CN115161992A - Preparation method of super-hydrophobic fabric for anti-icing and photo-thermal deicing - Google Patents

Preparation method of super-hydrophobic fabric for anti-icing and photo-thermal deicing Download PDF

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CN115161992A
CN115161992A CN202210664127.8A CN202210664127A CN115161992A CN 115161992 A CN115161992 A CN 115161992A CN 202210664127 A CN202210664127 A CN 202210664127A CN 115161992 A CN115161992 A CN 115161992A
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fabric
nickel
icing
deicing
solution
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张松楠
李国龙
张凤彩
任志涛
钱晓明
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Tianjin Polytechnic University
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Tianjin Polytechnic University
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    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M11/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/32Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
    • D06M11/36Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
    • D06M11/38Oxides or hydroxides of elements of Groups 1 or 11 of the Periodic System
    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C18/00Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/16Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
    • C23C18/31Coating with metals
    • C23C18/32Coating with nickel, cobalt or mixtures thereof with phosphorus or boron
    • C23C18/34Coating with nickel, cobalt or mixtures thereof with phosphorus or boron using reducing agents
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M11/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/83Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with metals; with metal-generating compounds, e.g. metal carbonyls; Reduction of metal compounds on textiles
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M15/00Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/19Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
    • D06M15/37Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M15/643Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2101/00Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/16Synthetic fibres, other than mineral fibres
    • D06M2101/30Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M2101/32Polyesters
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2200/00Functionality of the treatment composition and/or properties imparted to the textile material
    • D06M2200/10Repellency against liquids
    • D06M2200/12Hydrophobic properties
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2200/00Functionality of the treatment composition and/or properties imparted to the textile material
    • D06M2200/25Resistance to light or sun, i.e. protection of the textile itself as well as UV shielding materials or treatment compositions therefor; Anti-yellowing treatments
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2200/00Functionality of the treatment composition and/or properties imparted to the textile material
    • D06M2200/35Abrasion, pilling or fibrillation resistance

Abstract

The invention discloses a preparation method of a super-hydrophobic fabric for anti-icing and photothermal deicing, which mainly comprises the steps of pretreating the fabric in NaOH solution, soaking the pretreated fabric in nickel-containing activating solution to prepare an activating layer of metallic nickel on the surface, soaking the fabric in nickel-containing alkaline plating solution to carry out surface nickel plating, and finally uniformly spraying a layer of PMHS and ink mixed solution on the surface to prepare the super-hydrophobic fabric for anti-icing and photothermal deicing. The nickel and the ink are used as the photothermal conversion material, so that the raw materials are easy to obtain and the cost is low; the chemical plating and spraying method is adopted, so that the operation process is simple; and the environment-friendly PMHS is adopted as the low-surface-energy modifier, so that the environment is more environment-friendly. The prepared coating material has good anti-icing and photo-thermal deicing performances, achieves the dual purposes of anti-icing and deicing, is suitable for large-area preparation and application, is suitable for clothes application, and is also suitable for the industrial fields of anti-icing, deicing and the like.

Description

Preparation method of super-hydrophobic fabric for anti-icing and photo-thermal deicing
Technical Field
The invention relates to a preparation method of a super-hydrophobic fabric for anti-icing and photo-thermal deicing, belonging to the field of application of the super-hydrophobic fabric with the photo-thermal effect.
Background
Icing is a common natural phenomenon, and serious ice accumulation problems can generate adverse effects on the fields of spaceflight, traffic, power communication and the like, and even cause serious disasters and economic losses. Current work clothes meet water in cold environment and can freeze rapidly for the fabric sclerosis becomes heavily, influences personnel's of dress work efficiency and comfort level greatly. Therefore, in cold weather conditions, it is necessary to develop an outdoor garment fabric with anti-icing and deicing functions.
For example, chinese patent CN112852289B discloses a super-hydrophobic anti-icing and de-icing coating with a photothermal effect and a preparation method thereof, which comprises the steps of preparing melanin nano particles with the photothermal effect from ink sacs, and modifying SiO by using perfluorodecyl triethoxysilane for hydrophobization 2 Nanoparticles, preparation of hydrophobic SiO 2 Nano particles, namely mixing melanin nano particles with polydimethylsiloxane to prepare a spraying solution, then spraying the spraying solution on a substrate to prepare a photo-thermal coating, and then performing hydrophobic treatment on SiO 2 The nano particle dispersion liquid is sprayed on the surface of the photo-thermal coating to obtain the super-hydrophobic anti-icing coating with the photo-thermal deicing performance, and the surface temperature of the super-hydrophobic anti-icing coating can reach 61.2-68.1 ℃ under the irradiation of sunlight intensity. For example, chinese patent CN108978200B discloses "a method for preparing a super-hydrophobic and lubricant-infused smooth woven fabric for anti-fouling and anti-icing", which comprises the steps of fabric pretreatment, zinc oxide nanorod growth, modification of low surface energy substances, lubricant infusion and the like, wherein in the step of lubricant modification and lubricant infusion of low surface energy substances, the fabric is immersed in a perfluorooctanoic acid ethanol solution for 24 hours to obtain super-hydrophobic performance, and the lubricant infusion is perfluoropolyether Krytox100 to obtain an infusion smooth surface.
Therefore, the polyester fabric-based anti-icing and photothermal deicing superhydrophobic fabric is prepared by taking metal nickel and carbon nanoparticles in ink as photothermal conversion materials and PMHS (poly dimethyl hydrogen siloxane) as a low surface energy modifier, and the anti-icing and deicing performance of the fabric can be effectively improved. The method is characterized in that a layer of metal nickel is loaded on the surface of the fabric in a chemical nickel plating mode, the photo-thermal property and the surface roughness of the fabric are improved, and in order to further improve the hydrophobic effect and the photo-thermal conversion property of the material, a mixed solution of PMHS and ink is sprayed on the surface of the fabric, so that the photo-thermal effect on the surface of the fabric is enhanced while the wettability of the surface of the fabric is changed. The prepared photo-thermal hydrophobic material effectively improves the anti-icing and deicing effects of the coating.
Disclosure of Invention
The invention aims to: the preparation method of the super-hydrophobic fabric for anti-icing and photo-thermal deicing is provided, the coating with anti-icing and photo-thermal deicing performances is prepared on the surface of the polyester fabric by adopting a simple chemical plating and spraying method, and the problems of high preparation cost, complex preparation process and the like of the existing photo-thermal material are solved.
The technical scheme of the invention is as follows:
step one, preparing a NaOH solution, and preparing the NaOH solution with a certain concentration at room temperature;
step two, preparing a nickel-containing activating solution, adding nickel acetate and sodium dihydrogen phosphate into deionized water according to a certain proportion to obtain a mixed activating solution of the nickel acetate and the sodium dihydrogen phosphate;
and step three, preparing nickel-containing alkaline plating solution, adding nickel sulfate, sodium dihydrogen phosphate, ammonium chloride and sodium citrate into deionized water according to a certain proportion, and adjusting the pH value of the plating solution by using ammonia water to obtain the nickel-containing alkaline plating solution.
And step four, preparing a mixed solution of PMHS and ink, adding a certain amount of PMHS and ink, and diluting with isopropanol serving as a solvent to prepare a uniformly dispersed PMHS and ink mixed solution.
Preparing a photo-thermal hydrophobic fabric, cutting the polyester fabric, preparing the photo-thermal hydrophobic fabric by adopting a chemical plating and spraying method, firstly pretreating the polyester fabric by using the NaOH solution, secondly soaking the fabric in the nickel-containing activating solution to prepare an activated layer of metal nickel on the surface of the fabric, then soaking the fabric plated with the nickel activated layer in the nickel-containing alkaline plating solution to carry out surface nickel plating, and finally uniformly spraying a layer of the prepared PMHS and ink mixed solution to obtain the photo-thermal hydrophobic fabric.
Further, the mass/volume concentration of the NaOH solution prepared in the first step is 70g/L.
Further, the mass ratio of the nickel acetate and the sodium dihydrogen phosphate in the nickel-containing activation solution prepared in the second step is 1: 1-2.
Further, the mass/volume concentrations of nickel sulfate, sodium dihydrogen phosphate, ammonium chloride and sodium citrate in the nickel-containing alkaline plating solution prepared in the third step are respectively as follows: 20g/L, 24g/L, 13.5g/L and 6.5g/L, and adjusting the pH value of the solution to 8-10 by using ammonia water.
Furthermore, in the step four, the mass ratio of the PMHS to the ink in the mixed solution of the PMHS and the ink is 1: 0.5-1.5.
Further, in the step five, in the preparation of the photo-thermal hydrophobic fabric, the preparation method adopting chemical plating and spraying comprises the following steps: cutting a polyester fabric, soaking the polyester fabric in NaOH pretreatment solution, treating for 1h at 70 ℃, washing with deionized water, and putting into an oven for drying. And then soaking the pretreated polyester fabric in a nickel-containing activation solution for 30min, and drying at 190 ℃ for 20min to prepare an activation layer of metal nickel on the surface of the fabric. And then soaking the fabric in nickel-containing alkaline plating solution for 20min at constant temperature, drying in an oven at 80 ℃ for 3h, and preparing the photothermal conversion material metal nickel layer on the surface of the fabric. And finally, fixing the fabric on a flat plate, spraying a mixed solution of a low surface energy substance PMHS and a photothermal conversion substance ink at a position 15cm away from the fabric by using an automatic spray gun, and curing for 4 hours at the temperature of 80 ℃ to obtain the polyester fabric-based anti-icing and photothermal deicing superhydrophobic fabric.
Further, spraying a mixed solution of PMHS and ink in the fifth step, wherein each spraying time is 25cm 2 The fabric of (2.5-3.5) mL is required.
The invention has the advantages that:
the nickel and the ink are used as the photothermal conversion material, so that the raw materials are easy to obtain and the cost is low.
The chemical plating and spraying method is adopted, and the operation process is simple.
The environment-friendly PMHS is adopted to replace fluorine-containing or long silicon carbon chain compounds to serve as the low surface energy modifier for preparing the hydrophobic surface of the material, so that the operation is simple, and the environment is more green and environment-friendly.
The contact angle between the hydrophobic surface prepared by the method and water can reach 141.18 degrees, the hydrophobic surface has good hydrophobic property, the temperature rise rate of the material is high, and the equilibrium temperature of 72 ℃ can be reached within 80 seconds under the irradiation intensity of sunlight. Under the condition of-15 ℃, the freezing time of water drops on the surface of the material can be delayed by 1018s, and the coating can be quickly melted and fall along the inclined plane bone under the irradiation of sunlight after being frozen, so that the material is proved to have good anti-icing and photo-thermal deicing performances, and the dual purposes of anti-icing and deicing are achieved. In addition, the prepared fabric surface has good wear resistance and ultraviolet resistance, and can be used outdoors for a long time.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without inventive exercise. Wherein the content of the first and second substances,
FIG. 1 is a surface SEM image of a superhydrophobic fabric for anti-icing and photo-thermal deicing prepared in the first example;
FIG. 2 is a surface SEM image of an untreated polyester fabric;
FIG. 3 is a surface SEM image of a polyester fabric-based nickel-plated fabric prepared as described in comparative example one;
FIG. 4 is a surface SEM image of a sprayed PMHS and ink mixed solution coating based on a polyester fabric prepared as described in comparative example II;
FIG. 5 is a graph comparing the contact angles of the hydrophobic surface of the superhydrophobic fabric for anti-icing and photo-thermal deicing prepared in the first example with the contact angles of the surface of the untreated polyester fabric, the surface of the fabric prepared in the first comparative example, and the surface of the fabric prepared in the second comparative example;
FIG. 6 is a graph comparing the absorption spectrum ranges of a fabric for anti-icing and thermal de-icing made in the first example with an untreated polyester fabric material, a fabric made in the first comparative example, and a fabric made in the second comparative example;
FIG. 7 shows 1000W/m of a fabric prepared in example one and used for anti-icing and photothermal deicing compared with an untreated polyester fabric material, a fabric prepared in comparative example one and a fabric prepared in comparative example two 2 Temperature change graph under illumination intensity;
FIG. 8 is a graph showing the test of the photothermal conversion durability of a fabric for ice protection and photothermal deicing prepared in the first example;
FIG. 9 is a graph comparing the temperature change at different light intensities for a fabric for anti-icing and thermal de-icing made in the first example;
FIG. 10 is a graph showing the test of photoresponse sensitivity and photothermal stability of a fabric for ice protection and photothermal deicing prepared in the first example;
FIG. 11 is a graph comparing the freezing time of the surface of a fabric for anti-icing and thermal de-icing made in example one with the freezing time of the surface of a fabric made in comparative example one and a fabric made in comparative example two;
FIG. 12 is a graph comparing the ice adhesion strength on the surface of a fabric for anti-icing and photo-thermal deicing made in example one with the fabric made in comparative example one and the fabric made in comparative example two;
FIG. 13 is a graph comparing the time for which the ice layer melts under one solar illumination intensity for one fabric prepared in example one for anti-icing and photo-thermal deicing with the fabric prepared in comparative example one and the fabric prepared in comparative example two;
FIG. 14 is a graph showing the abrasion resistance test of a fabric for ice protection and thermal deicing prepared in the first example;
FIG. 15 is a graph showing the UV resistance of a fabric for anti-icing and thermal deicing prepared in the first example;
Detailed Description
In order to make the above objects, features and advantages of the present invention more comprehensible, embodiments accompanying figures, examples and comparative examples are described further below. The invention is not limited to the embodiments shown but also encompasses any other known variations within the scope of the invention as claimed.
First, reference herein to "embodiment one" or "embodiment one" means that a particular feature, structure, or characteristic described in connection with the embodiment is included in at least one implementation of the invention. The present invention is described in detail by using the schematic structural diagrams, etc., and for convenience of illustration, the schematic diagrams are not enlarged partially according to the general scale when describing the embodiments of the present invention, and the schematic diagrams are only examples, which should not limit the scope of the present invention. In addition, the actual fabrication process should include three-dimensional space of length, width and depth.
In addition, the acronyms referred to in the invention are all fixed acronyms in the field, wherein part of the letters are explained as follows: PET: a polyester fabric; PMHS: polydimethylhydrosiloxane; SEM: the image is displayed by electronic scanning.
Example one
The super-hydrophobic fabric for anti-icing and photothermal deicing is prepared according to the following steps;
firstly, preparing NaOH solution of pretreatment solution
Slowly dripping a certain amount of NaOH into water at room temperature, and preparing 500mL of pretreatment solution with the mass/volume concentration of 70 g/L;
second step, preparing activation liquid containing nickel
Respectively adding 3g of nickel acetate and 4.5g of sodium dihydrogen phosphate into deionized water to prepare 60mL of activating solution;
third step, preparing nickel-containing alkaline plating solution
4g of nickel sulfate, 6g of sodium dihydrogen phosphate and 3.375g of ammonium chloride and 1.625g of sodium citrate are respectively added into deionized water, and the pH value of the plating solution is adjusted to 9 by ammonia water, so that 250mL of nickel-containing alkaline plating solution is obtained.
Step four, preparing a mixed solution of PMHS and ink
Using isopropanol as a solvent, 3mL of a mixed solution was prepared from PMHS and ink in a mass ratio of 1: 1.
Step five, preparing the photo-thermal hydrophobic fabric
Cutting a 5 x 5cm polyester fabric, soaking the polyester fabric in a pretreatment solution of NaOH, fully soaking the polyester fabric for 1 hour at 70 ℃, washing the polyester fabric with deionized water, and then putting the polyester fabric into an oven for drying. And then soaking the pretreated polyester fabric in a nickel-containing activating solution for ultrasonic treatment for 30min, taking out the fabric, and then drying the fabric in a baking oven at 190 ℃ for 20min to obtain an activated layer of metal nickel on the surface of the fabric. And then soaking the fabric in nickel-containing alkaline plating solution for 20min at the constant temperature of 50 ℃, putting the fabric in an oven at the temperature of 80 ℃ for drying for 3h, and preparing the photothermal conversion material metal nickel layer on the surface of the fabric. And finally, fixing the fabric on a flat plate, spraying 3mL of mixed solution of a low-surface-energy substance PMHS and photothermal conversion substance ink at a position 15cm away from the fabric by using an automatic spray gun, and curing at 80 ℃ for 4 hours to obtain the polyester fabric-based anti-icing and photothermal deicing hydrophobic fabric.
Referring to fig. 1, the surface condition of a superhydrophobic fabric for anti-icing and photo-thermal deicing manufactured in this embodiment is shown, and fig. 1 is a surface SEM image of the fabric manufactured in the first embodiment of the present invention. As shown in figure 1, the polyester fabric surface after chemical nickel plating treatment and spraying treatment has a large amount of uniform fabric.
Referring to fig. 5, fig. 5 shows the static contact angle of water on the hydrophobic surface of the superhydrophobic fabric for anti-icing and photothermal deicing according to this embodiment. As shown in fig. 5, the hydrophobic surface prepared in the first embodiment has a static contact angle of 141.18 ° with water, and has good hydrophobic property.
Referring to fig. 6, fig. 6 shows an absorption spectrum range of the fabric prepared in the first embodiment of the present invention, and as shown in fig. 6, a light absorption rate of the fabric prepared in the first embodiment of the present invention accounts for more than 97% of a whole wavelength range, and the fabric has a good light absorption performance.
Comparative example 1
The comparative scheme prepares a nickel-plated fabric according to the following steps;
firstly, preparing NaOH solution of pretreatment solution
Slowly dropping a certain amount of NaOH into deionized water at room temperature to prepare 500mL of pretreatment solution with the mass/volume concentration of 70 g/L;
second step, preparing activation liquid containing nickel
Respectively adding 3g of nickel acetate and 4.5g of sodium dihydrogen phosphate into deionized water to prepare 60mL of activating solution;
third step, preparing nickel-containing alkaline plating solution
4g of nickel sulfate, 6g of sodium dihydrogen phosphate, 3.375g of ammonium chloride and 1.625g of sodium citrate are respectively added into deionized water, and the pH value of the plating solution is adjusted to 9 by ammonia water, so that 250mL of nickel-containing alkaline plating solution is obtained.
Step four, preparing the nickel-plated fabric
Cutting a 5 x 5cm polyester fabric, soaking the fabric in a pretreatment solution of NaOH, fully soaking the fabric for 1h at 70 ℃, washing the fabric with deionized water, and drying the fabric in an oven. And then soaking the pretreated polyester fabric in activation solution containing nickel for ultrasonic treatment for 30min, taking out the fabric, placing the fabric in an oven at 190 ℃ for drying for 20min, and preparing an activation layer of metal nickel on the surface of the fabric. And then soaking the fabric in nickel-containing alkaline plating solution for 20min at the constant temperature of 50 ℃, drying in an oven at 80 ℃ for 3h to obtain a metal nickel layer on the surface of the fabric, thus obtaining the nickel-plated fabric based on the polyester fabric.
Referring to fig. 3, the surface condition of a polyester fabric-based nickel-plated fabric prepared in this comparative example is shown, and fig. 3 is a surface SEM image of the fabric prepared in the comparative example of the present invention. As shown in fig. 3, the polyester fabric surface subjected to the electroless nickel plating treatment is uniformly loaded with a metal nickel layer.
The water static contact angle of the surface of the nickel-plated fabric based on the polyester fabric prepared in the comparative example is shown in fig. 5, and fig. 5 contains the water static contact angle of the surface of the fabric prepared in the comparative example of the present invention. As shown in fig. 5, the surface prepared in the first comparative example had a static contact angle of water of 67.14 °, and exhibited hydrophilic properties.
Referring to fig. 6, fig. 6 shows the absorption spectrum range of the fabric prepared in the first comparative example of the present invention, and as shown in fig. 6, the light absorption rate of the fabric prepared in the first comparative example accounts for more than 90% of the entire wavelength range, and has better light absorption performance, but is slightly lower than that of the first example.
Comparative example No. two
According to the comparison scheme, the fabric sprayed with the PMHS and ink mixed solution is prepared according to the following steps;
firstly, preparing NaOH solution of pretreatment solution
Slowly dropping a certain amount of NaOH into water at room temperature, and preparing 500mL of pretreatment solution with the mass/volume concentration of 70 g/L;
second step, preparing mixed solution of PMHS and ink
Using isopropanol as a solvent, 3mL of a mixed solution was prepared from PMHS and ink in a mass ratio of 1: 1.
Thirdly, preparing the fabric sprayed with the PMHS and the ink mixed solution
Cutting a 5 x 5cm polyester fabric, soaking the fabric in a pretreatment solution of NaOH, fully soaking the fabric for 1h at 70 ℃, washing the fabric with deionized water, and drying the fabric in an oven. Then, the fabric was fixed on a flat plate, 3mL of the mixed solution of PMHS and photothermal conversion substance ink, which is a low surface energy substance, was sprayed at a position 15cm away from the flat plate using an automatic spray gun, and cured at 80 ℃ for 4 hours, to prepare a polyester fabric-based fabric sprayed with the mixed solution of PMHS and ink.
Referring to fig. 4, the surface condition of a fabric prepared by spraying a PMHS and ink mixed solution on a polyester-based fabric according to the comparative example is shown in fig. 4, which is a surface SEM image of a fabric prepared according to the comparative example of the present invention. As shown in fig. 4, the surface of the polyester fabric subjected to the spray coating treatment was loaded with a large amount of PMHS and carbon clusters in the ink.
Referring to fig. 5, the static contact angle of water on the hydrophobic surface of a fabric prepared by spraying PMHS and ink mixed solution on a polyester-based fabric prepared in this example is shown in fig. 5, which includes the static contact angle of water on the hydrophobic surface of a fabric prepared in comparative example two of the present invention. As shown in fig. 5, the hydrophobic surface prepared in the second comparative example has a static contact angle of 135.72 ° with water, and has good hydrophobic properties.
Referring to fig. 6, the photo-thermal performance of a fabric prepared in this comparative example and based on a mixed solution of polyester sprayed PMHS and ink is shown in fig. 6, where fig. 6 shows the absorption spectrum range of the fabric prepared in the second comparative example of the present invention, and as shown in fig. 6, the light absorption rate of the fabric prepared in the second comparative example accounts for more than 90% of the whole wavelength range, and has better light absorption performance, but is slightly lower than that of the first example.
In order to characterize the elemental composition of the surface of the different samples, table 1 is a table of the elemental composition of the surface of a superhydrophobic fabric for anti-icing and photo-thermal deicing prepared in example one with the surface of an untreated polyester fabric, the surface of a nickel-plated fabric prepared in comparative example one, and the surface of a fabric sprayed with a PMHS and ink mixed solution prepared in comparative example two.
TABLE 1
Figure BSA0000274667900000061
Referring to table 1, by comparing the contents of C, O, ni, and P elements of the surfaces of the four samples, the surfaces of the untreated polyester fabric and the fabric prepared in the comparative example in which the content of C element in the fabric prepared by spraying the PMHS and ink mixed solution reached 67.7% due to the attachment of carbon nano-particles to the fiber surface in the PMHS and ink mixed solution were mainly comprised of C and O. The Ni content of the fiber surface after the electroless nickel plating treatment of comparative example one was increased to 65.25%, while the C and O element contents were 21.71% and 8.88%, respectively. Compared with the fabric prepared in the comparative example I, the content of the C element on the surface of the fabric prepared in the example I is increased from 21.71% to 53.17%, and further the successful attachment of the carbon particles on the surface of the material is proved, and the metal nickel nanoparticles and the carbon nanoparticles can be uniformly coated on the surface of the fiber as shown in Table 1.
Referring to fig. 7, fig. 7 shows a superhydrophobic fabric for anti-icing and thermal deicing prepared in the first example and an untreated polyester fabric, compared with each otherThe fabric prepared in example one and the fabric prepared in comparative example two were at 1000W/m 2 Temperature change under illumination intensity is compared with graph. By contrast, the superhydrophobic fabric for anti-icing and photothermal deicing prepared in the first example reaches 72 ℃ after being irradiated for 80 seconds, and is superior to the photothermal conversion efficiency of the untreated polyester fabric, the fabric prepared in the first comparative example and the fabric prepared in the second comparative example.
Referring to fig. 8, fig. 8 is a test chart of the photothermal conversion durability of the superhydrophobic fabric for anti-icing and photothermal deicing prepared in the first embodiment, and when the superhydrophobic fabric for anti-icing and photothermal deicing prepared in the first embodiment is placed in the air for 8 months, as shown in fig. 8, the equilibrium temperature reached by photothermal conversion does not drop significantly, and the photothermal conversion performance is proved to be stable under long-term illumination and to have good durability.
Referring to fig. 9, fig. 9 is a graph comparing the temperature change of the superhydrophobic fabric for anti-icing and photothermal deicing prepared in the first embodiment under different illumination intensities, and when the superhydrophobic fabric for anti-icing and photothermal deicing prepared in the first embodiment is placed under different illumination intensities, as shown in fig. 9, the surface temperature rise is positively correlated with the illumination intensity, which indicates that the fabric can achieve the photothermal deicing effect under different illumination intensities.
Referring to fig. 10, fig. 10 is a test chart of the photoresponse sensitivity and the photothermal stability of the superhydrophobic fabric for anti-icing and photothermal deicing prepared in the first embodiment, the superhydrophobic fabric for anti-icing and photothermal deicing prepared in the first embodiment is placed under a xenon lamp simulating sunlight for a plurality of times of light and no light cycle tests, as shown in fig. 10, after the xenon lamp is turned on and off, the surface temperature of the superhydrophobic fabric changes immediately, which indicates that the prepared fabric has good photoresponse sensitivity, and the temperature change trend of each switching period is consistent, thus proving that the superhydrophobic fabric has good photothermal stability.
Referring to fig. 11, fig. 11 is a graph comparing the freezing time of the surfaces of the superhydrophobic fabric for anti-icing and thermal deicing prepared in the first example with the freezing time of the surfaces of the fabric prepared in the first comparative example and the fabric prepared in the second comparative example, and 10 μ L of water is dropped on the surfaces of the fabric prepared in the first example, the first comparative example and the second comparative example, as shown in fig. 11, the freezing time of the water drops on the surfaces of the three fabrics is 1018 ± 242s, 60 ± 20s and 599 ± 94s, respectively, and it is apparent that the freezing time of the fabric prepared in the first example is prolonged to the maximum under the same conditions, and the fabric prepared in the first example has good anti-icing performance.
Referring to fig. 12, fig. 12 is a graph comparing ice adhesion strength of the surfaces of the superhydrophobic fabric for anti-icing and thermal deicing prepared in example one with those of the fabric prepared in comparative example one and the fabric prepared in comparative example two, and the three samples were exposed to-15 ℃, as shown in fig. 12, ice adhesion strength of the surfaces of the fabric prepared in example one was 55.14kPa, ice adhesion strength of the surfaces of the fabric prepared in comparative example one was 135kPa, and ice adhesion strength of the surfaces of the fabric prepared in comparative example two was 64.74kPa, demonstrating that the fabric prepared in example one has good ice shedding performance and low ice adhesion strength.
Referring to fig. 13, fig. 13 is a comparison graph of the time for melting the ice layer under one sunlight intensity between the superhydrophobic fabric for anti-icing and thermal deicing prepared in the first example and the fabric prepared in the second example, and three fabrics with the ice layer of 3mm thickness attached on the surface are placed under one sunlight intensity condition of-10 ℃, as shown in fig. 13, the surface ice melting of the fabric prepared in the first example into liquid water only needs 455s, which is far lower than that of the fabric prepared in the first and second examples, and the photothermal conversion performance of the fabric prepared in the first example is better and the thermal deicing performance is good.
Referring to fig. 14, fig. 14 is a graph illustrating the wear resistance of the fabric for anti-icing and photothermal deicing prepared in the first embodiment, as shown in fig. 14, after the fabric prepared in the first embodiment is subjected to multiple rubbing cycles, the contact angle of the surface of the fabric tends to decrease slightly, but after 8 cycles, the contact angle is still over 130 °, and good hydrophobicity is shown, which proves that the fabric has good wear resistance.
Referring to fig. 15, fig. 15 is a test chart of ultraviolet resistance of the fabric for anti-icing and photo-thermal deicing prepared in the first example, as shown in fig. 5, after the fabric prepared in the first example is irradiated by ultraviolet rays for a long time, the contact angle of the surface of the fabric does not change significantly, and the contact angle is still maintained to be more than 138 ° after the fabric is irradiated for 6 hours, which proves that the fabric has good ultraviolet resistance.
In conclusion, the invention discloses a preparation method of a super-hydrophobic fabric for anti-icing and photo-thermal deicing, which is more environment-friendly on the basis of the existing fabric preparation technology, mild in preparation conditions, simple and convenient in process, easy to operate, suitable for large-area preparation and application, suitable for clothes application, and also suitable for industrial fields such as anti-icing and deicing.
It should be noted that the above examples and comparative examples are only intended to illustrate the technical solutions of the present invention, and not to limit the present invention, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions may be made to the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention, which should be covered by the scope of the claims of the present invention.

Claims (7)

1. A preparation method of a super-hydrophobic fabric for anti-icing and photothermal deicing is characterized by mainly comprising the following steps: the method comprises the steps of soaking the polyester fabric in NaOH solution for pretreatment experiment, soaking the pretreated polyester fabric in nickel-containing activating solution to prepare a nickel activating layer, soaking the fabric in nickel-containing alkaline plating solution to prepare a metal nickel layer, and uniformly spraying a layer of mixed solution of PMHS and ink on the surface of the metal nickel layer to prepare the super-hydrophobic fabric for anti-icing and photo-thermal deicing.
2. The method of claim 1, wherein the NaOH solution is formulated at room temperature and has a mass-volume concentration of 70g/L. The polyester fabric is soaked in NaOH solution for pretreatment experiment at 60-70 deg.c for 1-2 hr.
3. The method for preparing the nickel-containing activating solution according to claim 1, wherein the mixed activating solution of nickel acetate and sodium dihydrogen phosphate is prepared by adding nickel acetate and sodium dihydrogen phosphate into deionized water according to a certain proportion, wherein the mass ratio of nickel acetate to sodium dihydrogen phosphate is 1: 1-1: 2. And (3) soaking the pretreated polyester fabric in a nickel-containing activation solution for 30min, and then drying the polyester fabric for 20min at 190 ℃ to obtain an activation layer of metal nickel on the surface of the fabric.
4. The method for preparing the nickel-containing alkaline plating solution according to claim 1, characterized in that nickel sulfate, sodium dihydrogen phosphate, ammonium chloride and sodium citrate are added into deionized water according to a certain proportion, and the pH value of the plating solution is adjusted by ammonia water to prepare the nickel-containing alkaline plating solution, wherein the mass-volume concentrations of the nickel sulfate, the sodium dihydrogen phosphate, the ammonium chloride and the sodium citrate are respectively as follows: 20g/L, 24g/L, 13.5g/L and 6.5g/L, and the pH value is 8-10. And (3) soaking the fabric with the nickel activation layer attached to the surface in nickel-containing alkaline plating solution at a constant temperature of 50 ℃ for 20min, and then drying the fabric in an oven at 80 ℃ for 3h to obtain a metal nickel layer on the surface of the fabric.
5. The method of claim 1, wherein isopropyl alcohol is used as a solvent, and the ratio of PMHS to ink is 1: 0.5 to 1: 1.5 by mass. Fixing the fabric attached with the metallic nickel layer on a flat plate, spraying a mixed solution of PMHS and ink at a position 15cm away from the flat plate by using an automatic spray gun, and curing for 4 hours at the temperature of 80 ℃ to obtain the polyester fabric-based super-hydrophobic fabric for anti-icing and photo-thermal deicing.
6. The method for preparing the superhydrophobic fabric for anti-icing and photothermal deicing according to claim 5, wherein the mixed solution of PMHS and ink is sprayed for 25cm 2 The fabric of (2.5) to (3.5) mL is required.
7. A superhydrophobic fabric for anti-icing and photothermal deicing obtained by the preparation method according to any one of claims 1 to 6, having particular application in the fields of anti-icing and deicing.
CN202210664127.8A 2022-06-14 2022-06-14 Preparation method of super-hydrophobic fabric for anti-icing and photo-thermal deicing Pending CN115161992A (en)

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