CN113088255A - Super-hydrophobic Prussian blue nano-particles with photo-thermal performance and preparation method thereof - Google Patents
Super-hydrophobic Prussian blue nano-particles with photo-thermal performance and preparation method thereof Download PDFInfo
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Abstract
The invention discloses super-hydrophobic Prussian blue nano-particles with photo-thermal properties and a preparation method thereof, belonging to the technical field of functional materials. The method for preparing the super-hydrophobic Prussian blue nano-particles comprises the following steps: (1) dissolving potassium ferricyanide and polyvinylpyrrolidone in a hydrochloric acid solution to react; after the reaction is finished, centrifuging, washing and drying to obtain prussian blue nano-particles; (2) uniformly dispersing prussian blue nano particles in absolute ethyl alcohol, adding mercaptan, and reacting; after the reaction is finished, centrifuging, washing and drying to obtain super-hydrophobic Prussian blue nano-particles; wherein the concentration of mercaptan in the absolute ethyl alcohol is 1 mmol/L-L00 mmol/L. The super-hydrophobic Prussian blue nano-particles prepared by the method have good waterproof performance, the water contact angle is higher than 150 degrees, the water rolling angle is smaller than 10 degrees, the super-hydrophobic Prussian blue nano-particles also have excellent photo-thermal performance, and the temperature can be rapidly increased to 55 ℃ after the near-infrared light is irradiated for 180 seconds.
Description
Technical Field
The invention relates to super-hydrophobic Prussian blue nano-particles with photo-thermal properties and a preparation method thereof, belonging to the technical field of functional materials.
Background
Many animals and plants in nature have special wetting characteristics, for example, lotus leaves are not easy to wet by rainwater; animals such as the water strider and the like can quickly crawl on the water surface; the mosquito's eyes have waterproof and antifogging properties. Inspired by these natural biological phenomena, artificial superhydrophobic materials having a large contact angle (greater than 150 °) and a small sliding angle (less than 10 °) have been widely used in many fields including biofouling prevention, self-cleaning, drag reduction, oil-water separation, and ice coating prevention, etc.
It is well known that the combination of appropriate micro/nano-scale structures with low surface energy modifiers is the basic strategy to build superhydrophobic surfaces. Based on this strategy, technical methods for structuring rough surface structures have been widely developed, typically involving photolithography, chemical etching, hydrothermal reaction, sol-gel methods, and electrochemical deposition, followed by surface modification using low surface energy molecules (e.g., long chain alkyl silanes, hydrocarbons, or fluorinated hydrocarbons). For example, the Chinese patent application with the publication number of CN 102807775A discloses a water-proof and oil-proof magnetic SiO2/Fe3O4A method of making a composite particle comprising the steps of: (1) FeCl is added2·4H2O、Na2SO3Dissolving polyvinylpyrrolidone and NaOH in deionized water, and preparing Fe through high-temperature high-pressure reaction3O4Particles; (2) fe to be prepared3O4Uniformly dispersing the particles in ethanol, adding ammonia water, stirring for several hours, dropwise adding tetraethyl orthosilicate, reacting for several hours, and separating, washing and drying to obtain the water-proof and oil-proof magnetic particles; (3) the water-proof and oil-proof magnetic SiO2/Fe3O4Composite particle dissolutionDripping fluorosilane into alcohol/water mixed solution, stirring and separating to obtain magnetic SiO2/Fe3O4A composite particulate product; (4) water and oil repellent automotive coatings are prepared by adding particles and film forming resins (acrylic, polyester and amino resins). The Chinese patent publication CN 109796859A discloses a preparation method and application of a super-hydrophobic coating with a photo-thermal effect, wherein fluorinated polyurethane is prepared firstly, then Prussian blue is dispersed in the fluorinated polyurethane, and the super-hydrophobic coating is obtained by coating or spraying.
Disclosure of Invention
[ problem ] to
Most of the current methods require complicated equipment, time-consuming processes and expensive low surface energy modifiers, limiting the large-scale application of artificial superhydrophobic surfaces. And the prussian blue is generally compounded with a polyurethane coating to obtain the super-hydrophobic coating, and no document discloses how to prepare the super-hydrophobic prussian blue particles.
[ solution ]
In order to solve at least one of the problems, the invention provides the super-hydrophobic prussian blue nano-particles obtained by reacting potassium ferricyanide with polyvinylpyrrolidone and performing thiol post-modification. The nano-particles prepared by the method have excellent super-hydrophobic property, the contact angle with water is more than 150 degrees, the rolling angle is less than 10 degrees, and the nano-particles also show excellent photo-thermal conversion capability. In addition, the preparation method disclosed by the invention is simple in process, short in time consumption and easy to realize large-scale production.
The first object of the invention is to provide a method for preparing super-hydrophobic prussian blue nanoparticles with photo-thermal properties, which comprises the following steps:
(1) dissolving potassium ferricyanide and polyvinylpyrrolidone in a hydrochloric acid solution to react; after the reaction is finished, centrifuging, washing and drying to obtain prussian blue nano-particles;
(2) uniformly dispersing prussian blue nano particles in absolute ethyl alcohol, adding mercaptan, and reacting; after the reaction is finished, centrifuging, washing and drying to obtain super-hydrophobic Prussian blue nano-particles with photo-thermal properties; wherein the concentration of mercaptan in the absolute ethyl alcohol is 1 mmol/L-L00 mmol/L.
In one embodiment of the invention, the concentration of the mercaptan in the absolute ethanol in the step (2) is 50mmol/L to L00 mmol/L.
In one embodiment of the present invention, the mass ratio of potassium ferricyanide to polyvinylpyrrolidone in step (1) is 1: 12 to 20.
In one embodiment of the present invention, the concentration of the hydrochloric acid solution in the step (1) is 0.01mol/L to 0.1 mol/L.
In one embodiment of the invention, the ratio of potassium ferricyanide to hydrochloric acid solution in step (1) is 1 g: 50-200 mL.
In one embodiment of the present invention, the reaction conditions in step (1) are: the temperature is 60-90 ℃, the time is 12-24 h, and the reaction pH is 1-4; the reaction is carried out in an oil bath or water bath mode.
In one embodiment of the present invention, the centrifugation in step (1) is at 8000rpm to 12000rpm for 5 to 20 min.
In one embodiment of the present invention, the washing in step (1) is water washing.
In one embodiment of the present invention, the ratio of the prussian blue nanoparticles to the absolute ethyl alcohol in step (2) is 1 g: 50-200 mL.
In one embodiment of the present invention, the thiol in step (2) is selected from one of alkyl thiol or perfluoroalkyl thiol.
In one embodiment of the present invention, the alkyl mercaptan in step (2) has the formula CnH2n+1SH, wherein n represents an integer of 10 to 20.
In one embodiment of the present invention, the perfluoroalkyl thiol in step (2) has the formula CnF2(n-2)+1H4SH, wherein n represents an integer of 6 to 8.
In one embodiment of the invention, the reaction time in the step (2) is 6-12 h, and the temperature is 20-30 ℃ at room temperature.
In one embodiment of the present invention, the centrifugation in step (2) is at 3000rpm to 5000rpm for 5 to 20 min.
In one embodiment of the present invention, the washing in step (2) is alcohol washing, and the alcohol washing includes washing with one of 95% ethanol and absolute ethanol.
In one embodiment of the invention, the drying in the step (1) and the step (2) is carried out at a drying temperature of 70-80 ℃ for 6-12 h.
In one embodiment of the invention, the super-hydrophobic prussian blue nanoparticles obtained in the step (2) have a particle size of 100nm to 200nm and a cubic configuration.
The second purpose of the invention is to prepare the super-hydrophobic Prussian blue nano-particles with photo-thermal properties by the method.
The third purpose of the invention is the application of the super-hydrophobic Prussian blue nano-particles with photo-thermal properties in biofouling prevention, self-cleaning, drag reduction, oil-water separation and ice coating prevention.
The fourth purpose of the invention is to provide a super-hydrophobic product, wherein the super-hydrophobic product is obtained by loading the super-hydrophobic Prussian blue nano-particles with photo-thermal properties obtained by the invention on various substrates.
In one embodiment of the present invention, the substrate comprises one of fabric, wood, metal, glass, and ceramic.
[ advantageous effects ]
(1) The preparation method provided by the invention is simple in process and easy to operate, and can be expanded to large-scale preparation.
(2) The super-hydrophobic Prussian blue nano-particles with photo-thermal properties prepared by the invention have better waterproof properties, the water contact angle is higher than 150 degrees, the water rolling angle is smaller than 10 degrees, and meanwhile, the super-hydrophobic Prussian blue nano-particles have excellent environmental stability, and the defect that the hydrophobicity of the super-hydrophobic particles is easy to damage can be greatly improved.
(3) The super-hydrophobic Prussian blue nano-particles with photo-thermal properties can rapidly increase the surface temperature under near-infrared laser irradiation, have obvious photo-thermal phenomenon, and can be used for ice coating prevention and photo-thermal deicing.
Drawings
Fig. 1 is a transmission electron micrograph of the superhydrophobic prussian blue nanoparticles.
Fig. 2 is a photograph of the static water contact angle of the superhydrophobic prussian blue nanoparticles in the superhydrophobic test.
Fig. 3 is an X-ray diffraction (XRD) pattern of the superhydrophobic prussian blue nanoparticles.
FIG. 4 shows super-hydrophobic Prussian blue nanoparticle N2Adsorption-desorption isotherm spectra.
FIG. 5 is a temperature rise curve of the super-hydrophobic Prussian blue nanoparticles under near-infrared illumination (808nm excitation light, 1W/cm)2) And thermal infrared imaging.
Fig. 6 is an environmental stability test chart of the superhydrophobic prussian blue nanoparticles.
Detailed Description
The following description of the preferred embodiments of the present invention is provided for the purpose of better illustrating the invention and is not intended to limit the invention thereto.
The test method comprises the following steps:
1. and (3) testing the super-hydrophobic property:
the prepared prussian blue nanoparticles were fixed on a glass slide by double-sided tape, and a water contact angle was obtained by measuring 5 μ L of water at five positions of each sample with a contact angle measuring instrument (Powereach JC2000D1) at room temperature, and calculating an average value.
2. Testing the photo-thermal performance:
the prepared Prussian blue nanoparticles were fixed on a glass slide by double-sided tape by using near-infrared laser (808nm excitation light, 1W/cm) at room temperature2) The photothermal properties were measured by irradiating five positions of each sample for 180 seconds and calculating the average heating capacity.
3. And (3) testing environmental stability:
(1) and (3) water impact resistance test: fixing the prepared super-hydrophobic Prussian blue nano particles on a glass slide through a double faced adhesive tape, placing the glass slide at the lower end of water flow, continuously impacting for 30 minutes, and recording the water contact angle of a tested sample through a contact angle measuring instrument;
(2) sand impact resistance test: fixing the prepared super-hydrophobic Prussian blue nano particles on a glass slide through a double faced adhesive tape, placing the glass slide at the lower end of 100-mesh sand, continuously impacting for 30 minutes, and recording the water contact angle of a tested sample through a contact angle measuring instrument;
(3) and (3) ultraviolet resistance test: fixing the prepared super-hydrophobic Prussian blue nano-particles on a glass slide through double faced adhesive tape, placing the glass slide at the lower end (500W) of an ultraviolet high-pressure pump lamp, continuously irradiating for 30 minutes, and recording the water contact angle of a tested sample through a contact angle measuring instrument;
(4) ultrasonic resistance test: fixing the prepared super-hydrophobic Prussian blue nano particles on a glass slide through double faced adhesive tape, placing the glass slide in an ultrasonic cleaner (500W), continuing to perform ultrasonic treatment for 30 minutes, and recording the water contact angle of a tested sample through a contact angle measuring instrument;
(5) and (3) high temperature resistance test: fixing the prepared super-hydrophobic Prussian blue nano-particles on a glass slide through a double faced adhesive tape, placing the glass slide in an oven at the temperature of 150 ℃, continuously heating for 12 hours, and recording the water contact angle of a tested sample through a contact angle measuring instrument;
(6) and (3) low temperature resistance test: fixing the prepared super-hydrophobic Prussian blue nano-particles on a glass slide through a double faced adhesive tape, continuously placing the glass slide in liquid nitrogen for 30 minutes, and recording the water contact angle of a tested sample through a contact angle measuring instrument.
Example 1
A method for preparing super-hydrophobic Prussian blue nanoparticles with photo-thermal properties comprises the following steps:
(1) dissolving 0.3g of potassium ferricyanide and 4.5g of polyvinylpyrrolidone in 50mL of 0.1M hydrochloric acid solution, adjusting the pH value to 1, and heating and reacting in an oil bath at 80 ℃ for 20 hours; after the reaction is finished, centrifuging the product solution obtained by the reaction for 15min at the rotating speed of 10000rpm, repeatedly washing the product solution with water to be neutral, and drying the product solution in an oven at the temperature of 80 ℃ overnight to obtain Prussian blue nano particles;
(2) uniformly dispersing 0.2g of Prussian blue nanoparticles in 20mL of absolute ethyl alcohol, adding octadecyl mercaptan (wherein the concentration of the octadecyl mercaptan in the absolute ethyl alcohol is 50mmol/L), and reacting for 12h at 25 ℃; and after the reaction is finished, centrifuging the product solution obtained by the reaction for 15min at the rotating speed of 3000rpm, repeatedly cleaning with absolute ethyl alcohol, and drying in an oven at 80 ℃ overnight to obtain the super-hydrophobic Prussian blue nano-particles with photo-thermal properties.
The obtained super-hydrophobic Prussian blue nano-particles with photo-thermal properties are subjected to performance tests, and the test results are as follows:
FIG. 1 is a morphological analysis of super-hydrophobic Prussian blue nanoparticles with photo-thermal properties by Hitachi JEM-2100 transmission electron microscopy, Japan. As can be seen from fig. 1: uniformly dispersed Prussian blue nano-particles with a cubic configuration are successfully prepared, and the particle size of the particles is 100-200 nm.
Fig. 2 is a photograph of static water contact angle at the time of superhydrophobic test, as can be seen from fig. 2: the super-hydrophobic Prussian blue nano-particles with photo-thermal properties have a static water contact angle of 155.3 degrees, almost exhibit a regular sphere in the visual observation of water drops, show good super-hydrophobic properties, and can be widely used for preparing super-hydrophobic coatings.
FIG. 3 is an X-ray diffraction (XRD) spectrum which was subjected to X-ray diffraction analysis at room temperature using a DX-27000X-ray diffractometer using CuK α rays (wavelength. lambda.: 0.15405nm, scanning mode: continuous scanning, scanning speed: 0.1 °/s, scanning angle: 5 to 90 °, tube voltage: 35kV, tube current: 35mA) as a diffraction light source. As can be seen from fig. 3: diffraction peaks of the superhydrophobic prussian blue nanoparticle having photothermal properties at 2-fold diffraction angles of 17.3 °, 24.7 °, 35.1 °, 39.4 °, 43.6 °, 50.6 °, 53.8 ° and 57.1 ° respectively correspond to (100), (110), (200), (210), (211), (220), (300) and (310) crystal planes. These peaks align well with the face centered cubic phase of prussian blue (PDF card JCPDS 01-0239), further confirming the high purity of the synthesized nanoparticles.
FIG. 4 is N2The adsorption-desorption isotherm spectrum is used for the specific surface area and pore size analysis at room temperature by using a TriStar II 3flex type full-automatic specific surface and porosity analyzer. As can be seen from fig. 4: superphobic having photothermal propertiesThe specific surface area and total pore volume of the aqueous prussian blue nanoparticles was calculated to be 233.49m2G and 0.27cm3In terms of/g, the nanoparticles have a high specific surface area.
FIG. 5 is a graph showing the temperature rise curve under near-infrared light (808nm excitation light, 1W/cm)2) And thermal infrared imaging. As can be seen from fig. 5: after the 808nm near-infrared light is irradiated for 180s, the surface temperature of the super-hydrophobic Prussian blue nano-particles with photo-thermal properties is rapidly increased to 55 ℃, which shows that the super-hydrophobic Prussian blue nano-particles have excellent photo-thermal properties, and under the irradiation of the near-infrared light, the nano-particles can rapidly convert the photo-thermal energy into heat energy, so that the excellent photo-thermal effect is shown, and the preparation of photo-thermal materials and coatings is facilitated.
Fig. 6 is an environmental stability test chart of the superhydrophobic prussian blue nanoparticles. As can be seen from fig. 6: the prepared super-hydrophobic Prussian blue nano-particles can always maintain super-hydrophobicity in the environments of water impact, sand impact, strong ultraviolet light irradiation, strong ultrasonic waves, high temperature and low temperature, the water contact angle after the test is still larger than 150 degrees, and the requirement of hydrophobicity is met.
Example 2
The pH values of 2, 4 and 6 in the step (1) of the example 1 are adjusted, and the pH values are kept consistent with those of the example 1, so that the super-hydrophobic Prussian blue nano-particles with photo-thermal properties are obtained.
The obtained super-hydrophobic Prussian blue nano-particles with photo-thermal properties are subjected to performance tests, and the test results are as follows:
table 1 test results of example 2
Note: the photo-thermal property is the temperature after 808nm near-infrared light is irradiated for 180 s; the environmental stability test is to record the water contact angle of the sample after the test.
Example 3
The amounts of polyvinylpyrrolidone used in example 1 were adjusted to 2.4, 3, 3.6 and 6g, and the rest was kept the same as in example 1, to obtain superhydrophobic prussian blue nanoparticles having photothermal properties.
The obtained super-hydrophobic Prussian blue nano-particles with photo-thermal properties are subjected to performance tests, and the test results are as follows:
table 2 test results of example 3
Note: the photo-thermal property is the temperature after 808nm near-infrared light is irradiated for 180 s; the environmental stability test is to record the water contact angle of the sample after the test.
Example 4
The concentration of the octadecyl mercaptan in the ethanol solution in example 1 was adjusted to 30 and 100, and the rest was the same as that in example 1, so that the super-hydrophobic prussian blue nanoparticles with photo-thermal properties were obtained.
The obtained super-hydrophobic Prussian blue nano-particles with photo-thermal properties are subjected to performance tests, and the test results are as follows:
table 3 test results of example 4
Note: the photo-thermal property is the temperature after 808nm near-infrared light is irradiated for 180 s; the environmental stability test is to record the water contact angle of the sample after the test.
Example 5
The octadecyl mercaptan in example 1 was adjusted to the mercaptan described in table 4 below, and the rest was identical to example 1, to obtain superhydrophobic prussian blue nanoparticles having photothermal properties.
The obtained super-hydrophobic Prussian blue nano-particles with photo-thermal properties are subjected to performance tests, and the test results are as follows:
table 4 test results of example 5
Note: the photo-thermal property is the temperature after 808nm near-infrared light is irradiated for 180 s; the environmental stability test is to record the water contact angle of the sample after the test.
Comparative example 1
Adjusting the preparation method of prussian blue particles in the step (1) of example 1, the method comprises the following steps:
dissolving 0.3g of potassium ferrocyanide and 2.5g of ferric trichloride in 50mL of aqueous solution, adding 2g of citric acid as a surface covering agent, and heating in an oil bath at 60 ℃ for 20 hours for reaction; after the reaction is finished, centrifuging the product solution obtained by the reaction for 15min at the rotating speed of 10000rpm, repeatedly washing the product solution with water to be neutral, and drying the product solution in an oven at the temperature of 80 ℃ overnight to obtain Prussian blue nano particles; the rest is in agreement with example 1, yielding hydrophobic prussian blue nanoparticles with photothermal properties.
Comparative example 2
The octadecyl mercaptan in example 1 was adjusted to be a KH-570 silane coupling agent, and others were consistent with those in example 1, to obtain hydrophobic Prussian blue nanoparticles having photothermal properties.
Comparative example 3
The hydrochloric acid solution in example 1 was adjusted to water, and the others were kept the same as in example 1, to obtain hydrophobic prussian blue nanoparticles having photothermal properties.
The obtained super-hydrophobic Prussian blue nano-particles with photo-thermal properties are subjected to performance tests, and the test results are as follows:
TABLE 5 test results of comparative examples 1, 2 and 3
| Comparative example | Contact angle (°) | Rolling angle (°) | Photothermal Property (. degree. C.) |
| 1 | 138.2 | 20 | 41 |
| 2 | 89..3 | Is free of | 46 |
| 3 | 79.2 | Is free of | 28 |
Note: the photothermal properties were the temperature after 808nm near infrared irradiation for 180 s.
Example 6 preparation of superhydrophobic fabrics
Soaking 5 x 5cm cotton fabric in 20ml of aqueous solution dissolved with 0.2g of polyvinyl alcohol for 5min, then soaking in 10ml of absolute ethanol containing 0.2g of the super-hydrophobic prussian blue nanoparticles described in example 1 for 30min, and placing in an oven for drying to obtain the super-hydrophobic cotton fabric.
Through tests, the water contact angle of the obtained hydrophobic cotton fabric is 152.6 degrees, and the hydrophobic cotton fabric has excellent photo-thermal performance after being rapidly heated to 48 ℃ after being irradiated by near infrared light for 180 seconds.
Although the present invention has been described with reference to the preferred embodiments, it should be understood that various changes and modifications can be made therein by those skilled in the art without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (10)
1. A method for preparing super-hydrophobic Prussian blue nano-particles with photo-thermal properties is characterized by comprising the following steps:
(1) dissolving potassium ferricyanide and polyvinylpyrrolidone in a hydrochloric acid solution to react; after the reaction is finished, centrifuging, washing and drying to obtain prussian blue nano-particles;
(2) uniformly dispersing prussian blue nano particles in absolute ethyl alcohol, adding mercaptan, and reacting; after the reaction is finished, centrifuging, washing and drying to obtain super-hydrophobic Prussian blue nano-particles with photo-thermal properties; wherein the concentration of mercaptan in the absolute ethyl alcohol is 1 mmol/L-L00 mmol/L.
2. The method according to claim 1, wherein the mass ratio of potassium ferricyanide to polyvinylpyrrolidone in step (1) is 1: 12 to 20.
3. The process according to claim 1 or 2, wherein the reaction conditions in step (1) are: the temperature is 60-90 ℃, the time is 12-24 h, and the reaction pH is 1-4.
4. The method according to any one of claims 1 to 3, wherein the mercaptan in the step (2) is selected from one of alkyl mercaptan and perfluoroalkyl mercaptan; the molecular formula of the alkyl mercaptan in the step (2) is CnH2n+1SH, wherein n represents an integer of 10 to 20; the molecular formula of the perfluoroalkyl group mercaptan in the step (2) is CnF2(n-2)+1H4SH, wherein n represents an integer of 6 to 8.
5. The method according to any one of claims 1 to 4, wherein the reaction time in the step (2) is 6 to 12 hours and the temperature is 20 to 30 ℃ at room temperature.
6. The method according to any one of claims 1 to 5, wherein the concentration of the hydrochloric acid solution in the step (1) is 0.01mol/L to 0.1 mol/L.
7. The method according to any one of claims 1 to 6, wherein the ratio of potassium ferricyanide to hydrochloric acid solution in step (1) is 1 g: 50-200 mL.
8. The super-hydrophobic Prussian blue nano-particles with photo-thermal properties prepared by the method of any one of claims 1 to 7.
9. Use of the superhydrophobic prussian blue nanoparticles with photothermal properties according to claim 8 for biofouling prevention, self-cleaning, drag reduction, oil-water separation, ice-over prevention.
10. A superhydrophobic article, wherein the superhydrophobic article is obtained by supporting the superhydrophobic Prussian blue nanoparticles having photothermal properties obtained according to claim 8 on various substrates.
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| CN116040654A (en) * | 2022-12-13 | 2023-05-02 | 深圳华钠新材有限责任公司 | Super-hydrophobic Prussian blue material and preparation method and application thereof |
| CN117509675A (en) * | 2023-11-08 | 2024-02-06 | 武汉中科先进材料科技有限公司 | Iron-based Prussian blue with low crystal water content, and preparation method and application thereof |
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