CN112592652A - Preparation method of polyaniline/cerium nitrate/epoxy polymer coating - Google Patents
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- CN112592652A CN112592652A CN202011385193.9A CN202011385193A CN112592652A CN 112592652 A CN112592652 A CN 112592652A CN 202011385193 A CN202011385193 A CN 202011385193A CN 112592652 A CN112592652 A CN 112592652A
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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
- C09D179/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen, with or without oxygen, or carbon only, not provided for in groups C09D161/00 - C09D177/00
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- C09D163/00—Coating compositions based on epoxy resins; Coating compositions based on derivatives of epoxy resins
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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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
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Abstract
The invention discloses a preparation method of a polyaniline/cerium nitrate/epoxy polymer coating. The polyaniline can be formed by monomer aniline under the action of organic citric acid, and polyaniline epoxy resin is modified by doping certain rare earth salt cerous nitrate which has a passivation effect on metal, so that the chain structure of polyaniline is stabilized, the dispersibility of polyaniline in epoxy resin is improved, the defects in a coating are reduced, the coating is more compact and uniform, and the anti-corrosion effect of the coating is improved. Compared with a polyaniline epoxy resin coating, the corrosion resistance effect of the prepared polyaniline/cerium nitrate/epoxy polymeric coating is greatly improved, the electrical impedance is larger, the protection period is longer, and the prepared polyaniline/cerium nitrate/epoxy polymeric coating has a more lasting and stable protection effect on base metal.
Description
Technical Field
The invention relates to the field of metal anticorrosive coatings, in particular to a preparation method of a polyaniline/cerium nitrate/epoxy polymer coating.
Background
The metal and the alloy have wide application, relate to more fields and are one of important materials for national economic construction and development. However, because of the severe corrosion phenomena of metals, the annual quantities of metal equipment and materials scrapped due to corrosion are 1/3 times the annual production of metal. The metal corrosion phenomenon is widely existed, and particularly, the metal can be seriously corroded and damaged under the corrosion of chloride ions. For example, the corrosion of metals in fishing boat yachts and structural members, the corrosion of mining equipment in seaside mines and seabed mineral deposits, and the corrosion of monitoring equipment by brine water generated in the stockpiling of tailing reservoirs can be caused by the chloride ions existing in a large amount in the marine environment, and the corrosion phenomenon of the chloride salts brings huge economic loss to the fields. Therefore, it is necessary to protect metals and alloys from corrosion by some protective means.
At present, a plurality of metal protection methods are available, the most economic and effective protection means with convenient construction is to coat an organic coating, wherein the polyaniline epoxy resin composite coating has better protection performance on metals and is a hotspot and direction of current research and future research in a period of time.
The pure polyaniline coating cannot play a role in effectively protecting a metal matrix for a long time due to incompact molecular accumulation, porous film layers and poor adhesive force. The potential of the polyaniline is low, so that the potential of the metal can be increased; polyaniline has good redox reversibility, and when reversible conversion is carried out between an intermediate oxidation state and a reduction state, electrons generated during oxidation of aluminum alloy are consumed, so that a protective oxide film is formed on the surface of the aluminum alloy.
An epoxy resin coating is a widely used coating, and the epoxy resin contains two or more epoxy groups per molecule on average. The epoxy resin paint mainly comprises epoxy resin and a curing agent thereof, and the auxiliary components comprise pigment, filler and the like. The epoxy resin coating has excellent hydration resistance and chemical resistance (acid resistance, alkali resistance and organic solvent resistance), has good adhesion performance, and is suitable for coating steel and the like in various corrosive environments, especially the surfaces of various storage tanks.
The polyaniline epoxy resin can effectively combine two characteristics of polyaniline and organic epoxy resin, and can play a multiple protection role on a metal matrix. Polyaniline has good conductivity and can transfer the electrochemical reaction of the interface of the coating metal matrix to the interface of the coating electrolyte solution.
In addition, polyaniline has redox reversibility and can promote the generation of a passivation film on the surface of metal. However, polyaniline only has a mechanical barrier effect on a metal matrix in an environment with a pH value of more than 7, and has good conductivity and electrochemical activity in an environment with a pH value of less than 7. Citric acid is an environment-friendly and nontoxic organic acid, has a passivation effect on metal matrixes such as iron and stainless steel, and can provide an acid environment for polyaniline, so that the improvement of the anti-corrosion activity of the polyaniline by using the citric acid as a doping acid is a very necessary research.
The preparation process of the polyaniline epoxy resin has some problems, and the strong hydrogen bond acting force among polyaniline molecules can cause the agglomeration among the polyaniline molecules, so that the polyaniline can not be well dispersed in the epoxy resin, the agglomeration phenomenon occurs, and the defects of hole agglomeration and the like are caused in the organic base material resin, thereby causing the reduction of the shielding performance of the coating, accelerating the failure of the coating and reducing the service life of the coating. Therefore, the preparation of polyaniline epoxy anticorrosive paint needs to solve the problem that polyaniline cannot be well dispersed in epoxy resin.
The rare earth ions can form a passivation film on the metal surface to play a role in passivation protection. By adding rare earth salt cerous nitrate into polyaniline epoxy resin, the chain structure of polyaniline can be stabilized under the action of the epoxy resin, the dispersibility of polyaniline in the epoxy resin is improved, the defects in the coating are reduced, the polyaniline can be better dispersed into the epoxy resin, and the anti-corrosion effect of the coating is improved. However, the research reports in the aspect are less, so that the addition of rare earth salt in polyaniline epoxy resin has important significance for the research of developing novel polyaniline epoxy resin composite coatings.
Disclosure of Invention
The invention aims to solve the problem that polyaniline cannot be well dispersed in epoxy resin due to agglomeration among polyaniline molecules in the traditional preparation process of polyaniline epoxy resin.
The invention provides a preparation method of a polyaniline/cerium nitrate/epoxy polymer coating, which comprises the following specific steps:
(1) preparing polyaniline under the action of organic acid: under the action of citric acid, aniline is oxidized by an oxidant to obtain polyaniline.
(2) Preparing modified polyaniline doped with cerium nitrate: adding a certain amount of cerous nitrate into the polyaniline solution, fully stirring, and standing at a certain temperature for reaction to prepare the citric acid-cerous nitrate doped polyaniline colloidal solution. Standing and filtering to obtain a precipitate, washing the precipitate with deionized water to be neutral, washing with acetone for three to four times, vacuum drying to obtain a dark green polyaniline product doped with citric acid-cerium nitrate, and grinding the solid product after vacuum drying into powder.
(3) Preparing a polyaniline/cerium nitrate/epoxy polymer coating: dissolving a certain amount of epoxy resin into a certain amount of dimethylbenzene, adding a proper amount of polyaniline powder doped with citric acid-cerium nitrate obtained in the step (2), uniformly stirring, respectively stirring on an ultrasonic stirrer and a magnetic stirrer, adding a proper amount of curing agent, and fully stirring until the mixture is completely mixed to prepare the polyaniline/cerium nitrate/epoxy polymeric coating.
(4) Surface treatment of the protected metal substrate: respectively polishing with 240#, 400#, 600#, 800# and 1000# metallographic abrasive paper to a mirror surface, sequentially ultrasonically cleaning with deionized water and absolute ethyl alcohol to remove oil, and blow-drying with a hair dryer.
(5) Coating of the coating: the surface of a 316L type stainless steel substrate is manually brushed, and the dry film thickness of the polyaniline/cerium nitrate/epoxy polymer coating is 50 mu m.
(6) Soaking and corroding of a protected metal substrate: and (3) carrying out failure behavior research on the substrate coated with the polyaniline/cerium nitrate/epoxy polymeric coating in neutral seawater.
(7) Testing of coating failure behavior: placing the prepared metal test piece in neutral seawater to perform electrochemical impedance test, wherein the electrochemical impedance adopts a three-electrode system, the working electrode is a coating metal test piece, the reference electrode is a saturated calomel electrode, the auxiliary electrode is a platinum electrode, and the working area is 3.14cm2. The corrosion medium is neutral seawater, and the test condition is room temperature.
In the step (1), the oxidant is ammonium persulfate, and the acid is organic citric acid.
In the step (1), the mass ratio of ammonium persulfate to aniline is as follows: 1: 2.5, the concentration of the citric acid solution is 1.0 mol/L.
In the step (2), the addition amount of the cerium nitrate is 5 g/L.
In the step (2), cerium nitrate is added into the polyaniline solution, and the temperature and the time of standing reaction are 20 +/-3 ℃ and 24 hours.
In the step (2), the vacuum drying condition is 60 ℃ and 48 hours.
In the step (3), the epoxy resin can be selected from E44, E51 or a combination thereof, and the curing agent is polyamide resin 650.
In the step (3), the mass ratio of the epoxy resin, the dimethylbenzene to the polyamide resin is 1: 0.5: 0.8.
in the step (3), the stirring time of the polyaniline powder doped with citric acid-cerium nitrate on an ultrasonic stirrer and a magnetic stirrer is 30min and 3h respectively. The stirring speed of the magnetic stirrer is 150 r/min.
In the step (4), the surface of the protected body is coated with a polyaniline/cerium nitrate/epoxy polymer coating with a dry film thickness of 45-50 μm.
The invention has the beneficial effects that:
the preparation method of the polyaniline/cerium nitrate/epoxy polymeric coating can enable monomer aniline to form polyaniline under the action of organic citric acid, and stabilize the polyaniline chain structure under the action of epoxy resin by doping certain rare earth salt cerium nitrate which has a passivation effect on metal, so that the dispersity of polyaniline in epoxy resin is improved, polyaniline can be better dispersed in epoxy resin, the defects in the coating are reduced, the coating is more compact and uniform, and the anti-corrosion effect of the coating is improved. Compared with a polyaniline epoxy resin coating, the corrosion resistance effect of the prepared polyaniline/cerium nitrate/epoxy polymeric coating is greatly improved, the electrical impedance is larger, the protection period is longer, and the prepared polyaniline/cerium nitrate/epoxy polymeric coating has a more lasting and stable protection effect on base metal.
Drawings
The invention is further described in detail below with reference to the following drawings and embodiments:
fig. 1a is a Nyquist plot of a doped cerium nitrate polyaniline epoxy polymeric coating and an undoped cerium nitrate polyaniline epoxy polymeric coating, each in seawater at pH 7.5.
Fig. 1b is a Bode plot of the cerium nitrate-doped polyaniline epoxy polymer coating and the undoped cerium nitrate polyaniline epoxy polymer coating in seawater with pH of 7.5.
Fig. 2 is a Tafel plot of a cerium nitrate-doped polyaniline epoxy polymer coating and an undoped cerium nitrate polyaniline epoxy polymer coating in seawater with a pH of 7.5.
Detailed Description
Example 1
The embodiment provides a preparation method of a polyaniline/cerium nitrate/epoxy polymer coating, which comprises the following specific steps:
(1) preparing polyaniline under the action of citric acid: and (3) carrying out oxidation reaction on aniline by using ammonium persulfate under the action of citric acid to obtain polyaniline.
(2) Preparing modified polyaniline doped with cerium nitrate: adding a certain amount of cerous nitrate into the polyaniline solution, fully stirring, and standing at a certain temperature for reaction to prepare the citric acid-cerous nitrate doped polyaniline colloidal solution. Standing at 20 ℃ for 24h, filtering to obtain a precipitate, washing the precipitate with deionized water to neutrality, washing with acetone for three to four times, vacuum-drying at 60 ℃ for 48h to obtain a dark green polyaniline product doped with citric acid-cerium nitrate, and grinding the vacuum-dried solid product into powder.
(3) Preparing a polyaniline/cerium nitrate/epoxy polymer coating: dissolving a certain amount of E44 epoxy resin into a certain amount of dimethylbenzene, adding a proper amount of polyaniline powder doped with citric acid-cerium nitrate in the step (2), uniformly stirring by hand, carrying out ultrasonic stirring for 30min, stirring for 3h at 150r/min on a magnetic stirrer, adding a proper amount of polyamide resin 650 curing agent, completely mixing, and fully stirring to prepare the polyaniline/cerium nitrate/epoxy polymeric coating.
(4) The proportion of each component is as follows: the mass ratio of ammonium persulfate to aniline is as follows: 1: 2.5, the concentration of the citric acid solution is 1.0mol/L, the addition amount of the cerium nitrate is 5g/L, and the mass ratio of the epoxy resin to the xylene to the polyamide resin is 1: 0.5: 0.8.
(5) surface treatment of 316L type stainless steel substrate: the area of the 316L-shaped stainless steel is 29.63cm2Respectively polishing with 240#, 400#, 600#, 800# and 1000# metallographic abrasive paper, sequentially ultrasonic cleaning with deionized water and absolute ethyl alcohol to remove oil, and drying with an air duct.
(6) Coating of the coating: the surface of a 316L type stainless steel substrate is manually brushed, and the dry film thickness of the polyaniline/cerium nitrate/epoxy polymer coating is 50 mu m.
(7) Soaking and corroding a 316L type stainless steel substrate: the 316L type stainless steel matrix coated with the polyaniline/cerium nitrate/epoxy polymeric coating is subjected to failure behavior research in neutral seawater.
(8) Testing of coating failure behavior: placing the prepared 316L-shaped stainless steel test piece in neutral seawater to perform electrochemical impedance test, wherein the electrochemical impedance adopts a three-electrode system, the working electrode is the 316L-shaped stainless steel test piece coated with the coating, the reference electrode is a saturated calomel electrode, the auxiliary electrode is a platinum electrode, and the working area is 3.14cm2. The corrosion medium is neutral seawater, and the test condition is room temperature.
Example 2:
the failure behavior of the 316L type stainless steel substrate coated with the polyaniline/cerium nitrate/epoxy polymeric coating in neutral seawater is compared with that of the embodiment in which cerium nitrate is not added. According to the procedure of the example, a coating layer of polyaniline made directly from citric acid and epoxy resin was formed without doping cerium nitrate under the same preparation conditions as the examples, and the coating layer was tested for failure behavior using the same coating method (6) and electrochemical tests (7) (8) as the examples.
The embodiment provides a preparation method of a polyaniline/cerium nitrate/epoxy polymer coating, which is characterized by comprising the following steps: the method comprises the following specific steps:
(1) preparing polyaniline under the action of citric acid: and (3) carrying out oxidation reaction on aniline by using ammonium persulfate under the action of citric acid to obtain polyaniline.
(2) Preparing a polyaniline epoxy polymer coating: dissolving a certain amount of E44 epoxy resin into a certain amount of dimethylbenzene, adding a proper amount of polyaniline powder obtained in the step (1), uniformly stirring by hand, performing ultrasonic stirring for 30min, stirring for 3h at a speed of 150r/min on a magnetic stirrer, adding a proper amount of polyamide resin 650 curing agent, completely mixing, and sufficiently stirring to prepare the polyaniline epoxy polymerization coating.
(4) The proportion of each component is as follows: the mass ratio of ammonium persulfate to aniline is as follows: 1: 2.5, the concentration of the citric acid solution is 1.0mol/L, and the mass ratio of the epoxy resin, the dimethylbenzene to the polyamide resin is 1: 0.5: 0.8.
(5)surface treatment of 316L type stainless steel substrate: the area of the 316L-shaped stainless steel is 29.63cm2Respectively polishing with 240#, 400#, 600#, 800# and 1000# metallographic abrasive paper, sequentially ultrasonic cleaning with deionized water and absolute ethyl alcohol to remove oil, and drying with an air duct.
(6) Coating of the coating: the surface of a 316L type stainless steel substrate is manually brushed, and the dry film thickness of the polyaniline epoxy polymer coating is 50 mu m.
(7) Soaking and corroding a 316L type stainless steel substrate: the 316L type stainless steel matrix coated with the polyaniline epoxy polymerization coating is subjected to failure behavior research in neutral seawater.
(8) Testing of coating failure behavior: placing the prepared 316L-shaped stainless steel test piece in neutral seawater to perform electrochemical impedance test, wherein the electrochemical impedance adopts a three-electrode system, the working electrode is the 316L-shaped stainless steel test piece coated with the coating, the reference electrode is a saturated calomel electrode, the auxiliary electrode is a platinum electrode, and the working area is 3.14cm2. The corrosion medium is neutral seawater, and the test condition is room temperature.
As can be seen from fig. 1(a), the diameter of the low-frequency capacitive arc of the stainless steel coated with the polyaniline epoxy resin composite coating modified by adding cerium nitrate is larger than that of the stainless steel coated with the polyaniline epoxy resin composite coating without adding cerium nitrate. As can be seen from FIG. 1(b), the impedance modulus | Z tintof stainless steel of the polyaniline epoxy resin composite coating modified by adding cerium nitrate0.01HzIs 3.19X 107Ω·cm2Stainless steel impedance modulus | Z & lt & gt of polyaniline epoxy resin composite coating without cerium nitrate0.01HzIs 8.24X 105Ω·cm2The impedance modulus of the polyaniline epoxy resin composite coating stainless steel added with cerium nitrate is improved by 38.71 times compared with the impedance modulus of the polyaniline epoxy resin composite coating stainless steel not added with cerium nitrate. Therefore, the corrosion resistance of the stainless steel coated with the polyaniline epoxy resin composite coating modified by adding cerium nitrate is obviously higher than that of the stainless steel coated with the polyaniline epoxy resin composite coating without adding cerium nitrate.
As can be seen from FIG. 2, the stainless steel coated with the polyaniline epoxy resin composite coating modified by adding cerium nitrateAnd the self-corrosion potential (Ecorr) of the stainless steel coated with the polyaniline epoxy resin composite coating without the addition of the cerium nitrate is-0.159V and-0.361V respectively. According to the judgment standard of the corrosion condition of the steel bar in the technical Standard for building Structure detection (GB/T50344-2004), the Ecorr of the stainless steel coated with the composite coating modified by adding cerium nitrate is larger than-0.2V, which indicates that the stainless steel is not corroded, and the Ecorr of the stainless steel coated with the composite coating without adding cerium nitrate is smaller than-0.2V, which indicates that the stainless steel coated with the coating is locally corroded. In addition, compared with a stainless steel substrate coated with the polyaniline epoxy resin composite coating without adding cerium nitrate, the corrosion current density of the stainless steel in the polyaniline epoxy resin composite coating modified by adding cerium nitrate is 6.48 multiplied by 10-7mA·cm-2Reduced to 8.47 x 10-8mA·cm-2. Therefore, the corrosion resistance of the polyaniline epoxy resin composite coating modified by adding the cerous nitrate is further proved to be better than that of the polyaniline epoxy resin composite coating without adding the nitric acid.
The embodiments described above are intended to facilitate one of ordinary skill in the art in understanding and using the present invention. It will be readily apparent to those skilled in the art that various modifications to these embodiments may be made, and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the embodiments described herein, and those skilled in the art should make improvements and modifications within the scope of the present invention based on the disclosure of the present invention.
Claims (10)
1. A preparation method of polyaniline/cerium nitrate/epoxy polymer coating is characterized by comprising the following steps: the method comprises the following specific steps:
(1) preparing polyaniline under the action of organic acid: under the action of citric acid, aniline is subjected to oxidation reaction by using an oxidant to obtain polyaniline;
(2) preparing modified polyaniline doped with cerium nitrate: adding a certain amount of cerium nitrate into a polyaniline solution, fully stirring, standing at a certain temperature for reaction to prepare a citric acid-cerium nitrate doped polyaniline colloidal solution, standing and filtering to obtain a precipitate, washing the precipitate with deionized water to be neutral, washing with acetone for three to four times, performing vacuum drying to obtain a dark green citric acid-cerium nitrate doped polyaniline product, and grinding the vacuum dried solid product into powder;
(3) preparing a polyaniline/cerium nitrate/epoxy polymer coating: dissolving a certain amount of epoxy resin into a certain amount of dimethylbenzene, adding a proper amount of polyaniline powder doped with citric acid-cerium nitrate obtained in the step (2), uniformly stirring, respectively stirring on an ultrasonic stirrer and a magnetic stirrer, adding a proper amount of curing agent, and fully stirring until the mixture is completely mixed to prepare a polyaniline/cerium nitrate/epoxy polymeric coating;
(4) surface treatment of the protected metal substrate: respectively polishing with 240#, 400#, 600#, 800# and 1000# metallographic abrasive paper to a mirror surface, sequentially ultrasonically cleaning with deionized water and absolute ethyl alcohol to remove oil, and blow-drying with a hair dryer;
(5) coating of the coating: coating a polyaniline/cerium nitrate/epoxy polymer coating dry film on the surface of a 316L type stainless steel substrate by a manual brush;
(6) soaking and corroding of a protected metal substrate: carrying out failure behavior research on the substrate coated with the polyaniline/cerium nitrate/epoxy polymeric coating in neutral seawater;
(7) testing of coating failure behavior: and placing the prepared metal test piece in neutral seawater to perform electrochemical impedance test, wherein the electrochemical impedance adopts a three-electrode system, a working electrode is a coating metal test piece, a reference electrode is a saturated calomel electrode, an auxiliary electrode is a platinum electrode, a corrosion medium is neutral seawater, and the test condition is room temperature.
2. The method of claim 1, wherein the polyaniline/cerium nitrate/epoxy polymeric coating comprises: in the step (1), the oxidant is ammonium persulfate, and the acid is organic citric acid.
3. The method of claim 1, wherein the polyaniline/cerium nitrate/epoxy polymeric coating comprises: in the step (1), the mass ratio of ammonium persulfate to aniline is as follows: 1: 2.5, the concentration of the citric acid solution is 1.0 mol/L.
4. The method of claim 1, wherein the polyaniline/cerium nitrate/epoxy polymeric coating comprises: in the step (1), the oxidant is ammonium persulfate, and the acid is organic citric acid.
5. The method of claim 1, wherein the polyaniline/cerium nitrate/epoxy polymeric coating comprises: in the step (2), the addition amount of the cerium nitrate is 5 g/L.
6. The method of claim 1, wherein the polyaniline/cerium nitrate/epoxy polymeric coating comprises: in the step (2), cerium nitrate is added into the polyaniline solution, and the temperature and the time of standing reaction are 20 +/-3 ℃ and 24 hours.
7. The method of claim 1, wherein the polyaniline/cerium nitrate/epoxy polymeric coating comprises: in the step (2), the vacuum drying condition is 60 ℃ and 48 hours.
8. The method of claim 1, wherein the polyaniline/cerium nitrate/epoxy polymeric coating comprises: in the step (3), the epoxy resin can be selected from E44, E51 or a combination thereof, and the curing agent is polyamide resin 650.
9. The method of claim 1, wherein the polyaniline/cerium nitrate/epoxy polymeric coating comprises: in the step (3), the mass ratio of ammonium persulfate to aniline is 1: 2.5, the concentration of the citric acid solution is 1.0mol/L, and the addition amount of the cerium nitrate is 5 g/L.
10. The method of claim 1, wherein the polyaniline/cerium nitrate/epoxy polymeric coating comprises: in the step (3), the mass ratio of the epoxy resin, the dimethylbenzene to the polyamide resin is 1: 0.5: 0.8.
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