CN111849327B - preparation method of pH stimulation responsiveness intelligent self-warning self-repairing anticorrosion water-based coating - Google Patents
preparation method of pH stimulation responsiveness intelligent self-warning self-repairing anticorrosion water-based coating Download PDFInfo
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- CN111849327B CN111849327B CN202010648114.2A CN202010648114A CN111849327B CN 111849327 B CN111849327 B CN 111849327B CN 202010648114 A CN202010648114 A CN 202010648114A CN 111849327 B CN111849327 B CN 111849327B
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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
- C09D175/00—Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
- C09D175/04—Polyurethanes
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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
- 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
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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
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/65—Additives macromolecular
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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
- C09D7/70—Additives characterised by shape, e.g. fibres, flakes or microspheres
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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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2296—Oxides; Hydroxides of metals of zinc
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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 relates to the technical field of high polymer materials, and discloses a pH stimulation responsiveness intelligent self-warning and self-repairing anticorrosive water-based layer. Firstly, preparing a pH stimulus responsive organic-inorganic hybrid hollow microsphere which is low in toxicity and cost, takes a fluorescent probe and a corrosion inhibitor as cores and takes amphoteric nano particles and attapulgite as shells in one step by a Pickering emulsion photopolymerization method; and then blending the hybrid microspheres and the waterborne polyurethane by a mechanical blending method to obtain the pH stimulation responsive intelligent self-warning and self-repairing anticorrosive waterborne coating. When the pH value changes due to external stimulation, the amphoteric nano particles are dissolved, and the nano container intelligently releases the pre-stored fluorescent probe molecules and the pre-stored corrosion inhibitor molecules, so that the self-warning and self-repairing effects are achieved. The preparation process disclosed by the invention can be operated at room temperature, is simple and feasible, does not generate three wastes in the preparation process, is green and environment-friendly, and can be applied to the field of metal corrosion prevention.
Description
Technical Field
The invention relates to the field of high polymer materials, in particular to a pH stimulation responsiveness intelligent self-warning and self-repairing anticorrosive water-based coating with a pH sensitive fluorescent probe and inorganic nanoparticles as intelligent switches.
Background
The metal corrosion brings huge economic loss and social harm to human beings, and the metal materials scrapped due to corrosion are estimated to be more than 20% of the metal yield in the same year and account for about 5% of the total value of national production. The importance of metal corrosion protection is becoming increasingly prominent, with the most convenient and economical reasons for corrosion protection of coatings. The Waterborne Polyurethane (WPU) has the advantages of safety, environmental protection, good storage stability, good mechanical property and chemical resistance and the like, and becomes one of the most widely applied waterborne anticorrosive coatings at present. But it has the following problems in the metal corrosion prevention process: once the WPU coating is damaged, corrosive media directly permeate into the metal substrate, the corrosion resistance is lost, and the corrosion speed of the substrate is rapidly accelerated.
In order to solve the problems, the traditional anticorrosive coating generally adopts a method of directly doping the corrosion inhibitor, but the direct doping can cause the interaction between the corrosion inhibitor and the coating material, destroy the cohesiveness and the barrier property of the coating and reduce the activity of the corrosion inhibitor. In addition, the amount of the corrosion inhibitor which is directly added is not easy to control, and the coating can not exert effective active anticorrosion effect due to small amount; the corrosion inhibitor is released in a large amount, so that the surface of the coating is foamed, the aim of sustained release cannot be fulfilled, and the corrosion prevention effect of the coating is reduced; and timely self-warning of corrosion sites cannot be realized, and the optimal repair time is missed. Therefore, the development of the novel intelligent self-warning and self-repairing waterborne WPU anticorrosive coating can prevent and slow down corrosion, and has important significance for building conservation-oriented, low-carbon and environment-friendly society.
Disclosure of Invention
The purpose of the invention is as follows: in order to solve the problems, the invention provides a preparation method of a pH stimulus responsive intelligent self-warning and self-repairing anticorrosive water-based coating, when the pH value is changed due to external stimulus, a nano container intelligently releases pre-stored pH responsive fluorescent probe molecules and corrosion inhibitor molecules, and the self-warning and self-repairing functions are realized; the preparation process can be operated at room temperature, is simple and feasible, does not produce three wastes in the preparation process, is green and environment-friendly, and can be applied to the field of metal corrosion prevention.
The technical scheme is as follows: the invention provides a preparation method of a pH stimulation responsiveness intelligent self-warning self-repairing anticorrosive water-based coating, which is characterized by comprising the following steps of: s1: sequentially adding amphoteric inorganic nanoparticles, nano attapulgite, deionized water, an organic solvent, an acrylic monomer, fluorescent probe molecules and a corrosion inhibitor into a light-resistant container, ultrasonically dispersing for 5-10 min, adding a photoinitiator, and emulsifying for 5-30 min by high-speed stirring to form a Pickering emulsion with the synergistic stability of the amphoteric inorganic nanoparticles and the attapulgite; s2: introducing the Pickering emulsion into a photoreactor, sealing and illuminating for 5-20 min to obtain an organic-inorganic hybrid hollow microsphere suspension, and drying to obtain pH stimulus responsive organic-inorganic hybrid hollow microspheres; s3: and (3) blending the pH stimulation responsive organic-inorganic hybrid hollow microspheres with waterborne polyurethane, and coating the mixture on the surface of metal to obtain the anticorrosive coating.
Preferably, in the step S1, the weight ratio of the amphoteric inorganic nanoparticles, the nano attapulgite, the deionized water, the organic solvent, the acrylic monomer, the fluorescent probe molecules, the corrosion inhibitor and the photoinitiator is 1-3: 10-20: 30-60: 3: 3: 1-2.5: 0.8.
Preferably, in the S3, the mass ratio of the pH stimulus-responsive organic-inorganic hybrid hollow microspheres to the aqueous polyurethane is 1-10: 100.
preferably, the fluorescent probe molecule is a pH stimulus-responsive water-soluble fluorescent molecule, and the loading amount in the pH stimulus-responsive organic-inorganic hybrid hollow microsphere is 1-10 wt%.
Preferably, the details of S3 are as follows: dispersing the pH stimuli-responsive organic-inorganic hybrid hollow microspheres in acetone, ultrasonically dispersing for 20-30 min, slowly pouring the mixture into waterborne polyurethane under high-speed stirring, dispersing for 20-30 min at 500-1000 rpm to obtain a mixed solution of the pH stimuli-responsive organic-inorganic hybrid hollow microspheres and the waterborne polyurethane, and coating the mixed solution on the metal surface to form the pH stimuli-responsive intelligent self-early-warning self-repairing anticorrosive waterborne coating.
Preferably, the amphoteric inorganic nanoparticles are Al or Zn oxide or hydroxide capable of reacting with acid and alkali, and the diameter of the amphoteric inorganic nanoparticles is 20-80 nm.
Preferably, the organic solvent is toluene, n-octane, p-xylene, n-decanol or undecanol.
Preferably, the photoinitiator is 2-hydroxy-2-methyl-1-phenyl acetone, 1-hydroxy-cyclohexyl benzophenone, 2-hydroxy-2-methyl-1-p-hydroxyethyl ether phenyl acetone, 4-p-toluene mercapto benzophenone, 2,4, 6-trimethyl benzoyl-diphenyl phosphorus oxide, 2-isopropyl thioxanthone.
Preferably, the corrosion inhibitor molecule is a water-soluble inorganic corrosion inhibitor, a water-soluble organic corrosion inhibitor or a water-soluble polymer corrosion inhibitor.
Preferably, the waterborne polyurethane is a coating-specific waterborne polyurethane emulsion.
Has the advantages that: theoretically, H is either hydrogen evolution corrosion or oxygen evolution corrosion+Are all crucial inducing factors for corrosion, and OH is generated in the corrosion process-Characteristic of local micro-zone pH increase; according to the anticorrosive coating prepared by the invention, when metal is corroded, the pH of a corrosion micro-area is changed, and after the waterborne polyurethane coating is damaged, amphoteric nano particles in the shell of the pH-stimulated responsive organic-inorganic hybrid hollow microsphere are dissolved to form nano holes, so that the corrosion inhibitor and fluorescent probe molecules are slowly released, and the functions of self-warning and self-repairing are achieved. The preparation process disclosed by the invention can be operated at room temperature, is simple and feasible, does not generate three wastes in the preparation process, is green and environment-friendly, and can be applied to the field of metal corrosion prevention.
Drawings
FIG. 1 is a schematic structural view of a pH stimulation responsive intelligent self-warning and self-repairing anticorrosive water-based coating prepared by the invention;
FIG. 2 is a graph showing the release of benzotriazole molecules of pH stimuli-responsive organic-inorganic hybrid hollow microspheres at different pH values.
Detailed Description
The present invention will be described in detail with reference to the following embodiments.
Embodiment 1:
the embodiment provides a preparation method of a pH stimulation responsiveness intelligent self-warning self-repairing anticorrosive water-based coating, which comprises the following steps:
the method comprises the following steps: preparation of Pickering emulsion
Respectively weighing 0.15 g of nano ZnO and 0.15 g of nano attapulgite, adding into a brown bottle, adding 3 mL of deionized water, ultrasonically dispersing for 10 min, further adding 1 mL of monomer MMA, 1 mL of cross-linking agent EGDMA, 0.10 g of corrosion inhibitor BTA, 0.08 g of photoinitiator I819 and 5.5 mL of normal octane, and emulsifying for 10 min under the condition of 12 krpm by using an emulsifying machine to obtain the O/W type Pickering emulsion.
Step two: preparation of pH stimulation responsive organic-inorganic hybrid hollow microspheres
And pouring the prepared O/W type Pickering emulsion into a photoreactor, irradiating for 10 min to obtain polymeric slow-release hybrid microspheres, carrying out suction filtration and washing on the polymeric hybrid microspheres, and then putting the polymeric slow-release hybrid microspheres into a drying oven at 60 ℃ for drying for 24 h to obtain the pH stimulus-responsive organic-inorganic hybrid hollow microspheres.
Step three: preparation of waterborne polyurethane anticorrosive coating
And (2) dispersing 1 g of the pH stimulus responsive organic-inorganic hybrid hollow microspheres in 20 ml of acetone, ultrasonically dispersing for 20min, slowly pouring the mixture into waterborne polyurethane under high-speed stirring, dispersing for 30 min at 1000 r/min to obtain a mixed solution of the pH stimulus responsive organic-inorganic hybrid hollow microspheres and the waterborne polyurethane, and coating the mixed solution on the metal surface to form the pH stimulus responsive intelligent self-early warning and self-repairing anticorrosive waterborne coating.
Embodiment 2:
the embodiment provides a preparation method of a pH stimulation responsiveness intelligent self-warning self-repairing anticorrosive water-based coating, which comprises the following steps:
step one and step two are completely the same as embodiment 1, and are not described herein.
Step three: preparation of waterborne polyurethane anticorrosive coating
2 g of the pH stimulus responsive organic-inorganic hybrid hollow microspheres are dispersed in 20 ml of acetone, ultrasonically dispersed for 20min, slowly poured into waterborne polyurethane under high-speed stirring, and dispersed at high speed for 30 min at 1000 r/min to obtain a mixed solution of the pH stimulus responsive organic-inorganic hybrid hollow microspheres and the waterborne polyurethane, and the mixed solution is coated on the metal surface to form the pH stimulus responsive intelligent self-warning self-repairing anticorrosive waterborne coating.
Embodiment 3:
the embodiment provides a preparation method of a pH stimulation responsiveness intelligent self-warning self-repairing anticorrosive water-based coating, which comprises the following steps:
step one and step two are completely the same as embodiment 1, and are not described herein.
Step three: preparation of waterborne polyurethane anticorrosive coating
5 g of the pH stimulus responsive organic-inorganic hybrid hollow microspheres are dispersed in 20 ml of acetone, ultrasonically dispersed for 20min, slowly poured into waterborne polyurethane under high-speed stirring, and dispersed at high speed for 30 min at 1000 r/min to obtain a mixed solution of the pH stimulus responsive organic-inorganic hybrid hollow microspheres and the waterborne polyurethane, and the mixed solution is coated on the metal surface to form the pH stimulus responsive intelligent self-warning self-repairing anticorrosive waterborne coating.
In order to research the release capacity of the intelligent nano container-pH stimulation responsive organic-inorganic hybrid hollow microspheres to corrosion inhibitor molecules under different pH values, the invention designs the following experiments:
three batches of 1 mg of the pH stimuli-responsive organic-inorganic hybrid hollow microspheres prepared in embodiment 1 were weighed and placed on a semi-permeable membrane and immersed in cuvettes containing 3.5 ml of solutions with pH =4, 5, 12, respectively, to ensure that the particles were completely immersed and did not escape from the semi-permeable membrane. The release capacity of the nano container to the corrosion inhibitor benzotriazole under different pH values is inspected by detecting the change of the absorbance value of the cuvette liquid by an ultraviolet-visible spectrophotometer. As shown in FIG. 2, the release rate was different depending on the pH of the acid and the base, since the release amount was gradually increased with time. The pH stimulation responsive organic-inorganic hybrid hollow microspheres can respond to the change of pH and realize controllable release.
While the invention has been described with respect to a number of specific embodiments thereof, it will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention. The components not specified in this example can be realized by the prior art.
Claims (10)
1. A preparation method of a pH stimulation responsiveness intelligent self-warning self-repairing anticorrosion water-based coating is characterized by comprising the following steps:
s1: sequentially adding amphoteric inorganic nanoparticles, nano attapulgite, deionized water, an organic solvent, an acrylic monomer, fluorescent probe molecules and a corrosion inhibitor into a light-resistant container, ultrasonically dispersing for 5-10 min, adding a photoinitiator, and emulsifying for 5-30 min by high-speed stirring to form a Pickering emulsion with the synergistic stability of the amphoteric inorganic nanoparticles and the attapulgite;
s2: introducing the Pickering emulsion into a photoreactor, sealing and illuminating for 5-20 min to obtain an organic-inorganic hybrid hollow microsphere suspension, and drying to obtain pH stimulus responsive organic-inorganic hybrid hollow microspheres;
s3: and mixing the pH stimulus responsive organic-inorganic hybrid hollow microspheres with waterborne polyurethane, and coating the mixture on the surface of metal to obtain the pH stimulus responsive intelligent self-warning and self-repairing anticorrosive waterborne coating.
2. The preparation method of the pH stimulus responsive intelligent self-warning and self-repairing anticorrosive water-based coating according to claim 1, characterized in that: in the S1, the weight ratio of the amphoteric inorganic nanoparticles to the nano attapulgite, to the deionized water to the organic solvent to the acrylic monomer to the fluorescent probe molecules to the corrosion inhibitor to the photoinitiator is 1-3: 10-20: 30-60: 3: 3: 1-2.5: 0.8.
3. The preparation method of the pH stimulus responsive intelligent self-warning and self-repairing anticorrosive water-based coating according to claim 1, characterized in that: in the S3, the mass ratio of the pH stimulus responsive organic-inorganic hybrid hollow microspheres to the aqueous polyurethane is (1-10): 100.
4. the preparation method of the pH stimulus responsive intelligent self-warning and self-repairing anticorrosive water-based coating according to claim 1, characterized in that: the fluorescent probe molecule is a pH stimulus-responsive water-soluble fluorescent molecule, and the load capacity in the pH stimulus-responsive organic-inorganic hybrid hollow microsphere is 1-10 wt%.
5. The preparation method of the pH stimulus responsive intelligent self-warning and self-repairing anticorrosive water-based coating according to claim 1, characterized in that: the details of S3 are as follows:
dispersing the pH stimuli-responsive organic-inorganic hybrid hollow microspheres in acetone, ultrasonically dispersing for 20-30 min, slowly pouring the mixture into waterborne polyurethane under high-speed stirring, dispersing for 20-30 min at 500-1000 rpm to obtain a mixed solution of the pH stimuli-responsive organic-inorganic hybrid hollow microspheres and the waterborne polyurethane, and coating the mixed solution on the metal surface to form the pH stimuli-responsive intelligent self-early-warning self-repairing anticorrosive waterborne coating.
6. The preparation method of the pH stimulus responsive intelligent self-warning and self-repairing anticorrosive water-based coating according to claim 1, characterized in that: the amphoteric inorganic nanoparticles are Al or Zn oxide or hydroxide capable of reacting with acid and alkali, and the diameter of the amphoteric inorganic nanoparticles is 20-80 nm.
7. The preparation method of the pH stimulation responsive intelligent self-warning and self-repairing anticorrosive water-based coating according to any one of claims 1 to 6, characterized by comprising the following steps: the organic solvent is toluene, n-octane, p-xylene, n-decanol or undecanol.
8. The preparation method of the pH stimulation responsive intelligent self-warning and self-repairing anticorrosive water-based coating according to any one of claims 1 to 6, characterized by comprising the following steps: the photoinitiator is 2-hydroxy-2-methyl-1-phenyl acetone, 1-hydroxy-cyclohexyl benzophenone, 2-hydroxy-2-methyl-1-p-hydroxyethyl ether phenyl acetone, 4-p-toluene mercapto benzophenone, 2,4, 6-trimethyl benzoyl-diphenyl phosphorus oxide and 2-isopropyl thioxanthone.
9. The preparation method of the pH stimulation responsive intelligent self-warning and self-repairing anticorrosive water-based coating according to any one of claims 1 to 6, characterized by comprising the following steps: the corrosion inhibitor is water-soluble inorganic corrosion inhibitor, water-soluble organic corrosion inhibitor or water-soluble polymer corrosion inhibitor.
10. The preparation method of the pH stimulation responsive intelligent self-warning and self-repairing anticorrosive water-based coating according to any one of claims 1 to 6, characterized by comprising the following steps: the waterborne polyurethane is a waterborne polyurethane emulsion special for a coating.
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| CN113429966B (en) * | 2021-06-16 | 2022-04-26 | 东北大学 | Early metal corrosion probe and preparation method thereof |
| CN114196309B (en) * | 2021-12-20 | 2022-07-12 | 广东美涂士建材股份有限公司 | Weather-resistant self-repairing coating and preparation method thereof |
| CN115418154B (en) * | 2022-08-26 | 2023-09-01 | 江南大学 | Self-early-warning self-repairing functional coating based on porous microspheres and coating prepared from same |
| CN116376402A (en) * | 2023-04-21 | 2023-07-04 | 华中科技大学 | Application of pH response fluorescence MOFs (metal-organic frameworks) composite material in intelligent anti-corrosion coating material |
| CN117777820A (en) * | 2024-02-28 | 2024-03-29 | 太原理工大学 | Reversible self-early warning and self-repairing coating and preparation method thereof |
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Application publication date: 20201030 Assignee: Deqian Technology (Jiangsu) Co.,Ltd. Assignor: HUAIYIN INSTITUTE OF TECHNOLOGY Contract record no.: X2021980015041 Denomination of invention: Preparation method of pH stimulus responsive intelligent self-warning self repairing anti-corrosion waterborne coating Granted publication date: 20210817 License type: Common License Record date: 20211222 |