CN113248960B - Nano container filler with multiple self-repairing and anti-corrosion functions and application thereof - Google Patents
Nano container filler with multiple self-repairing and anti-corrosion functions and application thereof Download PDFInfo
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Abstract
本发明公开了一种具有多重自修复防腐功能的纳米容器填料，该纳米容器填料的制备方法主要包括两个步骤：首先制备空心聚苯胺胶囊：将五氧化二钒加入去离子水中，滴加苯胺单体和硫酸，在冰浴中搅拌混匀，再加入氧化剂，在冰浴中反应，得到产物C；将产物C分散在H2SO4溶液中，在90℃下搅拌反应24h，离心分离，干燥，得到空心聚苯胺胶囊；其次，制备纳米容器填料：石墨相氮化碳和空心聚苯胺胶囊结合成三维的纳米载体，纳米载体上负载BTA缓蚀剂，然后在表面包覆聚多巴胺层，得到可在水性涂料中通用的纳米容器填料。本发明中选择水性环氧涂料与纳米容器填料复合形成涂层。该复合涂层同时具有钝化、抑制多重自修复性质和高抗渗透性能，对金属保护效果良好。
The invention discloses a nano-container filler with multiple self-repairing and anti-corrosion functions. The preparation method of the nano-container filler mainly includes two steps: firstly preparing hollow polyaniline capsules: adding vanadium pentoxide into deionized water, adding aniline dropwise The monomer and sulfuric acid were stirred and mixed in an ice bath, then an oxidant was added, and the reaction was carried out in an ice bath to obtain product C; product C was dispersed in H 2 SO 4 solution, stirred and reacted at 90 ° C for 24 h, centrifuged, drying to obtain hollow polyaniline capsules; secondly, preparation of nano-container fillers: graphite phase carbon nitride and hollow polyaniline capsules are combined into a three-dimensional nano-carrier, BTA corrosion inhibitor is loaded on the nano-carrier, and then a polydopamine layer is coated on the surface, The result is a nanocontainer filler that can be used universally in waterborne coatings. In the present invention, the water-based epoxy coating and the nano-container filler are selected to be composited to form a coating. The composite coating has the properties of passivation, inhibition of multiple self-healing and high penetration resistance at the same time, and has a good effect on metal protection.
Description
Technical Field
The invention relates to the technical field of pigment and filler for an anticorrosive coating, in particular to a nano container filler with multiple self-repairing anticorrosive functions and an application method 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 application, due to Cl and O2、CO2And the like, the single epoxy coating, particularly the waterborne epoxy coating, often loses the protective capability for 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 water-based epoxy coating, the protection efficiency and the effective use duration of the self-repairing coating are obviously improved.
In the prior art, most of the used self-repairing fillers are mesoporous silica or halloysite nanotubes and the like which load active materials, but the self-repairing fillers have low active substance proportion and low load capacity and can only maintain the protection effect in a short time. Meanwhile, the single inhibition effect is difficult to meet the requirements of complex conditions in the industry. Therefore, there is a need for a nanofiller that can enhance the protective properties of aqueous coatings from a variety of angles and provide self-healing properties to the coatings over a long period of time to promote the development of industrial aqueous self-healing coatings.
Disclosure of Invention
The invention aims to provide a nano container filler with multiple self-repairing and anti-corrosion functions and an application method thereof, aiming at the defects of the existing self-repairing coating.
The preparation method of the nano-container filler with the multiple self-repairing anticorrosion functions provided by the invention comprises two main steps:
step one, preparing a hollow polyaniline capsule, which comprises the following specific operations:
(1) adding vanadium pentoxide particles into deionized water to form a suspension A; the concentration of vanadium pentoxide in the suspension A is 8.0-15.0 mg/mL.
(2) And (3) dropwise adding aniline monomer and concentrated sulfuric acid into the suspension A successively, and stirring and uniformly mixing in an ice bath (0 ℃) to obtain suspension B. In the reaction liquid, the concentration of aniline monomer is 8.0-12.0mg/mL, and the concentration of concentrated sulfuric acid is 8.0-14.0 mg/mL.
(3) Adding oxidant ammonium persulfate into the suspension B, controlling the concentration of the oxidant to be 9.0-14.0mg/mL, and reacting in an ice bath for more than 3 hours to obtain a product C.
(4) Product C was ultrasonically dispersed in 6 wt.% H2SO4Obtaining dispersion liquid D in the solution;
(5) stirring the dispersion liquid D at 90 ℃ for about 24 hours to etch the vanadium pentoxide core, wherein the stirring speed is 400r/min in the etching process to obtain a dispersion liquid E, centrifugally separating, repeatedly washing with deionized water and ethanol, and drying to obtain the hollow polyaniline capsule (MP for short).
Step two, preparing nano container filler, CPAA for short. The specific operation is as follows:
(1) and adding the graphite-phase carbon nitride nanosheets into deionized water, and treating for 10min at 500W by using an ultrasonic probe to obtain a dispersion liquid F. The concentration of the graphite-phase carbon nitride in the dispersion liquid F is 10.0-25.0 mg/mL. And adding the hollow polyaniline capsules into the dispersion liquid F, performing ultrasonic dispersion, and treating the dispersion liquid F for 10min at 500W by using an ultrasonic probe to obtain a dispersion liquid G. The mass ratio of the graphite phase carbon nitride to the hollow polyaniline capsule is 1: 1.
(2) Adding the BTA corrosion inhibitor into the dispersion G, carrying out load reaction for 12 hours under the vacuum (0.08MPa), centrifuging, and washing to obtain an intermediate product H. The concentration of the BTA corrosion inhibitor in the reaction liquid is controlled to be 5.0-30.0 mg/mL.
(3) And dispersing the intermediate product H in an aqueous solution of which the pH value is 8.5 and which is prepared by Tris-HCl buffer solution, adding dopamine, reacting for 12 hours to obtain a suspension I, and performing centrifugal separation and drying to obtain the nano container filler CPAA. In the reaction solution, the concentration of the intermediate product H is 5.0mg/mL, the concentration of dopamine is 1.0-4.0mg/mL, and the concentration of Tris-HCl solution is 1.0-1.5 mg/mL.
Preferably, the concentration of vanadium pentoxide in the suspension A is 10.0 mg/mL; the concentration of aniline monomer in the reaction liquid in the step one (2) is 11.0mg/mL, and the concentration of sulfuric acid is 9.0 mg/mL; controlling the concentration of an oxidant to be 12.0mg/mL in the first step (3); the concentration of graphite-phase carbon nitride in the dispersion liquid F is 20.0 mg/mL; the concentration of the BTA corrosion inhibitor solution in the reaction liquid in the step two (2) is 10.0 mg/mL; the concentrations of dopamine and Tris-HCl in the reaction solution of the step two (3) are respectively 2mg/mL and 1.2mg/mL, and the concentration of the intermediate product H is 5.0 mg/mL.
The invention provides an application method of nano container filler CPAA, which comprises the following steps:
and uniformly stirring and mixing the waterborne epoxy resin and the curing agent, wherein the weight ratio of the waterborne epoxy resin to the curing agent is 2:1, so as to obtain the base material.
And mixing the nano container filler CPAA with the base material and stirring to form the composite coating.
And (3) uniformly spraying the composite coating on the pretreated metal substrate, and curing to obtain the CPAA/epoxy resin nano composite coating with the multiple self-repairing and anti-corrosion functions. The curing agent is a mixture of ethylenediamine, diethylenetriamine and triethylene tetramine.
The nano container filler CPAA accounts for 0.5-1.5% of the mass of the composite coating; preferably, the nano container filler accounts for 1.0 percent of the mass of the composite coating.
Compared with the prior art, the invention has the advantages that:
the invention adopts two-dimensional lamellar graphite phase carbon nitride (g-C) with strong adsorbability3N4) And the hollow polyaniline capsule (MP) is combined into a three-dimensional nano carrier through the pi-pi chemical bond action to load the BTA corrosion inhibitor. Because of the large cavity of the whole materialThe accumulated and abundant functional groups and the pi-pi effect have strong adsorption capacity on BTA, so that the capacity of the container for integrally loading the corrosion inhibitor is remarkably improved compared with the traditional container such as halloysite nanotubes, hydrotalcite and the like.
And, in g-C of preparation3N4The @ PANI @ BTA is used as a template, and the surface of the template is coated with a polydopamine layer, so that on one hand, the compatibility of the nano container and resin is enhanced, and meanwhile, a certain pH response effect is given to the nano container, so that the corrosion inhibitor can be accurately released under the stimulation of an external environment where corrosion occurs, and further damage of the corrosion to a metal substrate is prevented.
Meanwhile, the g-C is used as a three-dimensional nano container carrier composition structure3N4And MP, besides being used for loading the corrosion inhibitor, the MP also serves as a two-dimensional sheet layer and a conductive polymer, plays a role in enhancing the barrier property of the coating and endowing the coating with passivation and self-repairing properties in resin, and delays the process that a corrosion medium reaches the surface of the metal through the coating and corrodes the metal.
Therefore, the nano container filler has obviously higher loading capacity on the corrosion inhibitor than that of the traditional container, and also has triple self-repairing protection performance of passivation/activity inhibition/obstruction, so that the long-term protection capability of the CPAA/waterborne epoxy coating on metal is greatly improved.
Additional advantages, objects, and features of the invention will be set forth in part in the description which follows and in part will become apparent to those having ordinary skill in the art upon examination of the following or may be learned from practice of the invention.
Drawings
FIG. 1 is a flow chart of the preparation concept of the three-dimensional CPAA nano-container filler of the present invention.
FIG. 2 is a schematic transmission electron microscope of a three-dimensional CPAA nano container-like filler of the present invention.
Figure 3 is an X-ray diffraction pattern of a three-dimensional CPAA-like nanocompartment filler of the present invention.
FIG. 4 is a schematic diagram of X-ray photoelectron spectroscopy analysis of a three-dimensional CPAA-like nano-container filler of the present invention.
Figure 5 is a uv-vis spectroscopy analysis of BTA loading for three-dimensional CPAA-like nano-container filler of the present invention.
FIG. 6 is a schematic diagram showing the open circuit potential change of the CPAA/waterborne epoxy self-healing composite coating of the present invention.
FIG. 7 is a schematic diagram of the measurement results of the electrochemical workstation in which the CPAA/waterborne epoxy self-repairing composite coating of the invention is soaked for 80 days: wherein a is a blank WEPs coating, b is an MP/WEPs coating, c is a CP/WEPs coating, and d is a CPAA/WEPs coating.
FIG. 8 is a schematic diagram of the results of the electrochemical workstation measurement of the CPAA/waterborne epoxy self-healing nanocomposite coating scratch treatment of the present invention: wherein a and b are blank WEPs coatings, c and d are MP/WEPs coatings, e and f are CP/WEPs coatings, and g and h are CPAA/WEPs coatings.
FIG. 9 is a schematic diagram of the measurement results of the CPAA/waterborne epoxy self-healing composite coating salt spray experiment of the present invention: wherein a and b are blank WEPs coatings, c and d are MP/WEPs coatings, e and f are CP/WEPs coatings, and g and h are CPAA/WEPs coatings.
Detailed Description
The preferred embodiments of the present invention will be described in conjunction with the accompanying drawings, and it will be understood that they are described herein for the purpose of illustration and explanation and not limitation.
Example 1
A preparation method of nano-container filler CPAA with multiple self-repairing anticorrosion functions is disclosed, wherein the flow schematic diagram is shown in figure 1, and the specific method comprises the following steps:
step one, preparing a hollow polyaniline capsule, which comprises the following specific operations:
(1) weighing 1.0g of V2O5The nanoparticles are added into 100mL of deionized water and subjected to ultrasonic treatment for 0.5 hour to ensure that V is formed2O5The nanoparticles were homogeneously dispersed to form suspension a.
(2) And (3) dropwise adding 1.0mL of aniline monomer and 1.0mL of concentrated sulfuric acid into the suspension A, rapidly stirring and uniformly mixing in an ice bath, and stirring for 30min to obtain a suspension B.
(3) Adding an oxidant (ammonium persulfate) into the suspension B, and continuing to react for 3 hours at the temperature below 5 ℃; the product was filtered and washed repeatedly with deionized water and ethanol, dried for 2 daysObtaining V2O5@ PANI (VP) composite material.
(4) Ultrasonically dispersing 0.5g of VP composite material in H with the mass percentage concentration of 6%2SO4To obtain a homogeneous dispersion D;
(5) dispersion D was transferred to a 250mL three-necked flask, and stirred at 400rpm at 90 ℃ for about 24 hours to etch away internal V2O5Core to obtain dispersion E; centrifuging at 9000r/min and repeatedly washing with deionized water and ethanol, and finally freeze-drying the obtained precipitate to obtain hollow polyaniline capsule product (MP).
Step two, preparing nano container filler, CPAA for short. The specific operation is as follows:
(1) the mass ratio of the graphite phase carbon nitride to the hollow polyaniline capsule is 1: 1. The g-C with good dispersity is obtained by stripping dicyandiamide through thermal oxidation3N4Two-dimensional nanosheets. 0.1g of g-C3N4Adding the nanosheet into 50mL of deionized water, ultrasonically dispersing for 10min at 500W by using an ultrasonic probe, then adding 0.1G of MP, and continuously ultrasonically treating for 10min to obtain a dispersion liquid G, wherein the dispersion liquid G contains a product CP (G-C)3N4@MP)。
(2) Adding the BTA corrosion inhibitor into the dispersion G, carrying out load reaction for 12 hours under the vacuum (0.08MPa), centrifuging, and washing to obtain an intermediate product H. The concentration of BTA corrosion inhibitor in the reaction solution was controlled to 10.0 mg/mL.
(3) And dispersing the intermediate product H in an aqueous solution of Tris-HCl buffer solution with the pH value of 8.5, adding 3mM dopamine, continuing to react for 12 hours, centrifuging at 12000r/min, washing the product with deionized water, and freeze-drying to obtain the nano container filler CPAA.
Example 2
An application method of nano-container filler CPAA with multiple self-repairing anticorrosion functions 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 (600r/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 CPAA/waterborne epoxy self-repairing composite coating
The appropriate amount of base material and the nano-container filler CPAA prepared in example 1 were weighed, mixed and stirred thoroughly for 30 minutes with an electric stirrer to form a uniformly dispersed CPAA/WEPs composite coating.
(3) Preparation of the coating
And (3) moving the composite coating into a spray gun, and uniformly spraying the coating on the treated steel sheet under high pressure. The resulting sample was cured at ambient temperature for 7 days to obtain the desired CPAA/epoxy nanocomposite coating.
And (3) performance testing:
CPAA/WEPs composite coatings were prepared according to the method of example 2, with CPAA accounting for 0.5 wt.%, 1.0 wt.%, 1.5 wt.% of the composite coating by mass, respectively. MP/WEPs and CP/WEPs composite coatings with the mass percent of 1.0 wt.% are also prepared by the same method respectively. MP refers to the hollow polyaniline capsule product, prepared by step one of example 1. CP means g-C3N4Conjugation with MP, by step two (1) of example 1. The prepared composite coating is moved into a spray gun and evenly sprayed 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. Pure water epoxy coatings (BlankWEPs) are referred to herein as blank samples.
(1) The morphology and the size of the nano-container filler CPAA are observed by adopting a JEM-2100F transmission electron microscope, and the result is shown in figure 2. In the figure, (a) represents VP and (b) represents MP (open PANI); (c) represents g-C3N4And (d) represents CP; (e) and (f) both represent CPAA. It can be seen that g-C is due to3N4The pi-pi chemical bond interaction with MP can be observed in the originally smooth g-C3N4The layer (fig. 2c) shows a number of oval capsule structures (fig. 2d), it is noted that it can also be observed that the majority of these capsules still maintain a hollow structure, which indicates the polyaniline hollows in fig. 2b during the preparation processThe structure is not damaged, and is at C3N4Is relatively uniform. Furthermore, in CPAA (fig. 2e and 2f)), the structure of this sheet/capsule stack is still clearly visible, unlike CP, where the hollow structure is clearly absent, indicating that BTA molecules are filled into the material. At the same time, an overlying layer of organic matter was also observed due to the coating of the PDA, indicating the encapsulation process of the PDA for the material as a whole. Thereby verifying the successful preparation of CPAA nanocompartments. In addition, the physical crystal structure and specific chemical composition of the synthesized material were characterized by XRD and XPS analysis of fig. 3 and 4.
(2) The loading of the corrosion inhibitor BTA in CPAA nano-containers was determined by UV-Vis analysis and the results are shown in fig. 5. Wherein each of the graphs (a) and (b) is a release graph. The graph shows that different release rates are exhibited at different pH conditions. Wherein, according to the quantitative analysis of the solution with 1mg/mL, the final release amount is about 17.64% in 48h under the condition of pH 3.
(3) The coated samples were tested using the CS350 electrochemical workstation and the results are shown in fig. 6-8. As can be seen in fig. 7, the maximum radius of resistance of the CPAA/WEPs coating is observed after more than 80 days of soaking. The anticorrosion performance of the coating is obviously better than that of the epoxy coating added with MP, CP filler and blank under the condition of adding CPAA filler. The electrochemical test results after the coating was artificially scratched are shown in fig. 8, and the resistance of the test sample added with the CPAA composite coating at 48h is rather higher than the initial test results, compared with other coating samples with rapidly decreasing resistance, showing a significant self-healing protection effect. In addition, as can be seen in fig. 6, due to the blocking effect of the three-dimensional container with a high aspect ratio and the synergistic self-repair effect of the BTA corrosion inhibitor and passivation, it can be observed that the composite coating loaded with 1.0 wt.% of cpa shows a lower decreasing trend and a higher increasing trend respectively at the early stage and the later stage, and shows the most positive OCP value in the whole process. The CPAA nano container filler disclosed by the invention is added into a water-based epoxy coating in a proper proportion, so that the self-repairing performance and the corrosion resistance of the coating can be effectively improved.
(4) The corrosion resistance of the coated samples was tested using the salt spray test and the results are shown in figure 9. It can be seen that after 300h of salt spray treatment, the 1.0 wt.% CPAA/WEPs coating corroded the least, significantly better than the other three coatings used for the control.
In conclusion, the nano container filler CPAA provided by the invention is combined with the epoxy coating to form a coating, so that the multiple self-repairing and corrosion-resisting properties of passivation/inhibition/barrier are enhanced, and the protection effect of the nano container filler CPAA on metal is enhanced.
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 (9)
1. A nano-container filler with multiple self-repairing anticorrosion functions is characterized in that the preparation method of the nano-container filler comprises the following steps:
s1, preparing the hollow polyaniline capsule, comprising the following substeps:
s11, adding vanadium pentoxide into deionized water to form a suspension A;
s12, dropwise adding aniline monomer and concentrated sulfuric acid into the suspension A, and uniformly stirring in an ice bath to obtain a suspension B;
s13, adding an oxidant ammonium persulfate into the suspension B, and reacting for more than 3 hours in an ice bath to obtain a product C;
s14, ultrasonically dispersing the product C in H with the mass percentage concentration of 6%2SO4Obtaining dispersion liquid D in the solution;
s15, stirring and reacting the dispersion liquid D at 90 ℃ for 24 hours to etch vanadium pentoxide cores to obtain a dispersion liquid E, and centrifugally separating, cleaning and drying to obtain hollow polyaniline capsules;
s2, preparing nano container filler: the graphite-phase carbon nitride and the hollow polyaniline capsule are combined to form a three-dimensional nano carrier, the BTA corrosion inhibitor is loaded on the nano carrier, and then the surface of the nano carrier is coated with a polydopamine layer to obtain the nano container filler.
2. The nano-container filler with multiple self-repairing and anti-corrosion functions as claimed in claim 1, wherein in step S12, aniline monomer and concentrated sulfuric acid are sequentially added dropwise in a dropwise manner.
3. The nano-container filler with multiple self-repairing corrosion prevention functions of claim 1, wherein the ice bath temperature in the step S12 is maintained at 0 ℃.
4. The nano-container filler with multiple self-healing and corrosion-prevention functions of claim 1, wherein the step S2 includes the following substeps:
s21, dispersing the graphite-phase carbon nitride nanosheets in deionized water to obtain a dispersion liquid F, adding hollow polyaniline capsules into the dispersion liquid F, and performing ultrasonic dispersion to obtain a dispersion liquid G;
s22, adding the BTA corrosion inhibitor into the dispersion G, reacting for several hours under vacuum condition, centrifuging and washing to obtain an intermediate product H
And S23, coating a polydopamine layer on the surface of the intermediate product H to obtain the nano container filler.
5. The nano-container filler with multiple self-repairing anticorrosion functions as claimed in claim 4, wherein in the step S22, the reaction is performed for 12 hours in a vacuum atmosphere of 0.08 MPa.
6. The nano-container filler with multiple self-healing and corrosion-prevention functions of claim 4, wherein the step S23 is performed by: and dispersing the intermediate product H in an aqueous solution of which the pH value is 8.5 and which is prepared by Tris-HCl buffer solution, adding dopamine, reacting for 12 hours, centrifuging, and drying to obtain the nano container filler.
7. The application method of the nano container filler with the multiple self-repairing anticorrosion functions as claimed in any one of claims 1 to 6, wherein the nano container filler is added into the water-based epoxy resin coating.
8. The application method of the nano-container filler with the multiple self-repairing anticorrosion functions as claimed in claim 7, wherein the waterborne epoxy resin and the curing agent are uniformly stirred to obtain a base material; mixing nano container filler and base material, and uniformly stirring to form a composite coating; and (3) uniformly spraying the composite coating on a metal substrate, and curing to obtain the composite coating with multiple self-repairing anticorrosion functions.
9. The method for applying the nano-container filler with the multiple self-repairing anticorrosion functions as claimed in claim 8, wherein the curing agent is a mixture of ethylenediamine, diethylenetriamine and triethylenetetramine.
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