CN113801538A - Metal organic framework/epoxy coating and preparation method and application thereof - Google Patents
Metal organic framework/epoxy coating and preparation method and application thereof Download PDFInfo
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- 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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- 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 relates to the technical field of coatings, and particularly discloses a metal organic framework/epoxy coating as well as a preparation method and application thereof. The metal organic framework/epoxy coating comprises a metal organic framework and epoxy resin, wherein the mass ratio of the metal organic framework to the epoxy resin is (0.01-0.05): 10. The metal organic framework comprises zeolitic methylimidazolium framework nanosheets or zeolitic methylimidazolium framework nanoparticles. According to the invention, the metal organic framework and the epoxy resin are compounded according to a specific mass ratio to obtain the coating, the doping amount of the metal organic framework is reduced, the compatibility of the metal organic framework and the epoxy resin is facilitated, the anti-corrosion performance of the coating can be enhanced, the anti-corrosion performance of the composite coating containing the coating on the surface is further improved, and the production cost is saved on the basis of improving the anti-corrosion protection performance of the composite coating.
Description
Technical Field
The invention relates to the technical field of coatings, in particular to a metal organic framework/epoxy coating and a preparation method and application thereof.
Background
Among the four corrosion protection technologies, the surface coating technology is popular because of its advantages of rapidness, convenience, various types, mature process, controllable cost, etc. The epoxy resin is the most common synthetic resin, has certain hardness, wear resistance and corrosion resistance, but still cannot adapt to the corrosion environment of high salt, high humidity and high heat in south China sea, and the service life of metal products is greatly shortened due to the severe corrosion problem.
The key discipline problems of the failure of the epoxy coating in the marine environment service are as follows: the integrity of the coating is destroyed and the barrier properties to corrosive media are diminished. In the curing process, a large number of microscopic channels are formed by solvent volatilization and resin water absorption shrinkage, so that the compactness of the coating is obviously reduced. Corrosive media such as water, oxygen, chloride ions and the like easily permeate into the metal surface from the defects of the coating, local electrochemical corrosion reaction immediately occurs, and finally, the cathode is stripped, and the coating is rapidly failed.
In order to enhance the integrity of organic coatings and thus improve their corrosion resistance, it is common practice to dope the coatings with certain inorganic fillers, thereby blocking microscopic pores formed by polymeric resins during film formation on metal surfaces. At present, the two-dimensional filler is widely applied to an anticorrosive coating, particularly, graphene is taken as a representative, but the inherent conductivity of the graphene can accelerate a local corrosion reaction to initiate electrochemical corrosion. On the other hand, if using nano SiO with better insulation2Amorphous SiO prevents the "corrosion acceleration effect" of graphene2The particle size is not uniform enough, the shielding effect cannot be achieved when the local particle size is too small, and the expansion of the coating defects is facilitated when the local particle size is too large.
Metal Organic Frameworks (MOFs) are three-dimensional framework crystalline materials obtained by the bonding of organic molecular ligands with corresponding metal ions through coordination bonds. The metal organic framework has high porosity, low density and good chemical stability. In recent years, metal-organic framework materials have come to be used for modifying epoxy resins, but conventional metal-organic framework materials are in the form of particles, and it is intended to achieve a shielding effect equivalent to that of graphene, and they can be achieved only by increasing the doping amount. However, an excessive doping amount not only causes an increase in coating preparation cost, but also promotes the generation of coating defects.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a metal organic framework/epoxy coating as well as a preparation method and application thereof. The metal organic framework used in the invention has the advantages of small dosage, outstanding shielding performance and durable stability, the metal organic framework with less doping amount is used as the filler of the epoxy resin, the metal organic framework with less doping amount has stronger shielding effect on corrosive substances, the anti-corrosion performance of the coating can be improved, the anti-corrosion performance of the composite coating is further improved, and the production cost is also saved.
In order to achieve the purpose, the invention adopts the technical scheme that:
the first purpose of the invention is to provide a metal organic framework/epoxy coating, which comprises a metal organic framework and epoxy resin, wherein the mass ratio of the metal organic framework to the epoxy resin is (0.01-0.05): 10.
The crystal grain size distribution of the metal organic framework is concentrated, which is beneficial to the dispersion of the metal organic framework in the epoxy resin matrix and reduces the defects of the composite coating.
According to the invention, the metal organic framework and the epoxy resin are compounded according to a specific mass ratio to obtain the coating, the doping amount of the metal organic framework is reduced, the compatibility of the metal organic framework and the epoxy resin is facilitated, the anti-corrosion performance of the coating can be enhanced, the anti-corrosion performance of the composite coating containing the coating on the surface is further improved, and the production cost is saved on the basis of improving the anti-corrosion protection performance of the composite coating. The reason why the amount of doping of the metal organic framework is reduced to enhance the anticorrosive property of the coating is two-fold: the metal organic framework with small doping amount is beneficial to enhancing the interface stability of the metal organic framework and an epoxy resin matrix, the microscopic defects of the coating are reduced, and the integrity of the coating is higher; secondly, under the condition of sufficient dispersion, the shielding effect of the metal organic framework with less doping amount on corrosive media is stronger.
More preferably, the mass ratio of the metal organic framework to the epoxy resin is 0.01: 10.
According to the work of Wang-Liang-Li et al published on Materials and Corrosion under the name of Corrosion protection of epoxy coatings ZSM-5 Zeolite on Mg-Li alloys, when the doping amount of the inorganic filler is 0.5 wt%, the composite coating obtains the best Corrosion protection performance, so the best doping amount of the inorganic/organic filler is mostly 0.5 wt%, in the invention, the doping amount of the metal organic framework in the epoxy resin is only 0.1 wt%, and the Corrosion resistance of the coating is obviously improved; and the integrity of the coating is high.
As a preferred embodiment of the metal-organic framework/epoxy coating of the present invention, the metal-organic framework comprises zeolitic methylimidazolium framework nanosheets or zeolitic methylimidazolium framework nanoparticles.
The zeolite methyl imidazole ester framework nanosheet or zeolite methyl imidazole ester framework nanoparticle is used as a filler of epoxy resin and applied to metal corrosion protection, so that the obtained coating has good corrosion resistance, and further the composite coating has good corrosion resistance.
According to the invention, common zeolite methylimidazolium ester framework nanosheets or zeolite methylimidazolium ester framework nanoparticles are used as the filler of the epoxy resin, and the extremely fine doping amount greatly reduces the preparation cost of the coating or the composite coating; in addition, zinc nitrate hydrate, water and zinc acetate, zinc gluconate, cobalt nitrate hydrate and 2-methylimidazole which are precursors of zeolite methylimidazolium framework nanosheets or zeolite methylimidazolium framework nanoparticles are industrially produced in large quantities, and can be prepared by simply mixing at normal temperature and normal pressure, so that the preparation method is simple, and the cost is further reduced compared with other metal-organic framework materials.
More preferably, the metal organic framework is zeolitic methylimidazolium framework nanosheets.
The zeolite methylimidazolium ester framework nanosheet has a larger length-diameter ratio and an ordered crystal structure, provides shielding performance equivalent to that of graphene, and simultaneously avoids the possibility of electrochemical corrosion.
The shielding effect of the zeolite methylimidazolium framework nanosheet with small doping amount on a corrosive medium is stronger than that of the zeolite methylimidazolium framework nanoparticle with large doping amount, so that the anticorrosive performance of the coating prepared from the zeolite methylimidazolium framework nanosheet with small doping amount is better than that of the coating prepared from the zeolite methylimidazolium framework nanoparticle with large doping amount.
As a preferred embodiment of the metal organic framework/epoxy coating material of the present invention, the epoxy resin comprises E-42 epoxy resin, E-44 epoxy resin, E-51 epoxy resin or epoxy resin having an epoxy value of 0.46mol/100g to 0.5mol/100 g. The above epoxy resin is not limited thereto but includes epoxy resins conventionally used in the art.
The invention provides a preparation method of the metal organic framework/epoxy coating, which comprises the following steps:
s1, adding the metal organic framework into an organic solvent, carrying out ultrasonic treatment, and stirring and dissolving to obtain a mixed solution;
s2, adding epoxy resin into the mixed solution, stirring uniformly, and performing ultrasonic treatment again to obtain a white turbid solution;
and S3, adding a curing agent into the white turbid liquid, uniformly stirring, and performing vacuum degassing to obtain the metal organic framework/epoxy coating.
More preferably, the organic solvent is methanol, and herein is not limited thereto, but includes organic solvents known in the art.
As a preferable embodiment of the preparation method of the metal organic framework/epoxy coating, the mass ratio of the curing agent to the epoxy resin is 1: 4.
As a preferred embodiment of the method for preparing the metal organic framework/epoxy coating material, the curing agent comprises one of aliphatic amine, aromatic amine and polyamide.
As a preferred embodiment of the preparation method of the metal organic framework/epoxy coating material, in the step S1, the ultrasonic time is 30min to 35min, and in the step S2, the ultrasonic time is 2h to 2.5 h.
The third purpose is that the composite coating prepared by the metal organic framework/epoxy coating is utilized.
As a preferred embodiment of the composite coating, the metal organic framework/epoxy coating is coated on the surface of an aluminum plate in a scraping way, the wet film thickness is 100 mu m, and then the composite coating is respectively cured for 2h and 6h at 60 ℃ and room temperature, so as to obtain the composite coating.
The composite coating prepared by the invention has wide application range and still has strong corrosion protection performance in harsh environments such as 'high salt, high humidity and high heat' in south China sea and the like. Also, if the coating of the invention is soaked in corrosive media for a long time, it is still possible for zeolitic methylimidazolium framework nanosheets or zeolitic methylimidazolium framework nanoparticles as inorganic filler to degrade, but Zn is released after the framework collapse2+、Co2+2-methylimidazole is frequently used as a corrosion inhibitor, and it is still possible to retard the expansion of the corrosion zone.
Compared with the prior art, the invention has the following beneficial effects:
1. the preparation method starts with solving the corrosion acceleration effect of the graphene filler, provides the metal organic framework with less doping amount, outstanding shielding performance and durable stability as the filler of the epoxy resin, improves the corrosion resistance of the coating, further improves the corrosion resistance of the composite coating, and saves the production cost;
2. the composite coating prepared by the metal organic framework/epoxy coating has wide application range and still has stronger corrosion protection performance and integrity in the environment of high salt, high humidity and high heat in south China sea.
3. When the doping amount of the zeolite methylimidazolium ester framework nanosheet in the epoxy resin is only 0.1 wt%, the corrosion resistance of the coating or the composite coating is obviously improved.
Drawings
FIG. 1 is a crystal structure diagram of zeolitic methylimidazolium framework nanosheets of example 1;
figure 2 is a schematic view of zeolitic methylimidazolium framework nanosheets/epoxy composite coatings prepared in examples 3 and 4;
FIG. 3 is a Bode plot of the electrochemical impedance spectra of the composite coatings prepared in examples 3-6 after immersion in corrosive media for 3 days;
figure 4 is a graph of the electrochemical results of zeolite methylimidazolium framework nanoparticles prepared using deionized water instead of methanol at different times in example 2.
Detailed Description
To better illustrate the objects, aspects and advantages of the present invention, the present invention will be further described with reference to the accompanying drawings and specific embodiments.
In the following examples, the experimental methods used were all conventional methods unless otherwise specified, and the materials, reagents and the like used were commercially available without otherwise specified.
Example 1 preparation of Zeolite methylimidazolium framework nanosheets
A preparation method of zeolite methylimidazolium ester framework nanosheets comprises the following steps:
0.33g of Zn (NO)3)2·6H2Adding O into 90mL of deionized water, and stirring until the O is completely dissolved; similarly, 0.985g of 2-methylimidazole was added to 90mL of deionized water and stirred until completely dissolved. Then, the two solutions were mixed together and stirred at room temperature for 24 hours to obtain a white turbid liquid. The white turbid solution is centrifuged at 8000rpm for 5min and then washed with deionized water for 3 times. And finally, vacuum drying the collected white solid at 110 ℃ for 4h to obtain white powder, namely the zeolite methylimidazolium framework nanosheet (the average size is 2-5 mu m, and the crystal structure diagram refers to figure 1).
The reaction formula for preparing the zeolite methylimidazolium ester framework nanosheet is as follows:
Zn2++2MeIm→Zn(MeIm)2+2H+。
example 2 preparation of Zeolite methylimidazolium ester framework nanoparticles
A preparation method of zeolite methylimidazolium ester framework nanoparticles comprises the following steps:
adding 1.6g of 2-methylimidazole into 20mL of deionized water, and stirring until the 2-methylimidazole is completely dissolved; likewise, 1.225g of zinc nitrate hexahydrate was dissolved in 30mL of deionized water. After the two substances are completely dissolved, the solution containing zinc nitrate hexahydrate is slowly added into the 2-methylimidazole solution by a dropper, the dropping process is about 10min, and after the dropping process is finished, a preservative film is covered to continuously react for 2 hours at room temperature under the condition of stirring. The product was then centrifuged for 5 minutes at 8000r/min and washed 3 times with deionized water. And finally, drying in an oven at 110 ℃ for 8 hours (or drying in a vacuum oven at 110 ℃ for 4 hours) to obtain white powder, namely the zeolite methylimidazolium ester framework nano-particles.
A preparation method of a zeolite methylimidazolium framework nanosheet/epoxy composite coating comprises the following steps:
s1, adding 0.01g of the zeolite methylimidazolium framework nanosheet prepared in the embodiment 1 into 5mL of methanol, performing ultrasonic treatment for 30min, and stirring until the materials are completely dissolved to obtain a mixed solution;
s2, adding 10g E-44 epoxy resin into the mixed solution, uniformly stirring, and performing ultrasonic treatment for 2 hours again to obtain a white turbid solution;
s3, adding 2.5g of aliphatic amine into the white turbid liquid, uniformly stirring, and carrying out vacuum degassing for 5min to obtain the zeolite methylimidazolium skeleton nanosheet/epoxy coating;
s4, blade-coating the zeolite methyl imidazole ester framework Nanosheet/epoxy coating on the surface of an aluminum plate, wherein the wet film thickness is 100 microns, and then respectively curing for 2h and 6h at 60 ℃ and room temperature to obtain the composite coating (the doping amount of the zeolite methyl imidazole ester framework Nanosheet Nanosheet is 0.1% wt).
A preparation method of a zeolite methylimidazolium framework nanosheet/epoxy composite coating comprises the following steps:
s1, adding 0.05g of the zeolite methylimidazolium framework nanosheet prepared in the example 1 into 5mL of methanol, performing ultrasonic treatment for 30min, and stirring until the materials are completely dissolved to obtain a mixed solution;
s2, adding 10g E-44 epoxy resin into the mixed solution, uniformly stirring, and performing ultrasonic treatment for 2 hours again to obtain a white turbid solution;
s3, adding 2.5g of aliphatic amine into the white turbid liquid, uniformly stirring, and carrying out vacuum degassing for 5min to obtain the zeolite methylimidazolium skeleton nanosheet/epoxy coating;
s4, blade-coating the zeolite methyl imidazole ester framework Nanosheet/epoxy coating on the surface of an aluminum plate, wherein the wet film thickness is 100 microns, and then respectively curing for 2h and 6h at 60 ℃ and room temperature to obtain the composite coating (the doping amount of the zeolite methyl imidazole ester framework Nanosheet Nanosheet is 0.5% wt).
Schematic diagrams of zeolitic methylimidazolium framework nanosheets/epoxy composite coatings prepared in examples 3 and 4 are shown in fig. 2.
Example 5 Zeolite methylimidazolium framework nanoparticle/epoxy composite coating and preparation method thereof
A preparation method of zeolite methylimidazolium skeleton nanoparticle/epoxy composite coating comprises the following steps:
s1, adding 0.01g of the zeolite methylimidazolium ester framework nanoparticles prepared in the embodiment 2 into 5mL of methanol, performing ultrasonic treatment for 30min, and stirring until the nanoparticles are completely dissolved to obtain a mixed solution;
s2, adding 10g E-44 epoxy resin into the mixed solution, uniformly stirring, and performing ultrasonic treatment for 2 hours again to obtain a white turbid solution;
s3, adding 2.5g of aliphatic amine into the white turbid liquid, uniformly stirring, and carrying out vacuum degassing for 5min to obtain the zeolite methylimidazolium skeleton nanosheet/epoxy coating;
s4, blade-coating the zeolite methyl imidazole ester framework nanosheet/epoxy coating on the surface of an aluminum plate, wherein the wet film thickness is 100 microns, and then respectively curing for 2h and 6h at 60 ℃ and room temperature to obtain the composite coating (the doping amount of zeolite methyl imidazole ester framework Nanoparticle nanoparticles is 0.1% wt).
Example 6 Zeolite methylimidazolium framework nanoparticle/epoxy composite coating and preparation method thereof
A preparation method of zeolite methylimidazolium skeleton nanoparticle/epoxy composite coating comprises the following steps:
s1, adding 0.05g of the zeolite methylimidazolium ester framework nanoparticles prepared in the embodiment 2 into 5mL of methanol, performing ultrasonic treatment for 30min, and stirring until the nanoparticles are completely dissolved to obtain a mixed solution;
s2, adding 10g E-44 epoxy resin into the mixed solution, uniformly stirring, and performing ultrasonic treatment for 2 hours again to obtain a white turbid solution;
s3, adding 2.5g of aliphatic amine into the white turbid liquid, uniformly stirring, and carrying out vacuum degassing for 5min to obtain the zeolite methylimidazolium skeleton nanosheet/epoxy coating;
s4, blade-coating the zeolite methyl imidazole ester framework nanosheet/epoxy coating on the surface of an aluminum plate, wherein the wet film thickness is 100 microns, and then respectively curing for 2h and 6h at 60 ℃ and room temperature to obtain the composite coating (the doping amount of zeolite methyl imidazole ester framework Nanoparticle nanoparticles is 0.5% wt).
Test examples, determination of the Corrosion protection Properties of different composite coatings
In order to simulate the environment of high salt, high humidity and high heat in south China sea, the test conditions of the experiment are that NaCl solution with the mass fraction of 3.5%, the humidity is 80-98%, and the temperature is 28-30 ℃.
In the three-electrode system, the working electrode was a 3004 aluminum alloy sheet coated with the composite coating prepared in examples 3-6, and the working area was 4.9cm2(ii) a The reference electrode is an Ag/AgCl electrode; the auxiliary electrode is a 1cm x 1cm platinum sheet electrode. The sine disturbance value is 50mV, and the frequency range is 105～10-2Hz, 3.5 percent of NaCl solution as electrolyte, the temperature is 28-30 ℃, and the soaking time is 3 days.
Referring to fig. 3, EIS results show that the composite coating prepared in example 3 has an impedance mode value of 2.64 × 10 in the low frequency region10Ω·cm2While the composite coating prepared in example 4 has an impedance modulus value of only 6.83 × 10 in the low frequency region9Ω·cm2。
EIS results show that the composite coating prepared in example 5 has an impedance mode in a low frequency regionThe value reaches 1.5 multiplied by 1010Ω·cm2While the composite coating prepared in example 6 has an impedance modulus value of only 3.32 × 10 in the low frequency region9Ω·cm2。
When the doping amount of the zeolite methylimidazolium framework Nanosheet is 0.25% wt (corresponding to 0.025g of methylimidazolium ester) or 1% wt (corresponding to 0.1g of methylimidazolium ester), the impedance modulus value of the coating in a low frequency region is lower than that of the composite coating prepared in the example 3-4, and the corrosion resistance of the prepared composite coating is lower than that of the composite coating prepared in the example 3-4.
In the process of preparing the nanoparticles of example 2, the inventors tried to change deionized water into methanol and observed the corrosion resistance of the nanoparticles at different times, but the corrosion resistance of the nanoparticles prepared by the method is far lower than that of the nanoparticles prepared in an aqueous environment, and refer to fig. 4.
In conclusion, when the doping amount of the zeolite methylimidazolium ester framework nanosheet in the epoxy resin is 0.1 wt%, the composite coating has the strongest anti-corrosion performance. The shielding effect of the zeolite methylimidazolium framework nanosheet with low doping amount on corrosive media is stronger than that of zeolite methylimidazolium framework nanoparticles with large doping amount. The invention saves the production cost and also improves the corrosion resistance of the composite coating.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and not for limiting the protection scope of the present invention, and although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Claims (9)
1. The metal organic framework/epoxy coating is characterized by comprising a metal organic framework and epoxy resin, wherein the mass ratio of the metal organic framework to the epoxy resin is (0.01-0.05): 10.
2. The metal-organic framework/epoxy coating of claim 1, wherein the metal-organic framework comprises zeolitic methylimidazolium framework nanosheets or zeolitic methylimidazolium framework nanoparticles.
3. The metal-organic framework/epoxy coating of claim 1, wherein the epoxy resin comprises an E-42 epoxy resin, an E-44 epoxy resin, an E-51 epoxy resin, or an epoxy resin having an epoxy value of 0.46mol/100g to 0.5mol/100 g.
4. The method for preparing a metal organic framework/epoxy coating according to any one of claims 1 to 3, comprising the following steps:
s1, adding the metal organic framework into an organic solvent, carrying out ultrasonic treatment, and stirring and dissolving to obtain a mixed solution;
s2, adding epoxy resin into the mixed solution, stirring uniformly, and performing ultrasonic treatment again to obtain a white turbid solution;
and S3, adding a curing agent into the white turbid liquid, uniformly stirring, and performing vacuum degassing to obtain the metal organic framework/epoxy coating.
5. The method according to claim 4, wherein the mass ratio of the curing agent to the epoxy resin is 1: 4.
6. The method of claim 4, wherein the curing agent comprises one of an aliphatic amine, an aromatic amine, and a polyamide.
7. The method of claim 4, wherein the sonication time in step S1 is 30min to 35min, and the sonication time in step S2 is 2h to 2.5 h.
8. A composite coating prepared by using the metal organic framework/epoxy coating as defined in any one of claims 1 to 3.
9. The composite coating of claim 8, wherein the metal organic framework/epoxy coating of any one of claims 1 to 3 is knife-coated on the surface of an aluminum plate with a wet film thickness of 100 μm, and then cured for 2h and 6h at 60 ℃ and room temperature respectively to obtain the composite coating.
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Application publication date: 20211217 |