HANT with redox characteristics is compounded with graphene with strong shielding performance, on one hand, the dispersibility of the graphene and the compatibility of the graphene with a high polymer matrix are improved through the compounding of the organic matter and a graphene sheet layer; the redox active sites of the organic matter can also fill the structural defects of the graphene sheet layer at the edge part, and prolong the diffusion path of the corrosive medium. On the other hand, due to the existence of the graphene, the barrier effect of the coating is enhanced, the conductivity of the organic matter is increased, the potential difference between the inside and the outside of the coating is effectively reduced, and better electrochemical protection is realized.
Furthermore, the HANT @ graphene is formed by growing HANT on graphene oxide in situ by a hydrothermal synthesis method. By adopting an in-situ synthesis method, the HANT grows on the graphene oxide, a chemical bond can be formed between the graphene and the HANT, compared with the method of loading on the graphene, the HANT and the graphene are combined more tightly, the composite structure is more stable, and the mechanical properties of the anticorrosion coating, such as tensile strength, peeling strength and the like, are macroscopically improved.
Furthermore, the thickness of the anti-corrosion coating is 50-150 μm, and preferably 100 μm.
Further, the preparation method of HANT @ graphene specifically comprises the following steps: dissolving graphene oxide powder in acetic acid; then adding hexa-ketone cyclohexane and o-phenylenediamine into the solution, stirring the mixture evenly, and heating the obtained solution under reflux; and after the reaction is finished, filtering, washing and drying the suspension to obtain powder of HATN @ graphene. According to the method, cheap and easily-obtained raw materials of hexaketone cyclohexane and o-phenylenediamine are used as raw materials, HANT grows in situ on graphene oxide, and the method is simple and convenient to operate. It is worth mentioning that in this reaction, graphene oxide not only provides a growth substrate for HANT, but also acts as a catalyst.
Further, the mass ratio of the graphene oxide to the hexaketocyclohexane to the o-phenylenediamine is as follows: 1:3:3.75.
Further, the temperature of reflux heating is 100-150 ℃, and preferably 120 ℃.
Furthermore, the time of reflux heating is 8-48 h, preferably 10 h.
Further, the graphene oxide can be obtained by purchasing or preparing itself, and the preparation method includes but is not limited to the following steps:
slowly dissolving 2g of graphite and 1g of sodium nitrate in 46mL of concentrated sulfuric acid at 0 ℃, slowly adding 6g of potassium permanganate, and stirring for 2 hours; stirring the obtained mixed solution at 35 ℃ for 2 hours, then raising the temperature to 95 ℃, and slowly adding 124mL of warm water and 30mL of 30% hydrogen peroxide to obtain a yellow solution without generating bubbles; repeatedly centrifuging and washing with 5% hydrochloric acid and deionized water until the pH of the solution is neutral; and finally dissolving the graphene oxide powder in 100mL of water, carrying out ultrasonic treatment for 3 hours, and carrying out freeze drying to obtain graphene oxide powder.
Further, the preparation method of HANT @ graphene comprises but is not limited to the following steps:
taking 200mg of graphene oxide powder, and dissolving the graphene oxide powder in 50mL of acetic acid under uniform stirring; then 0.6g of cyclohexane hexaketone and 0.75g of o-phenylenediamine were added thereto, and the resulting solution was heated under reflux at 120 ℃ for 10 hours; after the reaction is finished, the suspension is subjected to vacuum filtration and washed for several times by sequentially using hot acetic acid, acetone, methanol and water; and finally, vacuum drying at 60 ℃ to obtain the powder of the HATN @ graphene composite material.
Further, the curing agent is a substance capable of curing an epoxy resin, including but not limited to a polyamide resin curing agent.
Further, the auxiliary agent is an agent commonly used in the art and capable of assisting, including but not limited to one or a mixture of two of a leveling agent or a defoaming agent.
The second purpose of the invention is to provide a preparation method of the corrosion-resistant coating containing HANT @ graphene, which has the same technical effect.
The technical purpose of the invention is realized by the following technical scheme:
the invention provides a preparation method of an anti-corrosion coating containing HANT @ graphene, which comprises the following operation steps:
s1, preparing graphene oxide;
s2, growing HANT on the graphene oxide in situ by a hydrothermal synthesis method to obtain HANT @ graphene;
s3, uniformly mixing HANT @ graphene with epoxy resin, and adding a curing agent and an auxiliary agent to obtain a mixed solution;
and S4, coating the mixed solution on a metal substrate and drying.
Further, the mass ratio of the epoxy resin to the curing agent is 2: 1.
Further, the invention provides a preparation method of the anti-corrosion coating containing HANT @ graphene, which comprises the following operation steps:
dispersing powder of the HATN @ graphene composite material in 1mL of ethanol, and carrying out ultrasonic treatment for 15 minutes; then adding 3g of epoxy resin, and mixing to prepare an epoxy resin mixed solution with the weight fraction of HATN @ graphene being 0.1%; then adding 1.5g of polyamide resin curing agent, a proper amount of defoaming agent and a leveling agent, spin-coating on a polished iron substrate to prepare an anticorrosive coating, and then placing the anticorrosive coating in a 60 ℃ oven, wherein the thickness of the dried coating is about 100 mu m.
In conclusion, the invention has the following beneficial effects:
(1) the HATN @ graphene composite material is prepared by a one-step hydrothermal method, and the synthesis method is simple to operate and low in cost;
(2) the HATN organic substance provides rich redox groups, improves the dispersibility of graphene and the compatibility of the graphene with a high-molecular substrate, and enables the blocking range of the graphene sheet layer to be more continuous.
(3) Besides the barrier effect of the graphene reinforced coating, the potential difference between the inside and the outside of the coating is effectively reduced, and better electrochemical protection is realized.
(4) The anticorrosive coating containing the HATN @ graphene composite material prepared by the invention can be widely applied to the engineering fields of metal corrosion protection and the like.
Drawings
FIG. 1 is a scanning electron microscope image of a HATN @ graphene composite material prepared in example 1 of the present invention;
FIG. 2 is a transmission electron micrograph of a HATN @ graphene composite prepared in example 1 of the present invention;
FIG. 3 is an X-ray diffraction pattern of the HATN @ graphene composite material prepared in example 1 of the present invention;
FIG. 4 is a Nyquist plot of the anticorrosion coating containing the HATN @ graphene composite prepared in example 1 of the present invention soaked in 3.5 wt% NaCl water solution for different days.
Detailed Description
To further illustrate the technical means and effects of the present invention for achieving the predetermined objects, the embodiments, features and effects of the anti-corrosion coating containing HANT @ graphene according to the present invention are described in detail below.
Example 1: anticorrosive coating containing HATN @ graphene and preparation method thereof
The preparation method of the anti-corrosion coating containing HANT @ graphene provided by the embodiment specifically comprises the following steps:
Step 2, preparing the HATN @ graphene composite material: taking 200mg of graphene oxide powder, and dissolving the graphene oxide powder in 50mL of acetic acid under uniform stirring; then 0.6g of cyclohexane hexaketone and 0.75g of o-phenylenediamine were added thereto, and the resulting solution was heated under reflux at 120 ℃ for 10 hours; after the reaction is finished, the suspension is subjected to vacuum filtration and washed for several times by sequentially using hot acetic acid, acetone, methanol and water; and finally, vacuum drying at 60 ℃ to obtain the powder of the HATN @ graphene composite material.
Step 3, preparing the anticorrosive coating containing HATN @ graphene: dispersing powder of the HATN @ graphene composite material in 1mL of ethanol, and carrying out ultrasonic treatment for 15 minutes; then adding 3g of epoxy resin (E-44), and mixing to prepare an epoxy resin mixed solution with the weight fraction of HATN @ graphene of 0.1%; then adding 1.5g of polyamide resin curing agent, 0.1g of defoaming agent and 0.08g of flatting agent, spin-coating on a polished iron substrate to prepare an anticorrosive coating, and then placing the anticorrosive coating in a 60 ℃ oven, wherein the thickness of the dried coating is about 100 microns.
The anticorrosive coating containing the HATN @ graphene composite material prepared by the method has the characteristics of low corrosion current and corrosion rate, excellent anticorrosive effect and the like. Fig. 1 and 2 are scanning electron microscope and transmission electron microscope images of the HATN @ graphene composite material, and it can be observed that the HATN of the rod-like structure is completely and effectively wrapped by the graphene nanosheets. Fig. 3 is an X-ray diffraction pattern of the HATN @ graphene composite material, which contains a relatively wide diffraction peak at 23.6 ° in addition to a characteristic peak of HATN, which corresponds to a (002) crystal face of graphene, and demonstrates effective recombination of HATN and graphene. FIG. 4 is a Nyquist plot of the HATN @ graphene containing anticorrosion coating obtained in this example immersed in a 3.5 wt% aqueous NaCl solution for various days. As can be seen from the graph, the impedance simulation value is as high as 1.31X 10 after the soaking day8Ωcm-2The coating is proved to have excellent corrosion protection capability. When the soaked product is soaked for 20 days, the impedance analog value can still be kept at 6.92 multiplied by 107Ωcm-2Left and right. Therefore, the anticorrosive coating has strong physical barrier capability and corrosion-retarding performance.
Example 2: anticorrosive coating containing HATN @ graphene and preparation method thereof
The preparation method of the anti-corrosion coating containing HANT @ graphene provided by the embodiment specifically comprises the following steps:
the preparation method comprises the following steps:
Step 2, preparing the HATN @ graphene composite material: taking 200mg of graphene oxide powder, and dissolving the graphene oxide powder in 50mL of acetic acid under uniform stirring; then 0.6g of cyclohexane hexaketone and 0.75g of o-phenylenediamine were added thereto, and the resulting solution was heated under reflux at 120 ℃ for 10 hours; after the reaction is finished, the suspension is subjected to vacuum filtration and washed for several times by sequentially using hot acetic acid, acetone, methanol and water; and finally, vacuum drying at 60 ℃ to obtain the powder of the HATN @ graphene composite material.
Step 3, preparing the anticorrosive coating containing HATN @ graphene: dispersing powder of the HATN @ graphene composite material in 1mL of ethanol, and carrying out ultrasonic treatment for 15 minutes; then adding 3g of epoxy resin (E-44), and mixing to prepare an epoxy resin mixed solution with the weight fraction of HATN @ graphene of 0.05%; then adding 1.5g of polyamide resin curing agent, 0.06g of defoaming agent and 0.1g of flatting agent, spin-coating on a polished iron substrate to prepare an anticorrosive coating, and then placing the anticorrosive coating in a 60 ℃ oven, wherein the thickness of the dried coating is about 100 microns.
Example 3: anticorrosive coating containing HATN @ graphene and preparation method thereof
The preparation method of the anti-corrosion coating containing HANT @ graphene provided by the embodiment specifically comprises the following steps:
the preparation method comprises the following steps:
Step 2, preparing the HATN @ graphene composite material: taking 200mg of graphene oxide powder, and dissolving the graphene oxide powder in 50mL of acetic acid under uniform stirring; then 0.6g of cyclohexane hexaketone and 0.75g of o-phenylenediamine were added thereto, and the resulting solution was heated under reflux at 120 ℃ for 10 hours; after the reaction is finished, the suspension is subjected to vacuum filtration and washed for several times by sequentially using hot acetic acid, acetone, methanol and water; and finally, vacuum drying at 60 ℃ to obtain the powder of the HATN @ graphene composite material.
Step 3, preparing the anticorrosive coating containing HATN @ graphene: dispersing powder of the HATN @ graphene composite material in 1mL of ethanol, and carrying out ultrasonic treatment for 15 minutes; then adding 3g of epoxy resin (E-44), and mixing to prepare an epoxy resin mixed solution with the weight fraction of HATN @ graphene of 0.02%; then 1.5g of polyamide resin curing agent, 0.02g of defoaming agent and 0.05g of flatting agent are added, an anticorrosive coating is prepared on a polished iron substrate by spin coating, and then the anticorrosive coating is placed in a 60 ℃ oven, and the thickness of the dried coating is about 100 mu m.
Example 4: anticorrosive coating containing HATN @ graphene and preparation method thereof
The preparation method of the anti-corrosion coating containing HANT @ graphene provided by the embodiment specifically comprises the following steps:
the preparation method comprises the following steps:
Step 2, preparing the HATN @ graphene composite material: taking 200mg of graphene oxide powder, and dissolving the graphene oxide powder in 50mL of acetic acid under uniform stirring; then 0.6g of cyclohexane hexaketone and 0.75g of o-phenylenediamine were added thereto, and the resulting solution was heated under reflux at 120 ℃ for 10 hours; after the reaction is finished, the suspension is subjected to vacuum filtration and washed for several times by sequentially using hot acetic acid, acetone, methanol and water; and finally, vacuum drying at 60 ℃ to obtain the powder of the HATN @ graphene composite material.
Step 3, preparing the anticorrosive coating containing HATN @ graphene: dispersing powder of the HATN @ graphene composite material in 1mL of ethanol, and carrying out ultrasonic treatment for 15 minutes; then adding 3g of epoxy resin (E-44), and mixing to prepare an epoxy resin mixed solution with the weight fraction of HATN @ graphene being 0.2%; then adding 1.5g of polyamide resin curing agent, 0.05g of defoaming agent and 0.1g of flatting agent, spin-coating on a polished iron substrate to prepare an anticorrosive coating, and then placing the anticorrosive coating in a 60 ℃ oven, wherein the thickness of the dried coating is about 100 microns.
Example 5: anticorrosive coating containing HATN @ graphene and preparation method thereof
The preparation method of the anti-corrosion coating containing HANT @ graphene provided by the embodiment specifically comprises the following steps:
the preparation method comprises the following steps:
Step 2, preparing the HATN @ graphene composite material: taking 200mg of graphene oxide powder, and dissolving the graphene oxide powder in 50mL of acetic acid under uniform stirring; then 0.6g of cyclohexane hexaketone and 0.75g of o-phenylenediamine were added thereto, and the resulting solution was heated under reflux at 120 ℃ for 10 hours; after the reaction is finished, the suspension is subjected to vacuum filtration and washed for several times by sequentially using hot acetic acid, acetone, methanol and water; and finally, vacuum drying at 60 ℃ to obtain the powder of the HATN @ graphene composite material.
Step 3, preparing the anticorrosive coating containing HATN @ graphene: dispersing powder of the HATN @ graphene composite material in 1mL of ethanol, and carrying out ultrasonic treatment for 15 minutes; then adding 3g of epoxy resin (E-44), and mixing to prepare an epoxy resin mixed solution with the weight fraction of HATN @ graphene being 0.3%; then adding 1.5g of polyamide resin curing agent, 0.05g of defoaming agent and 0.1g of flatting agent, spin-coating on a polished iron substrate to prepare an anticorrosive coating, and then placing the anticorrosive coating in a 60 ℃ oven, wherein the thickness of the dried coating is about 100 microns.
Example 6: anticorrosive coating containing HATN @ graphene and preparation method thereof
The preparation method of the anti-corrosion coating containing HANT @ graphene provided by the embodiment specifically comprises the following steps:
the preparation method comprises the following steps:
Step 2, preparing the HATN @ graphene composite material: taking 200mg of graphene oxide powder, and dissolving the graphene oxide powder in 50mL of acetic acid under uniform stirring; then 0.6g of cyclohexane hexaketone and 0.75g of o-phenylenediamine were added thereto, and the resulting solution was heated under reflux at 120 ℃ for 10 hours; after the reaction is finished, the suspension is subjected to vacuum filtration and washed for several times by sequentially using hot acetic acid, acetone, methanol and water; and finally, vacuum drying at 60 ℃ to obtain the powder of the HATN @ graphene composite material.
Step 3, preparing the anticorrosive coating containing HATN @ graphene: dispersing powder of the HATN @ graphene composite material in 1mL of ethanol, and carrying out ultrasonic treatment for 15 minutes; then adding 3g of epoxy resin (E-44), and mixing to prepare an epoxy resin mixed solution with the weight fraction of HATN @ graphene being 0.4%; then adding 1.5g of polyamide resin curing agent, 0.1g of defoaming agent and 0.07g of flatting agent, spin-coating on a polished iron substrate to prepare an anticorrosive coating, and then placing the anticorrosive coating in a 60 ℃ oven, wherein the thickness of the dried coating is about 100 microns.
TABLE 1 comparison of Corrosion Current and Corrosion Rate for Corrosion resistant coatings of inventive examples 1-6
Although the present invention has been described with reference to the preferred embodiments, it should be understood that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (10)
1. An anti-corrosion coating comprising HANT @ graphene, wherein the anti-corrosion coating comprises: epoxy resin, HANT @ graphene, a curing agent and an auxiliary agent; wherein the mass fraction of the HANT @ graphene in the anti-corrosion coating is 0.02-0.4%.
2. The anti-corrosion coating containing HANT @ graphene of claim 1, wherein the HANT @ graphene is grown in situ on graphene oxide by a hydrothermal synthesis method.
3. The anti-corrosion coating containing HANT @ graphene of claim 1, wherein the thickness of the anti-corrosion coating is 50-150 μm.
4. The anti-corrosion coating containing HANT @ graphene according to claim 1, wherein the preparation method of the HANT @ graphene specifically comprises: dissolving graphene oxide powder in acetic acid; then adding hexa-ketone cyclohexane and o-phenylenediamine into the solution, stirring the mixture evenly, and heating the obtained solution under reflux; and after the reaction is finished, filtering, washing and drying the suspension to obtain the powder of the HATN @ graphene.
5. The HANT @ graphene-containing anti-corrosion coating according to claim 4, wherein the mass ratio of the graphene oxide to the hexaketocyclohexane to the o-phenylenediamine is as follows: 1:3:3.75.
6. The anti-corrosion coating containing HANT @ graphene of claim 4, wherein the temperature of the reflow heating is 100-150 ℃.
7. The HANT @ graphene-containing anti-corrosion coating of claim 1, wherein the curing agent is a polyamide resin curing agent.
8. The anti-corrosion coating containing HANT @ graphene of claim 1, wherein the auxiliary agent is one or a mixture of two of a leveling agent and a defoaming agent.
9. The preparation method of the corrosion-resistant coating containing HANT @ graphene according to any one of claims 1 to 8, which is characterized by comprising the following operation steps:
s1, preparing graphene oxide;
s2, growing HANT on the graphene oxide in situ by a hydrothermal synthesis method to obtain HANT @ graphene;
s3, uniformly mixing the HANT @ graphene with epoxy resin, and adding a curing agent and an auxiliary agent to obtain a mixed solution;
and S4, coating the mixed solution on a metal substrate and drying.
10. The method for preparing the anti-corrosion coating containing HANT @ graphene according to claim 9, wherein the mass ratio of the epoxy resin to the curing agent is 2: 1.
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| CN116460017A (en) * | 2023-04-03 | 2023-07-21 | 上海槎南工贸发展有限公司 | Sheet metal part surface protective paint coating process |
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