Study on Preparation and Performance of Acid pH-Responsive Intelligent Self-Healing Coating
Abstract
:1. Introduction
2. Experimental
2.1. Materials
2.2. Preparation of Microcapsules
- (1)
- Preparation of microcapsules: We added 300 mL deionized water, 5 g polyvinyl alcohol solution with a concentration of 5 wt%, 5 g urea, 0.5 g resorcinol, and 0.5 g ammonium chloride into a 500 mL beaker. We used a glass stirring rod to stir the mixture. After all substances were dissolved, the pH of the solution was adjusted to 3.0 using hydrochloric acid at a concentration of 1 wt%. We mixed 20 mL of linseed oil and ground benzotriazole together in an ultrasonic water bath for 10 min to mix the two evenly. The mixture was then poured into a beaker and the solution was mechanically stirred for 10 min at room temperature. When the solution was in a stable state, we slowly heated the solution to 55 °C in a water bath. We slowly added 12.67 g of formaldehyde aqueous solution with a concentration of 37 wt% into the solution and continued stirring at a speed of 500 r/min for 240 min. The suspension obtained by the reaction was cooled to room temperature and washed with deionized water, absolute ethanol, and acetone in sequence, and the prepared microcapsules were collected.
- (2)
- Construct the polyelectrolyte layer: The chitosan clarification solution with a concentration of 1.5 mg/mL was prepared first. We dispersed the microcapsules in 25 mL of chitosan solution with a concentration of 1.5 mg/mL and soaked them at 30 °C for 20 min. We added the microcapsules to a three-neck round-bottomed flask and added 5 mL of acetonitrile and 0.0068 g of α-methacrylic acid. We sealed the three ports of the flask and stirred magnetically at room temperature for 30 min. Afterwards, 5 mg of free radical initiator 2,2′-azobisisobutyronitrile and 0.0495 g of cross-linking agent ethylene glycol dimethacrylate were added to the solution, and stirring was continued for 30 min. The mixture was heated in a water bath at 60 °C for 8 h under a nitrogen atmosphere to form poly(ethylene glycol dimethacrylate-co-methacrylic acid) (EM). After cleaning the microcapsules with deionized water and ethanol, we added 25 mL of chitosan solution and soaked them at 30 °C for 20 min to obtain acidic pH-responsive microcapsules. Figure 1 is a schematic diagram of the process and structure of the microcapsules prepared in this experiment.
2.3. Preparation of Acidic pH-Responsive Self-Healing Coatings
2.4. Characterization
2.4.1. Characterization of Microcapsules
- (1)
- Calculation of encapsulation efficiency and drug loading efficiency
- (2)
- Test method for sustained release curve
- (3)
- Morphological observation
- (4)
- Fourier transform infrared spectroscopy test (FTIR)
- (5)
- Thermogravimetric analysis (TGA)
- (6)
- Zeta potential test
2.4.2. Characterization of Self-Healing Properties of Coatings
2.4.3. Characterization of Anti-Corrosion Properties of Coatings
- (1)
- Salt spray test
- (2)
- Electrochemical testing
3. Results and Discussion
3.1. Optimization of Microcapsule Preparation Process
3.1.1. Effect of Chitosan Concentration on Microcapsules
3.1.2. Effect of Polymerization Time on Microcapsules
3.1.3. Effect of Heating Temperature during Polymerization on Microcapsules
3.1.4. Effect of Number of Polyelectrolyte Layers on Microcapsules
3.2. Properties of Microcapsules
3.2.1. Microcapsule Morphology and Sustained Release Curve
3.2.2. FTIR
3.2.3. TGA
3.2.4. Zeta Potential Test
3.3. Self-Healing Properties of Coatings
3.4. Anti-Corrosion Properties of Coating
3.4.1. Research on the Anti-Corrosion Performance of the Self-Healing Coating Based on the Salt Spray Test
3.4.2. Research on Anti-Corrosion Properties of Coatings Based on Electrochemical Experiments
3.4.3. Study of the Difference in Anti-Corrosion Performance of Self-Healing Coatings in Acid and Alkali Environments
4. Conclusions
Author Contributions
Funding
Data Availability Statement
Conflicts of Interest
References
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Stage | Time (h) | Rs (Ω·cm2) | Qc (F·cm−2) | Rc (Ω·cm2) | Qdl (F·cm−2) | Rt (Ω·cm2) |
---|---|---|---|---|---|---|
Self-healing | 0 | 4493 | 8.5381 × 10−11 | 4.74 × 107 | - | - |
4 | 4672 | 6.0461 × 10−11 | 8.15 × 107 | - | - | |
8 | 6157 | 1.9 × 10−11 | 8.66 × 107 | - | - | |
Infiltration | 12 | 6559 | 9.3759 × 10−10 | 7.69 × 107 | - | - |
24 | 5793 | 1.6446 × 10−10 | 6.18 × 107 | - | - | |
48 | 6534 | 1.9379 × 10−10 | 5.30 × 107 | - | - | |
72 | 3074 | 2.3812 × 10−10 | 4.12 × 107 | - | - | |
120 | 3127 | 2.9789 × 10−10 | 4.04 × 107 | - | - | |
Failure | 168 | 2667 | 3.420 × 10−10 | 2.32 × 107 | 1.26 × 10−10 | 4.07 × 107 |
216 | 5206 | 4.6131 × 10−10 | 2.28 × 107 | 1.36 × 10−10 | 5.28 × 106 | |
264 | 2771 | 4.6644 × 10−10 | 2.14 × 107 | 3.64 × 10−10 | 7.87 × 106 | |
312 | 6636 | 4.899 × 10−10 | 7.04 × 106 | 1.32 × 10−10 | 2.05 × 106 |
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Liu, J.; Chen, F.; Zhang, Q.; Xing, X.; Cui, G. Study on Preparation and Performance of Acid pH-Responsive Intelligent Self-Healing Coating. Polymers 2024, 16, 2473. https://doi.org/10.3390/polym16172473
Liu J, Chen F, Zhang Q, Xing X, Cui G. Study on Preparation and Performance of Acid pH-Responsive Intelligent Self-Healing Coating. Polymers. 2024; 16(17):2473. https://doi.org/10.3390/polym16172473
Chicago/Turabian StyleLiu, Jianguo, Feiyu Chen, Qiaosheng Zhang, Xiao Xing, and Gan Cui. 2024. "Study on Preparation and Performance of Acid pH-Responsive Intelligent Self-Healing Coating" Polymers 16, no. 17: 2473. https://doi.org/10.3390/polym16172473