CN111910232B - Mof anticorrosive film for aluminum material and preparation method thereof - Google Patents
Mof anticorrosive film for aluminum material and preparation method thereof Download PDFInfo
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- CN111910232B CN111910232B CN202010624472.XA CN202010624472A CN111910232B CN 111910232 B CN111910232 B CN 111910232B CN 202010624472 A CN202010624472 A CN 202010624472A CN 111910232 B CN111910232 B CN 111910232B
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D9/00—Electrolytic coating other than with metals
- C25D9/02—Electrolytic coating other than with metals with organic materials
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F15/00—Other methods of preventing corrosion or incrustation
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/34—Pretreatment of metallic surfaces to be electroplated
- C25D5/42—Pretreatment of metallic surfaces to be electroplated of light metals
- C25D5/44—Aluminium
Abstract
The invention discloses an Mof anticorrosive film for aluminum materials and a preparation method thereof. The method comprises the following steps: sequentially polishing the aluminum sheet by using abrasive paper, washing the aluminum sheet by using absolute ethyl alcohol and water, and then drying the aluminum sheet at constant temperature for later use; dissolving zinc acetate into a methanol solution for later use, then dissolving dimethyl imidazole into the methanol solution of the zinc acetate, and pouring the mixed solution into an electrolytic cell; placing an aluminum sheet as an anode and an inert electrode as a cathode into an electrolytic cell, and applying voltage for treatment; taking out an aluminum sheet, and cleaning the aluminum sheet with methanol and absolute ethyl alcohol; drying at constant temperature to obtain the Mof anticorrosive film. The preparation method is simple, and the anticorrosion test result shows that the invention provides a way for developing Mof film for metal anticorrosion.
Description
Technical Field
The invention belongs to the technical field of corrosion prevention of film materials, and particularly relates to an Mof anticorrosive film for aluminum materials and a preparation method thereof.
Background
The metal and the alloy material thereof are important structural materials, have the position of great importance in various industries, and are widely applied to the fields of aerospace, transportation, infrastructure, microelectronics, precise instruments and the like. However, in the long-term use process of daily life, inevitable external damages such as abrasion, mechanical distortion, photo-aging, environmental corrosion and the like are often faced, so that the performance of the material itself is reduced, and the use requirements of human beings cannot be met. Among them, the environmental corrosion problem is one of the hot problems in the whole country and the whole world, and has attracted extensive attention from both academic and industrial fields. According to statistics, the cost of corrosion of metal materials and the consumption of corrosion protection thereof accounts for about 2-5% of the total value of national production in industrialized countries, and huge economic loss and resource waste are caused. In addition, the spread of the corrosion problem may cause serious environmental pollution, life decay, and even accidents, such as: oil gas leakage, bridge collapse, civil aviation accident, cultural relic treasure loss and the like. Therefore, it is essential to adopt an efficient metal corrosion prevention technique.
Metal Organic Frameworks (MOFs) are a class of novel crystalline porous materials, which are highly ordered porous networks formed by metal ions or metal oxide clusters in the presence of organic linkers. Since the pioneering work in the 90's of the 20 th century, MOF materials have shown unprecedented opportunities for wide applications such as chemical separation, gas storage, catalysis, sensors, drug delivery, etc. However, metal organic frameworks are currently used only rarely in the field of metal corrosion protection. Currently, various hydrophobic and water-stable MOFs (e.g., ZIF-8, MIL-53, and UiO-66) have been designed and synthesized, which are prerequisites for potential applications in the preservative industry, greatly expanding the range of candidates for preservative applications. However, the current method for researching and synthesizing the ZIF to be applied to metal corrosion protection is a hydrothermal method or other methods (ACS appl. mater. Interfaces 2018, 10, 2259-. These problems all limit the utility of ZIF8 in the corrosion protection industry.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention aims to provide an Mof anticorrosive film for an aluminum material and a preparation method thereof. The method comprises the steps of firstly polishing an aluminum sheet by using sand paper, cleaning and drying the aluminum sheet for later use, then preparing an electrolyte from metal salt, an organic ligand and a solvent, finally inserting the aluminum sheet and an inert electrode, applying voltage for reaction, and obtaining the Mof anticorrosive film on the aluminum sheet after treatment.
The purpose of the invention is realized by at least one of the following technical solutions.
The invention provides a preparation method of an Mof anticorrosive film for aluminum materials, which comprises the following steps:
(1) pretreatment of an aluminum sheet material: polishing an aluminum sheet by using abrasive paper with different meshes, sequentially cleaning the aluminum sheet by using absolute ethyl alcohol and deionized water after polishing, and drying at constant temperature to obtain a pretreated aluminum sheet;
(2) preparing electrolyte: adding zinc acetate into a methanol solvent, and uniformly mixing and dissolving to obtain a solution A; then dissolving dimethyl imidazole in the solution A, and uniformly mixing to obtain an electrolyte;
(3) mof Synthesis of Membrane: and (2) taking the pretreated aluminum sheet in the step (1) as an anode and an inert electrode as a cathode, transferring the anode, the cathode and the electrolyte in the step (2) into an electrolytic cell (the anode and the cathode need to be soaked in the electrolyte), applying voltage for treatment to obtain a treated aluminum sheet, washing the treated aluminum sheet with methanol and absolute ethyl alcohol in sequence, and drying at constant temperature to obtain the aluminum sheet with the Mof anticorrosive film.
Further, in the step (1), 600, 800, 1200 and 1500-mesh sand papers are sequentially used for polishing the aluminum sheet.
Further, the cleaning of step (1) comprises: and sequentially using absolute ethyl alcohol and water to clean the aluminum sheet.
Preferably, the washing in step (1) is performed by washing with anhydrous ethanol for 3 times and then washing with deionized water for 3 times.
Further, the drying temperature in the step (1) is 30-50 ℃, and the drying time is 5-15 min.
Furthermore, in the electrolyte in the step (2), the concentration of zinc acetate is 0.05-0.15mol/L, and the solubility of dimethyl imidazole is 0.1-0.2 mol/L.
Further, in the electrolyte in the step (2), the molar ratio of zinc acetate to dimethyl imidazole is 1-3: 2-4.
Further, in the step (3), after the voltage is applied, the current in the electrolyte is constantly 10-20 mA.
Further, the temperature for applying the voltage for processing in the step (3) is 25-45 ℃, and the time for applying the voltage for processing is 5-15 min.
Further, the distance between the anode and the inert electrode in the step (3) in the electrolytic cell is 1-2 cm.
Preferably, the washing in step (3) is performed by washing with methanol for 3 times and then washing with deionized water for 3 times.
Further, the drying temperature in the step (3) is 30-50 ℃, and the drying time is 5-15 min.
The invention provides an Mof anticorrosive film for aluminum materials, which is prepared by the preparation method.
Compared with the prior art, the invention has the following advantages and beneficial effects:
(1) ZIF8 is a metal organic framework material, and is mainly used in the fields of chemical separation, gas storage, catalysis and the like by a hydrothermal synthesis method at present; however, the use of electrochemically synthesized ZIF8 films for metal corrosion protection is not addressed; the method grows the metal organic framework film on the aluminum sheet by an electrochemical method, is simple and efficient, has ultra-fast synthesis rate and good universality;
(2) the synthetic process of the method is carried out in an open system, the maintenance cost is reduced, the preparation is carried out at normal temperature, the energy loss is reduced, the whole preparation process is completed in one step, the processes of activation, pretreatment and the like are omitted, the operation process is simplified, and the production efficiency is improved.
Drawings
FIG. 1a is a scanning electron microscope image of Mof anticorrosive film for aluminum material prepared in example 1;
FIG. 1b is a scanning electron microscope image of Mof anticorrosive film for aluminum material prepared in example 2;
FIG. 1c is a scanning electron micrograph of an Mof anticorrosive film for aluminum material prepared in example 3;
FIG. 1d is a scanning electron microscope image of Mof anticorrosive film for aluminum material prepared in example 4;
FIG. 2 is an XRD pattern of ZIF8 films obtained in examples 1-4 of the present invention;
FIG. 3 is a Tafel polarization plot of the polished aluminum flakes and the electrochemically grown ZIF8 film aluminum flakes obtained in example 1 of the present invention after being soaked in 3.5Wt% NaCl aqueous solution for 1 day.
Detailed Description
The following examples are presented to further illustrate the practice of the invention, but the practice and protection of the invention is not limited thereto. It is noted that the processes described below, if not specifically described in detail, are all realizable or understandable by those skilled in the art with reference to the prior art. The reagents or apparatus used are not indicated to the manufacturer, and are considered to be conventional products available by commercial purchase.
Example 1
A preparation method of Mof anticorrosive film for aluminum material comprises the following steps:
(1) polishing an aluminum sheet by using abrasive paper with different meshes (sequentially polishing by using 600, 800, 1200 and 1500 mesh abrasive paper) to obtain a polished aluminum sheet, sequentially cleaning the polished aluminum sheet by using absolute ethyl alcohol and deionized water after polishing, and then drying the cleaned aluminum sheet in a constant-temperature drying oven at the constant temperature of 30 ℃ for 15 min;
(2) weighing 0.55g of zinc acetate, dissolving the zinc acetate into 50mL of methanol solution, performing ultrasonic dissolution to obtain a clear solution, then weighing 0.41g of dimethyl imidazole, dissolving the dimethyl imidazole into the clear solution, and pouring the obtained electrolyte into an electrolytic cell;
(3) and (3) putting the cleaned aluminum metal sheet serving as an anode and the inert electrode serving as a cathode into an electrolytic cell, wherein the distance difference between the two electrodes is 1 cm. Applying voltage to make current constant at 15mA, reacting at 25 deg.C for 10 min; and taking out the treated aluminum sheet, sequentially washing the aluminum sheet with methanol and absolute ethyl alcohol, and drying the aluminum sheet at constant temperature of 30 ℃ for 15min to obtain the Mof anticorrosive film (ZIF 8 film).
Example 2
A preparation method of Mof anticorrosive film for aluminum material comprises the following steps:
(1) polishing an aluminum sheet by using abrasive paper with different meshes (sequentially polishing by using 600, 800, 1200 and 1500 meshes of abrasive paper), sequentially cleaning the aluminum sheet by using absolute ethyl alcohol and deionized water after polishing, and then drying the cleaned aluminum sheet in a constant-temperature drying oven at the constant temperature of 40 ℃ for 10 min;
(2) weighing 1.65g of zinc acetate, dissolving the zinc acetate in 50mL of methanol solution, performing ultrasonic dissolution to obtain a clear solution, then weighing 0.82g of dimethyl imidazole, dissolving the dimethyl imidazole in the clear solution to obtain electrolyte, and pouring the electrolyte into an electrolytic cell;
(3) putting a cleaned metal aluminum sheet as an anode and an inert electrode as a cathode into an electrolytic cell, wherein the distance difference between the two electrodes is 1.5 cm; applying voltage to make current constant at 20mA, reacting at 35 deg.C for 5 min; and taking out the treated aluminum sheet, sequentially washing the aluminum sheet with methanol and absolute ethyl alcohol, and drying the aluminum sheet at constant temperature of 40 ℃ for 5min to obtain the Mof anticorrosive film.
Example 3
A preparation method of Mof anticorrosive film for aluminum material comprises the following steps:
(1) polishing an aluminum sheet by using abrasive paper with different meshes (sequentially polishing by using 600, 800, 1200 and 1500 meshes of abrasive paper), sequentially cleaning the aluminum sheet by using absolute ethyl alcohol and deionized water after polishing, and then drying the cleaned aluminum sheet in a constant-temperature drying oven at the constant temperature of 50 ℃ for 5 min;
(2) weighing 1.1g of zinc acetate, dissolving the zinc acetate in 50mL of methanol solution, performing ultrasonic dissolution to obtain a clear solution, then weighing 0.615g of dimethyl imidazole, dissolving the dimethyl imidazole in the clear solution, and pouring the obtained electrolyte into an electrolytic cell;
(3) putting a cleaned metal aluminum sheet as an anode and an inert electrode as a cathode into an electrolytic cell, wherein the distance difference between the two electrodes is 2 cm; applying voltage to make current constant at 10mA, reacting at 45 deg.C for 15 min; and taking out the treated aluminum sheet, sequentially washing the aluminum sheet with methanol and absolute ethyl alcohol, and drying the aluminum sheet at the constant temperature of 50 ℃ for 10min to obtain the Mof anticorrosive film.
Example 4
A preparation method of Mof anticorrosive film for aluminum material comprises the following steps:
(1) polishing an aluminum sheet by using abrasive paper with different meshes (sequentially polishing by using 600, 800, 1200 and 1500 meshes of abrasive paper), sequentially cleaning the aluminum sheet by using absolute ethyl alcohol and deionized water after polishing, and then drying the cleaned aluminum sheet in a constant-temperature drying oven at the constant temperature of 30 ℃ for 15 min;
(2) weighing 0.55g of zinc acetate, dissolving the zinc acetate in 50mL of methanol solution, performing ultrasonic dissolution to obtain a clear solution, then weighing 0.41g of dimethyl imidazole, dissolving the dimethyl imidazole in the clear solution to obtain electrolyte, and pouring the electrolyte into an electrolytic cell;
(3) putting a cleaned metal aluminum sheet as an anode and an inert electrode as a cathode into an electrolytic cell, wherein the distance between the two electrodes is different by 1 cm; applying voltage to make current constant at 20mA, reacting at 35 deg.C for 15 min; and taking out the treated aluminum sheet, sequentially washing the aluminum sheet with methanol and absolute ethyl alcohol, and drying the aluminum sheet at constant temperature of 30 ℃ for 10min to obtain the Mof anticorrosive film.
Analysis of characterization results
FIG. 1a is a scanning electron microscope image of Mof anticorrosive film for aluminum material prepared in example 1; FIG. 1b is a scanning electron microscope image of Mof anticorrosive film for aluminum material prepared in example 2; FIG. 1c is a scanning electron micrograph of an Mof anticorrosive film for aluminum material prepared in example 3; FIG. 1d is a scanning electron microscope image of Mof anticorrosive film for aluminum material prepared in example 4. As can be seen from fig. 1a, 1b, 1c and 1d, ZIF8 particles electrochemically grown on aluminum sheets are stacked in a square shape, and a dense and defect-free film is formed on the surface.
FIG. 2 is an XRD pattern of ZIF8 films obtained in examples 1-4 of the present invention. The 5-35 ° peak is shown in fig. 2, and a sharp ZIF8 peak around 7.5 ° is clearly visible, indicating successful electrochemical growth of ZIF8 on aluminum sheets.
Evaluation of Corrosion resistance
FIG. 3 is a Tafel polarization graph of polished aluminum flakes obtained in step (1) of example 1 of the present invention and electrochemically grown ZIF8 film aluminum flakes (aluminum flakes having Mof anticorrosive film obtained in step (3) of example 1) after soaking in 3.5Wt% NaCl aqueous solution for 1 day. As can be seen from fig. 3, the corrosion voltage of the aluminum sheet grown with the ZIF8 film (aluminum sheet with Mof corrosion-resistant film) was positively shifted from-0.890V to-0.872V, compared to the untreated aluminum sheet (i.e., the polished aluminum sheet obtained in step (1) of example 1); the corrosion current is 1.236 multiplied by 10 -5 Acm -2 Reduced to 3.768 × 10 -7 Acm -2 The magnitude of the corrosion current is reduced by nearly 100 times. The aluminum sheet of the electrochemically grown ZIF8 film (aluminum sheet with Mof corrosion-resistant film) was shown to have excellent corrosion resistance.
The above examples are only preferred embodiments of the present invention, which are intended to be illustrative and not limiting, and those skilled in the art should understand that they can make various changes, substitutions and alterations without departing from the spirit and scope of the invention.
Claims (6)
1. A preparation method of Mof anticorrosive film for aluminum material is characterized by comprising the following steps:
(1) polishing an aluminum sheet, cleaning and drying to obtain a pretreated aluminum sheet;
(2) adding zinc acetate into a methanol solvent, and uniformly mixing and dissolving to obtain a solution A; then dissolving dimethyl imidazole in the solution A, and uniformly mixing to obtain an electrolyte, wherein in the electrolyte, the concentration of zinc acetate is 0.05-0.15mol/L, and the solubility of dimethyl imidazole is 0.1-0.2 mol/L;
(3) taking the pretreated aluminum sheet obtained in the step (1) as an anode and an inert electrode as a cathode, transferring the anode, the cathode and the electrolyte obtained in the step (2) into an electrolytic cell, applying voltage for treatment to obtain a treated aluminum sheet, washing and drying to obtain an aluminum sheet with an Mof anticorrosive film; after voltage is applied, the current in the electrolyte is constant at 10-20 mA; the temperature for applying the voltage for processing is 25-45 ℃, and the time for applying the voltage for processing is 5-15 min; the distance between the anode and the inert electrode in the electrolytic cell is 1-2 cm.
2. The method of preparing Mof anticorrosive film for aluminum material according to claim 1, wherein in step (1), the aluminum sheet is ground using 600, 800, 1200, 1500-mesh sandpaper in sequence.
3. The method of preparing Mof anticorrosive film for aluminum material according to claim 1, wherein the washing of step (1) includes: and sequentially using absolute ethyl alcohol and water to clean the aluminum sheet.
4. The method of manufacturing Mof anticorrosive film for aluminum material according to claim 1, wherein the drying temperature in step (1) is 30-50 ℃ and the drying time is 5-15 min.
5. The method for preparing Mof anticorrosive film for aluminum material according to claim 1, wherein in the electrolyte of step (2), the molar ratio of zinc acetate to dimethylimidazole is 1-3: 2-4.
6. The method of preparing Mof anticorrosive film for aluminum material according to any one of claims 1-5, wherein the drying temperature in step (3) is 30-50 ℃ and the drying time is 5-15 min.
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| CN113668031A (en) * | 2021-07-16 | 2021-11-19 | 桂林理工大学 | Preparation method for electrodepositing Ce-MOFs corrosion-resistant film on aluminum alloy anodic oxidation surface |
| CN114045479B (en) * | 2021-10-22 | 2023-12-26 | 佛山科学技术学院 | Corrosion-resistant aluminum alloy composite coating and preparation method and application thereof |
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