CN111732849A - VPC nano composite material with self-repairing performance and preparation method of coating thereof - Google Patents
VPC nano composite material with self-repairing performance and preparation method of coating thereof Download PDFInfo
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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
- 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
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
- C08G73/02—Polyamines
- C08G73/026—Wholly aromatic polyamines
- C08G73/0266—Polyanilines or derivatives thereof
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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
- 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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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- 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
- 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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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
Abstract
The invention discloses a VPC nano composite material with self-repairing performance and a preparation method of a coating thereof, wherein the preparation method of the VPC nano composite material comprises the following steps: adding vanadium pentoxide particles into deionized water to form a suspension A; dropwise adding aniline monomer and phytic acid into the suspension A, and uniformly stirring in an ice bath to obtain a suspension B; adding an oxidant into the suspension B, and then reacting for more than 3 hours in an ice bath to obtain a product C; filtering the product C, repeatedly washing the product C with deionized water and ethanol, and drying to obtain a product D; adding the product D into deionized water to form a suspension E; adding ferric chloride and a tannic acid solution into the suspension E, stirring for reaction, and then performing centrifugal separation to obtain a product F; and washing the product F by using deionized water, and drying to obtain the VPC nano composite material. The VPC nano composite material is combined with epoxy coating to form a coating, so that the coating has self-repairing performance and the corrosion resistance of the coating is enhanced.
Description
Technical Field
The invention relates to the technical field of coatings, in particular to a VPC nano composite material with self-repairing performance and a preparation method of a coating thereof.
Background
Among the various corrosion protection strategies, organic coatings are a simple and economical way to protect metals from corrosion. Among them, epoxy coatings are widely used due to their good corrosion resistance and high adhesion to metals. However, in practical use, due to Cl-、O2、CO2And the like, the single epoxy coating often loses the protective capability of the metal substrate in a short time. One of the effective methods for improving the protective ability of the coating is to endow the coating with a certain self-repairing ability, and the function is usually realized by utilizing nano-fillers with self-repairing property. Relevant researches show that compared with a pure epoxy coating, the protection efficiency and the effective use time of the self-repairing coating are obviously improved.
In the prior art, a heavy metal such as chromium or thiazole corrosion inhibitor is often added into a coating to endow the coating with self-repairing performance, but the coating has poor protection efficiency and is easy to cause environmental pollution, so that a safe and environment-friendly nano filler capable of effectively improving the self-repairing performance of the coating is urgently needed.
Disclosure of Invention
Aiming at the problems, the invention aims to provide a VPC nano composite material with self-repairing performance and a preparation method of a coating thereof, and the VPC nano composite material is applied to the field of anticorrosive coatings to improve the self-repairing performance of the coating.
The technical scheme of the invention is as follows:
in one aspect, a preparation method of a VPC nanocomposite having self-healing properties is provided, comprising the steps of:
adding vanadium pentoxide particles into deionized water to form a suspension A;
dropwise adding aniline monomer and phytic acid into the suspension A, and uniformly stirring in an ice bath to obtain a suspension B;
adding an oxidant into the suspension B, and then reacting for more than 3 hours in an ice bath to obtain a product C;
filtering the product C, repeatedly washing the product C with deionized water and ethanol, and drying to obtain a product D;
adding the product D into deionized water to form a suspension E;
adding ferric chloride and a tannic acid solution into the suspension E, stirring for reaction, and then performing centrifugal separation to obtain a product F;
and washing the product F by using deionized water, and drying to obtain the VPC nano composite material.
Preferably, the concentration of the suspension A is 8.0-15.0mg/mL, the dosage of the aniline monomer is 8.0-12.0mg/mL, the dosage of the phytic acid is 8.0-14.0mg/mL, the dosage of the oxidant is 9.0-14.0mg/mL, the concentration of the suspension E is 1.0-3.0mg/mL, the dosage of the ferric chloride solution is 0.15-0.3mg/mL, and the dosage of the tannic acid is 2-4 times of the dosage of the ferric chloride solution. More preferably, the concentration of the suspension A is 10.0mg/mL, the dosage of the aniline monomer is 11.0mg/mL, the dosage of the phytic acid is 9.0mg/mL, the dosage of the oxidant is 12.0mg/mL, the concentration of the suspension E is 2.0mg/mL, the dosage of the ferric chloride solution is 0.2mg/mL, and the dosage of the tannic acid is 0.5 mg/mL.
Preferably, after the vanadium pentoxide particles are added into the deionized water, the suspension A is uniformly dispersed by ultrasonic oscillation for more than 0.5 hour.
Preferably, the aniline monomer and the phytic acid are added dropwise by a dropwise adding method.
Preferably, the temperature of the ice bath is less than 5 ℃, and more preferably, the temperature of the ice bath is maintained at 0 ℃.
Preferably, the oxidant is ammonium persulfate.
Preferably, the addition of the oxidizing agent is carried out after the suspension B has been stirred for 30 min.
In another aspect, there is also provided a method for preparing a VPC nanocomposite coating having self-healing properties, comprising the steps of:
respectively weighing the waterborne epoxy resin and the curing agent, and uniformly stirring to obtain uniformly dispersed base materials;
weighing the VPC nano composite material prepared by any one of the preparation methods as a nano filler of the base material;
mixing the base material and the nano filler, and stirring to form uniformly dispersed mixed coating;
and uniformly spraying the coating on the pretreated metal substrate, and curing to obtain the VPC/epoxy resin nano composite coating.
Preferably, the curing agent is a mixture of ethylenediamine, diethylenetriamine and triethylenetetramine.
Preferably, the weight ratio of the water-based epoxy resin to the curing agent is 2:1, and the nano filler accounts for 0.5-1.0% of the mass of the mixed coating; more preferably, the nanofiller comprises 1.0% by mass of the mixed coating.
Compared with the prior art, the invention has the following advantages:
according to the invention, the environment-friendly vanadium pentoxide is used as an effective substitute of hexavalent chromium, and the binding force of the vanadium pentoxide and the epoxy resin is improved through polymer modification; the polymer is polyaniline for modifying, the cost is low, and the metal passivation capability of the modified filler is improved through the unique reversible redox characteristic of polyaniline, so that the polyaniline has self-activating propertyA repair capability; by tannic acid with Fe3+The tannin-Fe complex is complexed to form a tannin-Fe complex, then the tannin-Fe complex is loaded on the surface of polyaniline modified vanadium pentoxide particles, and a tannin corrosion inhibitor is accurately released to prevent corrosion by responding the change of pH when micro-area corrosion occurs through the tannin-Fe complex, so that the self-repairing protection of the polyaniline modified vanadium pentoxide is more uniform, and the response is rapidly carried out when the polyaniline modified vanadium pentoxide is damaged by pitting corrosion; in conclusion, the VPC/epoxy resin coating is environment-friendly, has double self-repairing protection effects of oxidation passivation and corrosion inhibitor activity inhibition on the metal substrate, effectively inhibits and blocks corrosion on the metal substrate, and enhances the corrosion resistance of the coating. On the other hand, certain passive blocking is realized and the propagation path of corrosive media is prolonged by effectively dispersing the nano material in the coating and bonding the amino group on the polyaniline with the epoxy group in the coating, so that the corrosion resistance and the permeation resistance of the VPC/epoxy resin coating are improved.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without creative efforts.
FIG. 1 is a schematic representation of the scanning electron microscope results of the VPC nanocomposite of the invention;
FIG. 2 is a schematic infrared spectrum of a VPC nanocomposite of the present invention;
FIG. 3 is a schematic X-ray diffraction diagram of a VPC nanocomposite material according to the present invention;
FIG. 4 is a schematic representation of X-ray photoelectron spectroscopy analysis of a VPC nanocomposite material according to the present invention;
FIG. 5 is a schematic diagram of the measurement results of the electrochemical workstation of the VPC/epoxy resin nanocomposite coating of the present invention after 60 days immersion: wherein a is a blank WEPs coating and b is V2O5Coating of/WEPs, c is V2O5Coating of @ PANI/WEPs and coating of d VPC/WEPsA layer;
FIG. 6 is a schematic diagram of the results of the electrochemical workstation measurements of the scratch treatment of the VPC/epoxy nanocomposite coating of the present invention: wherein a is a blank WEPs coating and b is V2O5Coating of/WEPs, c is V2O5@ PANI/WEPs coating, d is VPC/WEPs coating;
FIG. 7 is a schematic illustration of the polarization curve of a VPC/epoxy nanocomposite coating of the invention;
FIG. 8 is a schematic diagram of the determination results of the salt spray test of the VPC/epoxy resin nanocomposite coating of the invention: WEPs coatings wherein a and g are blanks, b and h are V2O5Coating of/WEPs, c and i being V2O5@ PANI/WEPs coating, VPC/WEPs coating with d-f and j-l of 0.5 wt.%, 1.0 wt.% and 1.5 wt.%, respectively.
Detailed Description
The invention is further illustrated with reference to the following figures and examples. It should be noted that, in the present application, the embodiments and the technical features of the embodiments may be combined with each other without conflict. Unless defined otherwise, technical or scientific terms used in the present disclosure should have the ordinary meaning as understood by those of ordinary skill in the art to which the present disclosure belongs. The use of the terms "comprising" or "including" and the like in the disclosure of the present invention means that the element or item appearing before the term covers the element or item listed after the term and its equivalents, without excluding other elements or items.
Example 1
A preparation method of a VPC/epoxy resin nano composite coating with a passivation/activity inhibition dual self-repairing function comprises the following steps:
(1) preparation of the base stock
20g of commercially available waterborne epoxy resin (WEP) and 10g of amine curing agent (WTF) are respectively weighed, mixed at room temperature, and fully stirred (400r/min for 15min) to obtain uniformly dispersed base materials. The main components of the curing agent are Ethylenediamine (EDA), Diethylenetriamine (DTA) or Triethylene Tetramine (TTA).
(2) Preparation of VPC nanocomposites
First, 1.0g of V was weighed2O5The nanoparticles are added into 100mL of deionized water and subjected to ultrasonic treatment for 0.5 hour to ensure that V is formed2O5The nanoparticles are uniformly dispersed. 1.0mL of aniline monomer and 50% phytic acid were added dropwise to the dispersion and mixed well with rapid stirring in an ice bath. After stirring for 30min, an oxidizing agent (ammonium persulfate) was added, and then, the reaction was continued at a temperature of 5 ℃ or less for 3 hours. The product was filtered and washed repeatedly with deionized water and ethanol to obtain V after 2 days of drying2O5@ PANI nanoparticles. Thereafter, FeCl was added at room temperature3And tannic acid solution 2mg/mL V2O5@ PANI suspension. The mixture was stirred vigorously and reacted on a magnetic stirrer for 1 minute, and the product was separated by centrifugation and washed with deionized water to remove excess reactants. Obtaining the final V by drying2O5@ PANI @ Fe-TA (3) (VPC) nanoparticles.
(3) Preparation of self-repairing VPC/epoxy resin nano composite coating
Weighing a proper amount of base material and VPC nano composite material, mixing, and fully stirring for 30 minutes under an electric stirrer to form the uniformly dispersed VPC/WEPs nano composite coating. The mixed paint is moved into a spray gun, and the paint is uniformly sprayed on the processed steel sheet under high pressure. The obtained sample was cured at normal temperature for 7 days to obtain the desired VPC/epoxy nanocomposite coating.
Examples of the experiments
VPC/WEPs nano composite coating with the content of 0.5 wt.%, 1.0 wt.% and 1.5 wt.% are prepared by the method respectively. 1.0 wt.% of V was also prepared separately by the same method2O5WEPs and V2O5@ PANI/WEPs composite coating. And (3) transferring the prepared composite coating into a spray gun, and uniformly spraying the composite coating on the pre-polished base steel sheet under high pressure. After the spraying, the coated steel sheet was cured at room temperature for 7 days. The clear epoxy coating is referred to herein as a blank sample.
(1) Observing the prepared V by adopting JSM-6700 scanning electron microscope2O5Of the material @ PANI @ Fe-TA (3)The dimensional morphology and the result are shown in the attached figure 1. As can be seen in FIG. 1d, the modified VPC nanocomposite behaves as a 100-200nm ellipsoid. The internal structure of the material was observed by JEM-2100F transmission electron microscopy, and modified V is shown in FIG. 1a2O5Two-phase structure of @ PANI, V2O5It is dark tubular, and light spherical for PANI. In addition, as shown in FIGS. 1b and 1c, a rough thin layer appeared on the surface of the VPC particles, presumably deposition of Fe-TA (3) complex. The VPC nanocomposites prepared have a better spherical structure overall.
(2) The chemical composition and phase structure of the VPC nano material are analyzed and researched by FT-IR, XRD, XPS and the like, and the results are shown in figures 2-4. From fig. 2-4, the generation of carbon-nitrogen single bond or double bond, carbon-hydrogen bond and hydroxyl group corresponding to tannic acid on the surface of the nanomaterial corresponding to PANI can be observed. The phase structure remaining substantially unchanged indicates that there is no internal V in the process2O5Causing damage. In addition, the appearance of the P element and the Fe element respectively corresponds to the complexing ferric iron in the loading process of the phytic acid and the tannic acid doped in the aniline polymerization process. These results demonstrate in different respects the preparation of VPC nanofillers.
(3) The coated samples were tested using the CS350 electrochemical workstation and the results are shown in FIGS. 5-7. As can be seen in FIG. 5, the largest radius of resistance of the VPC/WEPs coating was observed after more than 60 days of soaking. Shows that the corrosion resistance of the coating is obviously better than that of the coating added with V under the condition of adding VPC filler2O5，V2O5@ PANI filler and blank epoxy coating. The electrochemical test results after the coating was artificially scratched are shown in fig. 6, and compared with other coating samples with rapidly decreasing impedance, the impedance of the test sample added with the VPC composite coating after 72h is rather higher than the initial test result, and a remarkable self-repairing protection effect is shown. And it can be seen from the polarization curve (fig. 7) and its fitting parameters (table 1) that after 2 days of immersion, the corrosion current density of the VPC/WEPs epoxy composite coating is much lower than that of the other samples. It is illustrated that after the VPC nanocomposite of the invention is added to an epoxy coating in a suitable ratio,the self-repairing performance and the corrosion resistance of the epoxy resin coating can be effectively improved.
TABLE 1 fitting parameters
(4) The corrosion resistance of the coating samples was tested using the salt spray test and the results are shown in figure 8. As can be seen from fig. 8, after 300h of salt spray treatment, a coating of 1.0 wt.% VPC/WEPs was observed with the lowest corrosion, significantly better than the VPC/WEPs coating in the ratio of 0.5 wt.% to 1.5 wt.%, and the other three coatings used for the control.
Although the present invention has been described with reference to a preferred embodiment, 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. A preparation method of a VPC nano composite material with self-repairing performance is characterized by comprising the following steps:
adding vanadium pentoxide particles into deionized water to form a suspension A;
dropwise adding aniline monomer and phytic acid into the suspension A, and uniformly stirring in an ice bath to obtain a suspension B;
adding an oxidant into the suspension B, and then reacting for more than 3 hours in an ice bath to obtain a product C;
filtering the product C, repeatedly washing the product C with deionized water and ethanol, and drying to obtain a product D;
adding the product D into deionized water to form a suspension E;
adding ferric chloride and a tannic acid solution into the suspension E, stirring for reaction, and then performing centrifugal separation to obtain a product F;
and washing the product F by using deionized water, and drying to obtain the VPC nano composite material.
2. The method of preparing a VPC nanocomposite with self-healing properties according to claim 1, wherein the concentration of the suspension a is 8.0-15.0mg/mL, the amount of aniline monomer is 8.0-12.0mg/mL, the amount of phytic acid is 8.0-14.0mg/mL, the amount of oxidant is 9.0-14.0mg/mL, the concentration of the suspension E is 1.0-3.0mg/mL, the amount of ferric chloride solution is 0.15-0.3mg/mL, and the amount of tannic acid is 2-4 times the amount of ferric chloride solution.
3. The preparation method of a VPC nanocomposite with self-healing properties according to claim 1, wherein the suspension A is uniformly dispersed by ultrasonic oscillation for more than 0.5 hours after adding vanadium pentoxide particles to deionized water.
4. The method of preparing a VPC nanocomposite with self-healing properties according to claim 1, wherein the aniline monomer and phytic acid are added dropwise in a dropwise manner.
5. A process for the preparation of VPC nanocomposites with self-healing properties according to claim 1, characterized in that the temperature of the ice bath is less than 5 ℃.
6. A method of preparing a VPC nanocomposite with self-healing properties according to claim 1, wherein the oxidant is ammonium persulfate.
7. A preparation method of VPC nanocomposite with self-healing properties according to claim 6, wherein the addition of the oxidizing agent is performed after the suspension B is stirred for 30 min.
8. A preparation method of a VPC nano composite material coating with self-repairing performance is characterized by comprising the following steps:
respectively weighing the waterborne epoxy resin and the curing agent, and uniformly stirring to obtain uniformly dispersed base materials;
weighing the VPC nanocomposite prepared by the preparation method of any one of claims 1-7 as a nanofiller of the base material;
mixing the base material and the nano filler, and stirring to form uniformly dispersed mixed coating;
and uniformly spraying the coating on the pretreated metal substrate, and curing to obtain the VPC/epoxy resin nano composite coating.
9. The method for preparing a VPC nanocomposite coating with self-healing properties according to claim 8, wherein the curing agent is a mixture of ethylenediamine, diethylenetriamine and triethylenetetramine.
10. The preparation method of a VPC nanocomposite coating with self-healing properties according to claim 8, wherein the weight ratio of the waterborne epoxy resin to the curing agent is 2:1, and the nanofiller is 0.5-1.0% of the mass of the hybrid coating.
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| CN113979646A (en) * | 2021-11-25 | 2022-01-28 | 山东大学 | Multicolor electrochromic composite film and preparation method and application thereof |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113248960A (en) * | 2021-05-26 | 2021-08-13 | 西南石油大学 | Nano container filler with multiple self-repairing and anti-corrosion functions and application thereof |
| CN113248960B (en) * | 2021-05-26 | 2022-02-01 | 西南石油大学 | Nano container filler with multiple self-repairing and anti-corrosion functions and application thereof |
| CN113979646A (en) * | 2021-11-25 | 2022-01-28 | 山东大学 | Multicolor electrochromic composite film and preparation method and application thereof |
| CN116239931A (en) * | 2023-02-10 | 2023-06-09 | 西南石油大学 | Preparation of phytic acid complexing copper ion h-BN based water-based epoxy intumescent fire-retardant coating |
| CN116239931B (en) * | 2023-02-10 | 2024-01-30 | 西南石油大学 | Preparation of phytic acid complexing copper ion h-BN based water-based epoxy intumescent fire-retardant coating |
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| CN111732849B (en) | 2022-02-08 |
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