CN113025107B - Preparation method and application of cuprous iodide-based hybrid fluorescent coating - Google Patents
Preparation method and application of cuprous iodide-based hybrid fluorescent coating Download PDFInfo
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- CN113025107B CN113025107B CN202110503221.0A CN202110503221A CN113025107B CN 113025107 B CN113025107 B CN 113025107B CN 202110503221 A CN202110503221 A CN 202110503221A CN 113025107 B CN113025107 B CN 113025107B
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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
- C09D5/22—Luminous 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
- C09D183/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Coating compositions based on derivatives of such polymers
- C09D183/04—Polysiloxanes
- C09D183/08—Polysiloxanes containing silicon bound to organic groups containing atoms other than carbon, hydrogen, and oxygen
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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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Abstract
The invention belongs to the technical field of fluorescent paint, and particularly relates to a preparation method and application of a cuprous iodide based hybrid fluorescent paint. The prepared hybrid fluorescent paint has the advantages of simple preparation method and film forming process, low cost, stable fluorescence performance, large-scale production and the like, can realize the corrosion protection function, can be applied to decorative coatings in modes of spin coating or blade coating and the like, and can also be applied to the fields of anti-counterfeiting and the like through printing technology.
Description
Technical Field
The invention belongs to the technical field of fluorescent paint, and particularly relates to a preparation method and application of a cuprous iodide-based hybrid fluorescent paint.
Background
The organic-inorganic hybrid coating material is mainly prepared by a sol-gel method, alkoxy compounds of silicon or other elements are hydrolyzed to generate fine inorganic particles with hydroxyl groups, and the particles of the fine inorganic particles are suspended in a colloidal state in a solution between 1 nm and 100nm, so that the organic-inorganic hybrid coating material is called as sol. The hydroxyl of the sol can react with the organic functional group mixed with the sol in the same solution under proper conditions to form chemical polymerization crosslinking and form the organic-inorganic hybrid nano coating material. In such hybrid coating materials, the inorganic components can achieve good hardness, wear resistance, weatherability, and the like; and the organic component can improve the flexibility, compactness, processability and the like of the material. The hybrid coating material has the advantages of adjustable structural performance, simple and convenient synthesis, environmental friendliness and the like, so that the hybrid coating material has a great development space.
At present, the intelligent coating which is very concerned at home and abroad needs a coating material to respond to the change of the environment and has the functions of corrosion protection and self-warning and self-repairing. The fluorescent coating is an important one of intelligent coatings, can be used as a decorative coating, can also be used as an intelligent coating to be applied to corrosion monitoring and early warning, and has a wide application field. At present, the organic-inorganic hybrid fluorescent coating material is mainly prepared by adding fluorescent substances, such as fluorescent powder, into the hybrid coating to realize the fluorescent performance, and no chemical bond is bonded between the fluorescent substances and the fluorescent powder. However, the physical mixing has various problems of uneven luminescent particles, easy sedimentation and the like, so that the luminescent particles are uneven and unstable in luminescence, the optical properties of the luminescent particles mainly come from the fluorescent powder, and the performance of the luminescent particles is not easy to regulate and control.
The cuprous iodide organic-inorganic hybrid material is a hybrid semiconductor material with excellent luminescence property. The inorganic components of the hybrid material have various structures, and can be clusters of cuprous iodide and chains or layers of cuprous iodide. These inorganic moieties are bound to organic ligands by chemical bonds (covalent and ionic) to form hybrid materials from zero to three dimensions. The material has various structures, is simple and convenient to synthesize, can be produced in a large scale, does not contain rare earth metal elements, is green and environment-friendly, and can be used as a substitute of commercial fluorescent materials without containing rare earth metal elements. However, no report is available at present for developing multifunctional fluorescent coating materials with stable luminescence properties.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention provides a preparation method of a cuprous iodide-based hybrid fluorescent coating, which combines a cuprous iodide hybrid fluorescent material with an organic-inorganic hybrid coating to synthesize a cuprous iodide cluster-based organic-inorganic hybrid functional coating with stable luminescence property, and can be applied to the fields of decoration, corrosion prevention and the like.
In order to achieve the purpose, the invention adopts the technical scheme that:
the invention provides a preparation method of a hybrid fluorescent paint based on cuprous iodide, which comprises the following steps:
s1, cuprous iodide silane precursor Cu4I4-synthesis of dpes: adding 2- (diphenylphosphino) ethyl triethoxysilane into CuI organic solvent suspension, stirring, filtering, and volatilizing the solvent to obtain the final product;
s2, preparing the hybrid fluorescent paint by a sol-gel method:mixing Cu4I4And (3) mixing the-dpes precursor with phenyltriethoxysilane, adding an organic solvent and hydrochloric acid, stirring, and evaporating the solvent to obtain the cuprous iodide-based hybrid fluorescent coating.
The cuprous iodide hybrid molecular cluster has excellent luminescence property, and the luminescence property mainly comes from the structure of the specific inorganic cluster. Therefore, small molecules with a specific cuprous iodide cluster structure are used as precursors at the molecular level and are bonded in a cross-linked framework of the organic-inorganic hybrid coating through chemical bonds to form a novel cuprous iodide cluster-based organic-inorganic hybrid fluorescent coating material, the optical performance of the cuprous iodide original molecular clusters can be maintained by the hybrid structure, and the inorganic component comprises both silicon oxide clusters and cuprous iodide clusters with specific structures. The existence of the inorganic component can keep the excellent protective performance of the original hybrid resin, and the cuprous iodide can endow the resin with excellent optical performance.
The specific method comprises the following steps: firstly, cuprous iodide and 2- (diphenylphosphino) ethyltriethoxysilane are utilized to successfully prepare a cuprous iodide silane precursor, and then a clear and transparent hybrid coating, namely the cuprous iodide-based hybrid fluorescent coating, is obtained by using the hydrolysis-condensation reaction of the cuprous iodide and phenyltriethoxysilane. Tests show that the prepared hybrid coating is colorless and transparent under natural light, emits yellow light under ultraviolet excitation, can be uniformly coated on the surface of a quartz plate by a spin coating method, and the luminous intensity of the coating is not weakened after the coating is kept stand in simulated seawater (wt 35% NaCl) for 40 days; in addition, the coating can also realize the corrosion protection effect by coating the coating on the surface of the carbon steel Q235.
Preferably, the mass ratio of CuI to 2- (diphenylphosphino) ethyltriethoxysilane is 1: 2.
preferably, the organic solvent in step S1 includes, but is not limited to, dichloromethane, and the concentration of CuI in the organic solvent suspension is 1g/20 mL.
Preferably, Cu4I4The molar ratio of the-dpes precursor to the phenyltriethoxysilane is 2X 10-3:1。
Preferably, the organic solvent in step S2 includes, but is not limited to, N-dimethylformamide, and the volume-to-mass ratio of the organic solvent to the phenyltriethoxysilane is 1:1 in mL: g.
Preferably, the pH of the hydrochloric acid in the step S2 is 2.5, and the volume-to-mass ratio of the hydrochloric acid to the phenyltriethoxysilane is 1 (8-9) in mL/g.
Preferably, the hybrid fluorescent paint based on cuprous iodide is mixed with tetrahydrofuran in a ratio of 1:1 and then spin-coated on the substrate when in use.
Preferably, both step S1 and step S2 are performed at room temperature.
Preferably, the stirring time in step S1 is 1-3h, and the stirring in step S2 is 4-6 h. Further, the stirring time in step S1 was 2 hours, and the stirring in step S2 was 5 hours.
The invention also provides the cuprous iodide-based hybrid fluorescent coating prepared by the preparation method.
The invention also provides application of the cuprous iodide-based hybrid fluorescent paint in the field of decoration or corrosion prevention.
It should be noted that the application field of the present invention is not limited to decoration and preservation, and can also be applied to other applicable fields such as anti-counterfeiting, indication, etc.
Compared with the prior art, the invention has the beneficial effects that:
the invention provides a preparation method of a cuprous iodide-based hybrid fluorescent coating, wherein cuprous iodide luminescent clusters are bonded into a hybrid coating material through chemical bonds, and the organic-inorganic hybrid functional coating with a stable luminescent property and a cuprous iodide cluster group base is synthesized. The prepared hybrid fluorescent paint has the advantages of simple preparation method and film forming process, low cost, stable fluorescence performance, large-scale production and the like, can realize the corrosion protection function, can be applied to decorative coatings in modes of spin coating or blade coating and the like, and can also be applied to the fields of anti-counterfeiting and the like through printing technology.
Drawings
FIG. 1 is a flow chart of the preparation of a hybrid fluorescent paint based on cuprous iodide;
FIG. 2 is a photograph of a quartz plate coated with a hybrid coating under natural light (a) and 254nm ultraviolet light excitation (b);
FIG. 3 is the appearance of the cross section of a glass sheet coated with a hybrid fluorescent coating observed under a scanning electron microscope;
FIG. 4 is a Nyquist plot (a) and a Bode plot (b) for a Q235 electrode and a Nyquist plot (c) and a Bode plot (d) for a Q235 electrode coated with a hybrid fluorescent coating;
in fig. 4, Z': real part of impedance, | Z "|: an imaginary impedance component; frequency: frequency, Phase angle: phase angle, | Z |: the resistance film value.
Detailed Description
The following further describes the embodiments of the present invention. It should be noted that the description of the embodiments is provided to help understanding of the present invention, but the present invention is not limited thereto. In addition, the technical features involved in the embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other.
The experimental procedures in the following examples were carried out by conventional methods unless otherwise specified, and the test materials used in the following examples were commercially available by conventional methods unless otherwise specified.
Example 1 preparation method of hybrid fluorescent paint based on cuprous iodide
(1) Cuprous iodide silane precursor Cu4I4-synthesis of dpes: at room temperature, 2- (diphenylphosphino) ethyltriethoxysilane, namely phosphine ligand L (1g, 2.66mmol), is added into a suspension of CuI (0.5g, 2.62mmol) in 10mL dichloromethane, the mixed solution is magnetically stirred at the room temperature at the rotating speed of 400r/min for 2 hours, then the mixture is filtered, and after the solvent is volatilized, a colorless oily substance with high viscosity, namely a cuprous iodide silane precursor, is obtained. The yield was 77% (1.16g, 0.5 mmol). The precursor emits orange light under ultraviolet excitation.
(2) Preparing a hybrid fluorescent coating by a sol-gel method: 1.16g of Cu at room temperature4I4The (dpes) precursor was mixed with 60g of phenyltriethoxysilane (molar ratio 2X 10)-31), adding 60mL of solvent N, N-Dimethylformamide (DMF) and 7mL of HCl (hydrochloric acid) with pH of 2.5, magnetically stirring for 5 hours at the rotating speed of 400r/min, and obtaining colorless and transparent viscous liquid after the solvent is evaporated, namely the cuprous iodide-based hybrid fluorescent paint.
The dope was mixed with tetrahydrofuran at a volume ratio of 1:1 and spin-coated (3000r/min, 60s) in an area of 4cm2The coating was found to be uniformly applied to the surface of a quartz glass plate by a spin coating method (FIG. 2a), and the obtained coating film was colorless and transparent in natural light and had a thickness of about 3 μm (FIG. 3); the coating emits yellow light under UV (254nm) excitation (FIG. 2b), and the luminescence intensity of the coating remains undiminished after standing in simulated seawater (wt 35% NaCl) for 40 days.
Example 2 preparation method of hybrid fluorescent paint based on cuprous iodide
(1) Cuprous iodide silane precursor Cu4I4-synthesis of dpes: at room temperature, 2- (diphenylphosphino) ethyltriethoxysilane-phosphine ligand L (0.2g, 0.53mmol) is added to a suspension of CuI (0.1g, 0.53mmol) in 10mL of dichloromethane, the mixed solution is stirred at room temperature for 2h, then the mixture is filtered, and after the solvent is volatilized, a colorless oily substance with high viscosity, namely cuprous iodide silane precursor, is obtained. The yield was 83% (0.25g, 0.11 mmol). The precursor emits orange light under ultraviolet excitation.
(2) Preparing a hybrid fluorescent coating by a sol-gel method: at room temperature, 0.25g of Cu4I4The (dpes) precursor was mixed with 13g of phenyltriethoxysilane (molar ratio 2X 10)-31), adding 13mL of N, N-Dimethylformamide (DMF) serving as a solvent and 1.5mL of HCl with pH of 2.5, stirring for 5 hours, and evaporating the solvent to obtain colorless and transparent viscous liquid, namely the cuprous iodide-based hybrid fluorescent paint.
The coating and tetrahydrofuran are mixed according to the volume ratio of 1:1 and then are coated on a quartz glass substrate in a spin mode, a colorless coating of a film is obtained, and the film forming of the coating is more uniform and thinner.
Example 3 preparation method of hybrid fluorescent paint based on cuprous iodide
(1) Cuprous iodide silane precursor Cu4I4-synthesis of dpes: at room temperature, 2- (diphenylphosphino) ethyltriethoxysilane-phosphine ligand L (0.1g, 0.26mmol) is added to a suspension of CuI (0.05g, 0.26mmol) in 10mL of dichloromethane, the mixed solution is stirred at room temperature for 2h, then the mixture is filtered, and after the solvent is volatilized, a colorless oily substance with high viscosity, namely cuprous iodide silane precursor, is obtained. The yield was 81% (0.122g, 0.05 mmol). The precursor emits orange light under ultraviolet excitation.
(2) Preparing a hybrid fluorescent coating by a sol-gel method: at room temperature, 0.122g of Cu4I4The-dpes precursor was mixed with 6.3g of phenyltriethoxysilane (molar ratio 2X 10)-31), adding 6.3mL of solvent N, N-Dimethylformamide (DMF) and 0.7mL of HCl with pH of 2.5, stirring for 5 hours, and evaporating the solvent to obtain colorless and transparent viscous liquid, namely the cuprous iodide-based hybrid fluorescent paint.
The coating and tetrahydrofuran are mixed according to the volume ratio of 1:1 and then are coated on a quartz glass substrate in a spin mode, a colorless coating of a film is obtained, and the film forming of the coating is more uniform and thinner.
Experimental example 1 Corrosion resistance test
The prepared hybrid coating (taking example 1 as an example) is coated on the surface of low-carbon steel Q235 and shows excellent corrosion protection performance. The specific test methods and results are as follows:
the corrosion resistance of the hybrid coating is characterized by Electrochemical Impedance Spectroscopy (EIS), EIS test is carried out on an x electrochemical workstation by adopting a standard three-electrode system, an excitation signal is a sine wave of 10mV, and a test frequency range is 10mV5-10-2Hz, using Q235 carbon steel sheets coated with or not coated with a hybrid coating as a working electrode, a platinum sheet electrode as a counter electrode and a saturated calomel electrode as a reference electrode.
As shown in fig. 4, the impedance modulus value of the low frequency region (Zf ═ 0.01) in the Bode diagram was used to evaluate the corrosion resistance of the coating, and compared with the graphs (b) and (c), the impedance modulus value of the Q235 carbon steel coated with the coating was improved by one order of magnitude, and the corrosion resistance was significantly improved. The radius of the capacitive arcs in the Nyquist plot was also used to characterize the corrosion resistance of the coating, and the radius of the capacitive arcs in plot (c) was significantly larger than the radius of the capacitive arcs in plot (a), indicating that the coating had good corrosion resistance. Graph (d) also illustrates that the coating can block the corrosive medium from contacting the metal substrate for protection.
The embodiments of the present invention have been described in detail, but the present invention is not limited to the described embodiments. It will be apparent to those skilled in the art that various changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, and the scope of protection is still within the scope of the invention.
Claims (10)
1. A preparation method of a hybrid fluorescent paint based on cuprous iodide is characterized by comprising the following steps:
s1, cuprous iodide silane precursor Cu4I4-synthesis of dpes: adding 2- (diphenylphosphino) ethyl triethoxysilane into CuI organic solvent suspension, stirring, filtering, and volatilizing the solvent to obtain the final product;
s2, preparing the hybrid fluorescent paint by a sol-gel method: mixing Cu4I4And (3) mixing the-dpes precursor with phenyltriethoxysilane, adding an organic solvent and hydrochloric acid, stirring, and evaporating the solvent to obtain the cuprous iodide-based hybrid fluorescent coating.
2. The preparation method of a hybrid fluorescent paint based on cuprous iodide, according to claim 1, wherein the mass ratio of CuI to 2- (diphenylphosphino) ethyltriethoxysilane is 1: 2.
3. the preparation method of a hybrid fluorescent paint based on cuprous iodide as claimed in claim 1, wherein the organic solvent in step S1 comprises dichloromethane, and the concentration of CuI in the organic solvent suspension is 1g/20 mL.
4. The method of claim 1The preparation method of the hybrid fluorescent paint based on cuprous iodide is characterized in that Cu4I4The molar ratio of the-dpes precursor to the phenyltriethoxysilane is 2X 10-3:1。
5. The preparation method of a hybrid fluorescent paint based on cuprous iodide as claimed in claim 1, wherein the organic solvent in step S2 comprises N, N-dimethylformamide, and the volume to mass ratio of the organic solvent to phenyltriethoxysilane is 1:1, and the unit is mL: g.
6. The preparation method of a hybrid fluorescent paint based on cuprous iodide as claimed in claim 1, wherein pH of hydrochloric acid in step S2 is 2.5, volume to mass ratio of hydrochloric acid to phenyltriethoxysilane is 1 (8-9), unit is mL: g.
7. The preparation method of the hybrid fluorescent paint based on cuprous iodide as claimed in claim 1, wherein in use, the hybrid fluorescent paint based on cuprous iodide is mixed with tetrahydrofuran in a volume ratio of 1:1 and then spin-coated on the substrate.
8. The preparation method of a hybrid fluorescent paint based on cuprous iodide as claimed in claim 1, wherein step S1 and step S2 are both performed at room temperature.
9. The cuprous iodide-based hybrid fluorescent paint prepared by the preparation method of the cuprous iodide-based hybrid fluorescent paint according to any one of claims 1 to 8.
10. Use of a hybrid fluorescent paint based on cuprous iodide as claimed in claim 9 in the field of decoration or corrosion prevention.
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