CN113772957B - Preparation of modified carbonyl iron powder for magnetic control super-hydrophobic surface construction and application of modified carbonyl iron powder in blue light curing super-hydrophobic film - Google Patents
Preparation of modified carbonyl iron powder for magnetic control super-hydrophobic surface construction and application of modified carbonyl iron powder in blue light curing super-hydrophobic film Download PDFInfo
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- CN113772957B CN113772957B CN202110940132.2A CN202110940132A CN113772957B CN 113772957 B CN113772957 B CN 113772957B CN 202110940132 A CN202110940132 A CN 202110940132A CN 113772957 B CN113772957 B CN 113772957B
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- C03—GLASS; MINERAL OR SLAG WOOL
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- C03C17/006—Surface treatment of glass, not in the form of fibres or filaments, by coating with materials of composite character
- C03C17/008—Surface treatment of glass, not in the form of fibres or filaments, by coating with materials of composite character comprising a mixture of materials covered by two or more of the groups C03C17/02, C03C17/06, C03C17/22 and C03C17/28
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Abstract
The invention discloses a preparation method of modified carbonyl iron powder for magnetic control super-hydrophobic surface construction and application thereof in a blue light curing super-hydrophobic film; the preparation process comprises the steps of preparing an ethanol-water mixed solution and adjusting the pH value; adding a modifier into an ethanol-water mixed solution, carrying out prehydrolysis for 30 minutes, heating to a certain temperature, weighing 5g of carbonyl iron powder, adding the carbonyl iron powder into the mixed solution, placing the mixture in a constant-temperature water bath kettle, stirring by using a mechanical stirrer, reacting for a certain time, carrying out magnetic separation, washing by using ethanol, and drying to obtain the modified carbonyl iron powder. The application process comprises the following steps: preparing photocuring coating slurry; and (2) preparing a hydrophobic film. The surface hydrophobicity of the carbonyl iron powder is improved by modifying the surface of the carbonyl iron powder; the modified carbonyl iron powder is used for preparing the magnetic control super-hydrophobic film, and the carbonyl iron powder is controllably arranged on the surface of the film to achieve the super-hydrophobic effect through the magnetic field effect and the blue light curing technology.
Description
Technical Field
The invention belongs to the field of super-hydrophobic films, and particularly relates to preparation of modified carbonyl iron powder for magnetic control super-hydrophobic surface construction and application of the modified carbonyl iron powder in a blue light curing super-hydrophobic film.
Background
A superhydrophobic surface generally refers to a surface having a contact angle with water of more than 150 ° and a rolling angle of less than 10 °. According to the 1997 German scientists Bathlott and Neinhuis, the main reason that the lotus leaf surface is superhydrophobic is mastoid and waxy substances with a surface microstructure, and domestic Jiang Lei academis, on the basis of which, a micro-nano composite structure and low surface free energy are further proposed as the root cause of superhydrophobicity, and the micro-nano structure enables the lotus leaf surface to be rough enough to trap a large amount of air and reduce the contact area of water drops and the surface. With the continuous deepening of the exploration and practice of wettability, people propose widely applicable WENZEL and CASSE-BAXTER wetting models through experimental processing and data analysis, and the functional applications of the super-hydrophobic surface are more and more, such as fluid drag reduction, self-cleaning coatings, oil-water separation, anti-icing, microfluid and the like.
At present, the preparation methods of the bionic super-hydrophobic surface proposed at home and abroad comprise a template method, an etching method, a sol-gel method and the like, but the methods need expensive raw materials, are complicated to operate and have high requirements on equipment, so that the application of the super-hydrophobic surface is limited. Recently, magnetic particles are dispersed into carrier liquid formed by low-surface-energy substances as a dispersion phase, the magnetic particles generate a single-magnetic-pole magnetic chain effect under the action of external magnetic field force, a special micro-nano composite structure is formed on the surface, and a super-hydrophobic surface with a lasting surface appearance is obtained.
However, when the surface appearance of the film is cured, the curing time is long when a traditional thermosetting mode is adopted, and compared with the traditional thermosetting mode, the photocuring technology has the specific advantages of economy, high efficiency, energy conservation, environmental protection, no solvent volatilization in the photocuring process and the like, and is rapidly developed in the industry. Compared with ultraviolet light and common visible light, the photoinitiation technology using blue light as a light source has the remarkable advantages of safety and high energy utilization rate. Therefore, in the experiment, blue light is adopted to initiate a curing reaction to obtain the film with the super-hydrophobic effect, and the method has important significance for safe and rapid production.
Disclosure of Invention
The invention aims to provide a preparation method of modified carbonyl iron powder for magnetic control super-hydrophobic surface construction and application of the modified carbonyl iron powder in a blue light curing super-hydrophobic film, and develops a controllable modification method of the carbonyl iron powder, and a rough surface is formed by means of magnetic chain reaction of the modified carbonyl iron powder under a light curing condition, so that a coating film with a super-hydrophobic effect is prepared.
In order to solve the technical problems, the following technical scheme is adopted:
a preparation method of modified carbonyl iron powder for magnetic control super-hydrophobic surface construction is characterized by comprising the following steps:
preparing modified carbonyl iron powder: preparing an ethanol-water mixed solution, and adjusting the pH value; adding a modifier into an ethanol-water mixed solution, pre-hydrolyzing for 30 minutes, heating to a certain temperature, weighing 5g of carbonyl iron powder, adding the carbonyl iron powder into the mixed solution, placing the mixture into a constant-temperature water bath kettle, stirring the mixture by using a mechanical stirrer, reacting for a certain time, performing magnetic separation, washing by using ethanol, and drying to obtain the modified carbonyl iron powder.
Preferably, the modifier is one or a mixture of two of gamma-aminopropyltrimethoxysilane and 1H.1H.2H.2H-perfluorodecyl trimethoxysilane; the mass ratio of the two is 4:0-0:4.
Preferably, after preparing an ethanol-water mixed solution, adjusting the pH value by using 0.1mol/L hydrochloric acid and sodium hydroxide, wherein V ethanol is V water = 10.
Preferably, the total mass fraction of the gamma-aminopropyl trimethoxy silane and the 1H.1H.2H.2H-perfluorodecyl trimethoxy silane in the ethanol-water mixed solution is 5 to 30 percent
Preferably, the reaction temperature is 35-95 ℃, and the reaction time is 0.5-3 h.
The application method of the modified carbonyl iron powder in the blue light curing super-hydrophobic film is characterized by comprising the following steps:
(1) Preparation of photocuring coating slurry: adding camphorquinone, 4-ethyl dimethyl benzoate and diphenyl iodohexafluorophosphate in certain mass fraction into hydroxyethyl acrylate monomer as a photoinitiation system, adding SM6202 resin after complete dissolution to adjust the viscosity of the system, finally adding modified carbonyl iron powder, and dispersing uniformly in an ultrasonic instrument to prepare coating slurry.
(2) Preparing a hydrophobic film: and (3) taking a glass sheet, coating the coating slurry in the step (2) on the glass sheet with different thicknesses by using a film scraping machine, irradiating blue light for a certain time under a certain magnetic field intensity, and curing to form a film.
Preferably, in the step (1), the mass fraction of the diphenyl iodonium hexafluorophosphate is 0.5 percent, the mass fraction of the camphorquinone is 0.5 to 3 percent, and the mass fraction of the 4-ethyl dimethyl benzoate is 0.5 to 3 percent; wherein the mass ratio of camphorquinone to ethyl 4-dimethylbenzoate is 1:1.
Preferably, the mass ratio of the hydroxyethyl acrylate monomer to the SM6202 resin in the step (1) is 1:9-9:1.
Preferably, in the step (1), the content of the carbonyl iron powder in the system is 20-60%.
Preferably, the thickness of the photocuring film in the step (2) is 50-250 μm, and the magnetic field intensity is 0-85 mT.
Due to the adoption of the technical scheme, the method has the following beneficial effects:
the invention discloses a preparation method of modified carbonyl iron powder for magnetic control super-hydrophobic surface construction and application of the modified carbonyl iron powder in a blue light curing super-hydrophobic film. The surface hydrophobicity of the carbonyl iron powder is improved by modifying the surface of the carbonyl iron powder; the modified carbonyl iron powder is used for preparing a magnetic control super-hydrophobic film, the carbonyl iron powder is controllably arranged and achieves a super-hydrophobic effect with the surface of the film through the magnetic field effect and the blue light curing technology, and the fixation fastness of the carbonyl iron powder in the film is improved by utilizing the covalent reaction of double bonds on the surface of the carbonyl iron powder and the film.
Drawings
The invention is further described with reference to the accompanying specific drawings in which:
FIG. 1 shows the surface contact angle of a magnetic control super-hydrophobic film based on blue light curing
Detailed Description
The invention is further illustrated by the following specific examples:
example 1
(1) An ethanol-water mixed solution (vsethanol: vsquel =10 = 1) was prepared, and the pH was adjusted to 6 using 0.1mol/L hydrochloric acid and sodium hydroxide. Adding 0.25g of gamma-aminopropyltrimethoxysilane and 0.75g of 1H.1H.2H.2H-perfluorodecyl trimethoxysilane into the solution, pre-hydrolyzing for 30 minutes, heating to 75 ℃, weighing 5g of carbonyl iron powder, adding into the mixed solution, placing into a constant temperature water bath kettle, stirring by a mechanical stirrer, reacting for 1.5 hours, carrying out magnetic separation, washing by ethanol, and drying. Hydrophobic magnetic particles are obtained.
(2) Preparation of photocuring coating slurry: adding 2 percent by weight of camphorquinone, 2%4-ethyl dimethylbenzoate and 0.5 percent of diphenyl iodohexafluorophosphate into 1.5g of hydroxyethyl acrylate monomer to serve as a photoinitiation system, adding 3.5g of SM6202 resin to adjust the viscosity of the system after the materials are completely dissolved, finally adding 5g of modified carbonyl iron powder in the step (1), and uniformly dispersing in an ultrasonic instrument to prepare coating slurry.
(3) Preparing a hydrophobic film: coating the coating slurry in the step (2) on a glass sheet with the thickness of 150 microns by using a film scraper, irradiating for 15min by blue light under the magnetic field strength of 75mT, and curing to form a film.
Example 2
(1) An ethanol-water mixed solution (vsethanol: vsquel =10 = 1) was prepared, and the pH was adjusted to 7 using 0.1mol/L hydrochloric acid and sodium hydroxide. Adding 0.5g of gamma-aminopropyltrimethoxysilane and 0.5g of 1H.1H.2H.2H-perfluorodecyl trimethoxysilane into the solution, pre-hydrolyzing for 30 minutes, heating to 70 ℃, weighing 5g of carbonyl iron powder, adding into the mixed solution, placing into a constant-temperature water bath kettle, stirring by using a mechanical stirrer, reacting for 2 hours, carrying out magnetic separation, washing by using ethanol, and drying. Hydrophobic magnetic particles are obtained.
(2) Preparing the photocuring coating slurry: to 2g of hydroxyethyl acrylate monomer were added 1.5% by weight of camphorquinone, 1.5% by weight of ethyl 4-dimethylbenzoate, 0.5% by weight of diphenyliodohexafluorophosphate as a photoinitiating system, after complete dissolution, 3g of SM6202 resin was added to adjust the viscosity of the system, and finally 4.5g of modified carbonyl iron powder of (1) was added and uniformly dispersed in an ultrasonic instrument to prepare a coating slurry.
(3) Preparing a hydrophobic film: coating the coating slurry in the step (2) on a glass sheet with the thickness of 180 microns by using a film scraper, irradiating for 15min by blue light under the magnetic field strength of 80mT, and curing to form a film.
Example 3
(1) An ethanol-water mixed solution (vsethanol: vsquel =10 = 1) was prepared, and the pH was adjusted to 7 using 0.1mol/L hydrochloric acid and sodium hydroxide. Adding 0.75g of gamma-aminopropyltrimethoxysilane and 0.25g of 1H.1H.2H.2H-perfluorodecyl trimethoxysilane into the solution, pre-hydrolyzing for 30 minutes, heating to 70 ℃, weighing 5g of carbonyl iron powder, adding into the mixed solution, placing into a constant-temperature water bath kettle, stirring by using a mechanical stirrer, reacting for 1.5 hours, carrying out magnetic separation, washing by using ethanol, and drying. Hydrophobic magnetic particles are obtained.
(2) Preparation of photocuring coating slurry: adding 1 percent by weight of camphorquinone, 1%4-ethyl dimethylbenzoate and 0.5 percent of diphenyl iodine hexafluorophosphate into 2.5g of hydroxyethyl acrylate monomer to serve as a photoinitiation system, adding 2.5g of SM6202 resin to adjust the viscosity of the system after the materials are completely dissolved, finally adding 4g of the modified carbonyl iron powder in the step (1), and uniformly dispersing in an ultrasonic instrument to prepare coating slurry.
(3) Preparing a hydrophobic film: coating the coating slurry in the step (2) on a glass sheet with the thickness of 100 micrometers by using a film scraper, irradiating the glass sheet with blue light for 12min under the magnetic field strength of 50mT, and curing to form a film.
The above are only specific embodiments of the present invention, but the technical features of the present invention are not limited thereto. Any simple changes, equivalent substitutions or modifications made on the basis of the present invention to solve the same technical problems and achieve the same technical effects are all covered in the protection scope of the present invention.
Claims (8)
1. The application method of the modified carbonyl iron powder in the blue light curing super-hydrophobic film is characterized by comprising the following steps:
(1) Preparing modified carbonyl iron powder: preparing an ethanol-water mixed solution, and adjusting the pH value; adding a modifier into an ethanol-water mixed solution, carrying out prehydrolysis for 30 minutes, heating to a certain temperature, weighing 5g carbonyl iron powder, adding into the mixed solution, placing in a constant-temperature water bath kettle, stirring by using a mechanical stirrer, reacting for a certain time, carrying out magnetic separation, washing by using ethanol, and drying to obtain modified carbonyl iron powder; the modifier is one or the mixture of two of gamma-aminopropyl trimethoxy silane and 1H.1H.2H.2H-perfluoro decyl trimethoxy silane; the mass ratio of the two is 4;
(2) Preparing the photocuring coating slurry: adding camphorquinone, 4-ethyl dimethyl benzoate and diphenyl iodohexafluorophosphate in certain mass fraction into hydroxyethyl acrylate monomer as a photoinitiation system, adding SM6202 resin to adjust the viscosity of the system after the materials are completely dissolved, and finally adding modified carbonyl iron powder to be uniformly dispersed in an ultrasonic instrument to prepare coating slurry;
(3) Preparing a hydrophobic film: and (3) taking a glass sheet, coating the coating slurry in the step (2) on the glass sheet with different thicknesses by using a film scraping machine, irradiating blue light for a certain time under a certain magnetic field intensity, and curing to form a film.
2. The application method of the modified carbonyl iron powder in the blue light curing super-hydrophobic film according to claim 1, characterized in that: after preparing an ethanol-water mixed solution, adjusting the pH value by using 0.1mol/L hydrochloric acid and sodium hydroxide, wherein V ethanol, V water = 10.
3. The application method of the modified carbonyl iron powder in the blue light curing super-hydrophobic film according to claim 1, characterized in that: the total mass fraction of the gamma-aminopropyl trimethoxy silane and the 1H.1H.2H.2H-perfluorodecyl trimethoxy silane in the ethanol-water mixed solution is 5-30%.
4. The application method of the modified carbonyl iron powder in the blue light curing super-hydrophobic film according to claim 1, characterized in that: the reaction temperature is 35-95 ℃, and the reaction time is 0.5-3 h.
5. The application method of the modified carbonyl iron powder in the blue-light curing super-hydrophobic film according to claim 1, characterized in that: in the step (1), the mass fraction of diphenyl iodonium hexafluorophosphate is 0.5 percent, the mass fraction of camphorquinone is 0.5-3 percent, and the mass fraction of ethyl 4-dimethylbenzoate is 0.5-3 percent; wherein the mass ratio of camphorquinone to ethyl 4-dimethylbenzoate is 1:1.
6. The application method of the modified carbonyl iron powder in the blue light curing super-hydrophobic film according to claim 1, characterized in that: the mass ratio of the hydroxyethyl acrylate monomer to the SM6202 resin in the step (1) is (1).
7. The application method of the modified carbonyl iron powder in the blue light curing super-hydrophobic film according to claim 1, characterized in that: in the step (1), the content of the carbonyl iron powder in the system is 20-60%.
8. The application method of the modified carbonyl iron powder in the blue light curing super-hydrophobic film according to claim 1, characterized in that: the thickness of the photocuring film in the step (2) is 50-250 mu m, and the magnetic field strength is 20mT-85mT.
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| CN1706765A (en) * | 2004-06-07 | 2005-12-14 | 通用电气公司 | Composition for opaque coating, lamp with coating, and method of manufacture |
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