CN114989701A - Anti-icing type electric heating hydrophobic coating and preparation method and application thereof - Google Patents

Anti-icing type electric heating hydrophobic coating and preparation method and application thereof Download PDF

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CN114989701A
CN114989701A CN202210818940.6A CN202210818940A CN114989701A CN 114989701 A CN114989701 A CN 114989701A CN 202210818940 A CN202210818940 A CN 202210818940A CN 114989701 A CN114989701 A CN 114989701A
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hydrophobic coating
icing
slurry
icing type
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张丹
范佳宇
司鹏翔
吴赟
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Jiangnan University
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Abstract

The invention discloses an anti-icing type electric heating hydrophobic coating, and a preparation method and application thereof, and belongs to the technical field of materials. The raw materials of the anti-icing type electric heating hydrophobic coating comprise the following components in parts by mass: 20-50 parts of epoxy resin, 50-80 parts of copper-clad silver powder, 4-10 parts of carbon black, 4-10 parts of boron nitride powder, 4-10 parts of carbon nano tube and SiO 2 2-8 parts of nano particles, 3-4 parts of triethylene tetramine, 4-7 parts of a defoaming agent, 4-5 parts of a dispersing agent, 3-5 parts of an adhesive and 2-5 parts of a thickening agent. The anti-icing type electric heating hydrophobic coating has better electric conductivity, heating performance and hydrophobic performance, and can improve the anti-icing and anti-icing performance of the surface of the original materialThe service life of the material in an extremely cold or easily frozen environment is prolonged; the raw materials used in the invention are all nontoxic and harmless, meet the environmental protection requirement, and can be used on various outdoor anti-icing and anti-skid base materials.

Description

Anti-icing type electric heating hydrophobic coating and preparation method and application thereof
Technical Field
The invention relates to an anti-icing type electric heating hydrophobic coating, a preparation method and application thereof; belongs to the technical field of materials.
Background
Icing is a common natural phenomenon in winter, and can cause serious icing/icing problems in the engineering fields of electric power, energy, traffic and the like. The ice formation/covering phenomenon is more serious in high and cold and strong wind and sand areas, for example, once a speed measuring radar and a bogie of a high-speed railway locomotive are covered with ice, the operation safety is greatly reduced; the coastal power generation fan blades are easy to form ice under the condition of great day and night temperature difference, so that the power generation efficiency is greatly reduced. The conventional coating can not meet the use requirements under severe environments of high and cold temperature, strong temperature and the like, and how to deal with and reduce the surface icing is a serious challenge at present.
At present, two main methods for preventing materials from icing comprise constructing a super-hydrophobic surface and adding special materials; the super-hydrophobic surface is obtained by coating a low-surface-energy material on a rough surface, and the low-surface-energy material has better waterproof performance and low surface energy, so that water droplets can be effectively removed, and the super-hydrophobic surface is widely applied to the field of anti-icing. However, there is a limitation in anti-icing applications because the superhydrophobic surface loses its superhydrophobic properties due to adsorption and condensation caused by temperature drop and during the process of icing and deicing.
Therefore, the problem of anti-icing of outdoor infrastructure materials for environments such as severe cold and strong sand wind still faces huge challenges.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide an anti-icing type electric heating hydrophobic coating, and a preparation method and application thereof, so as to solve the problems in the prior art. The anti-icing type electric heating hydrophobic coating can effectively improve the anti-icing and anti-icing capacity of the surface of the material by virtue of excellent heating and hydrophobic properties, well solves the problem that the outdoor base material is easy to ice/ice in extremely cold or easily damp and cold areas, does not cause any pollution to the environment, and provides a new product for the selection of the anti-icing coating in the market to a certain extent.
In order to achieve the purpose, the invention provides the following technical scheme:
the invention aims to provide an anti-icing type electric heating hydrophobic coating, which comprises the following raw materials in parts by mass: 20-50 parts of epoxy resin, 50-80 parts of copper-clad silver powder, 4-10 parts of carbon black, 4-10 parts of boron nitride powder, 4-10 parts of carbon nano tube and SiO 2 2-8 parts of nano particles, 3-4 parts of triethylene tetramine, 4-7 parts of a defoaming agent, 4-5 parts of a dispersing agent, 3-6 parts of an adhesive and 2-5 parts of a thickening agent.
Epoxy resins have many excellent characteristics: (1) the curing is convenient, and the curing can be carried out at 0-180 ℃; (2) the adhesive force is strong, the existence of inherent polar hydroxyl and ether bond in the molecular chain of the epoxy resin enables the epoxy resin to have very high adhesive force to various substances, the contractibility of the epoxy resin during curing is low, the generated internal stress is small, and the adhesive strength is also improved; (3) mechanical properties: the cured epoxy resin system has excellent mechanical property; (4) the chemical stability is strong: the cured epoxy resin system has excellent alkali resistance, acid resistance and solvent resistance.
The copper-clad silver powder is formed by forming silver coatings with different thicknesses on the surface of superfine copper powder by adopting an advanced chemical plating technology through a specific forming and surface treatment process; it not only overcomes the characteristic of copper powder easy to be oxidized, but also has the characteristics of good conductivity, high chemical stability, difficult oxidation, low price and the like, and is a high-conductivity filler with development prospect.
The carbon black has fine carbon black particles with a high structure, a net chain is tightly stacked, the specific surface area is large, the number of particles per unit mass is large, a chain type conductive structure can be formed in a polymer, the carbon black has excellent conductive performance, the carbon black particles have a microcrystalline structure, the arrangement of carbon atoms is ordered, and the carbon black has a certain effect on constructing a micro-nano structure on the surface of a coating.
The boron nitride powder has excellent heat conductivity, high strength, high resistivity and excellent corrosion resistance, can be used as a heat transfer filler and has a certain effect on the environment corrosion resistance of an outdoor coating.
The carbon nano tube has high modulus and high strength, higher electrical conductivity and thermal conductivity, is a better filler as a heat transfer coating, can improve stable heat transfer and simultaneously can keep the friction resistance of the coating, and is used as a one-dimensional nano material, has light weight, perfect connection of a hexagonal structure and strong surface activity, is combined with a large amount of surface groups, and is favorable for constructing a super-hydrophobic coating.
SiO 2 The nano particles have high strength, high extensibility and excellent surface micro-nano structure, so that the phenomenon that the super-hydrophobic surface is easy to scratch and wear can be effectively prevented, and the hydrophobic performance of the coating is improved.
In one embodiment of the present invention, the epoxy resin includes one or more of bisphenol a type epoxy resin, bisphenol F type epoxy resin, polyphenol type glycidyl ether epoxy resin, aliphatic glycidyl ether epoxy resin, glycidyl ester type epoxy resin.
In one embodiment of the invention, the dispersant comprises one or more of triethylhexyl phosphoric acid, sodium dodecyl sulfate, sodium tripolyphosphate, and polyacrylamide.
In one embodiment of the invention, the defoamer comprises one or more of polydimethylsiloxane, isopropanol, fatty acid amide.
In one embodiment of the invention, the thickener comprises one or more of myristyl alcohol, sodium alginate propylene glycol, polyurethane, diallyl phthalate.
In one embodiment of the invention, the binder comprises one or more of polyvinyl alcohol, polystyrene, polyacrylate.
In one embodiment of the present invention, the copper-clad silver powder is 50 parts, 60 parts, 70 parts or 80 parts.
In one embodiment of the invention, the raw materials of the coating comprise the following components in parts by mass: 40 parts of epoxy resin, 70 parts of copper-clad silver powder, 8 parts of carbon black, 8 parts of boron nitride powder, 8 parts of carbon nano tube and SiO 2 6 parts of nano particles, 4 parts of triethylene tetramine, 6 parts of defoaming agent, 5 parts of dispersing agent, 5 parts of adhesive and 4 parts of thickening agent.
The second purpose of the invention is to provide a preparation method of an anti-icing type electric heating hydrophobic coating, which comprises the following steps:
(1) adding epoxy resin, copper-coated silver powder, carbon black and a dispersing agent into a planetary stirrer, and uniformly stirring and mixing to obtain slurry A;
(2) adding boron nitride powder into the grinding machine, and grinding to obtain slurry B;
(3) continuously adding the carbon nano tube and SiO into the slurry B prepared in the step (2) 2 Fully and uniformly grinding the nano particles and the dispersing agent to obtain slurry C;
(4) adding a defoaming agent into the slurry C prepared in the step (3), fully mixing, and then putting into an ultrasonic dispersion machine for ultrasonic dispersion to obtain a slurry D in a wire-drawing viscous state;
(5) adding the slurry A prepared in the step (1) and the slurry D prepared in the step (4) into a planetary stirrer at the same time, continuously stirring, and then adding triethylene tetramine, an adhesive and a thickening agent to obtain slurry E;
(6) and (4) adding the slurry E prepared in the step (5) into a spraying machine, spraying the slurry E on a base material, and heating and curing to obtain the anti-icing type electric heating hydrophobic coating.
In one embodiment of the present invention, the rotation speed of the stirring in step (1) is 800-1200 rpm, and the time is 40-50 minutes.
In one embodiment of the present invention, the grinding machine rotation speed 1200-.
In one embodiment of the present invention, the fully ground grinder in step (3) has a rotation speed of 1500-.
In one embodiment of the present invention, the time for the ultrasonic dispersion in the step (4) is 30 to 40 minutes.
In one embodiment of the invention, the rotation speed of the planetary stirrer in the step (5) is 500-800 rpm, and the time is 20-30 minutes.
In one embodiment of the present invention, the temperature of the heat curing in the step (6) is: 100-150 ℃.
The third purpose of the invention is to provide the application of the anti-icing type electric heating hydrophobic coating in the anti-icing/anti-icing of the outdoor substrate.
The beneficial effects of the invention are:
(1) the invention is the common use of composite materials, enhances the performance of the original single material, and has the effect that one plus one is more than two; the preparation process is simple to operate, has high practicability and can provide good economic benefits; the raw materials are safe and harmless, and the environment is friendly.
(2) The anti-icing type electric heating hydrophobic coating prepared by the invention can solve the problems that the deicing coating is easy to corrode and fall off in the market, and the prepared anti-icing type electric heating hydrophobic coating has better electrical conductivity, thermal conductivity and hydrophobic property.
(3) The anti-icing type electric heating hydrophobic coating prepared by the invention is divided into two layers, the bottom layer is an electric heating coating taking copper-clad silver powder as a heating layer, carbon black, carbon nano tubes and boron nitride as heat transfer layers, epoxy resin as a substrate, and the top layer is coated with SiO 2 The super-hydrophobic coating is constructed by taking the nano particles as a main filler and taking the epoxy resin as a substrate, the nano particles and the epoxy resin are combined together, meanwhile, due to the special structures of the carbon black and the carbon nano tubes, the hydrophobic property of the top super-hydrophobic coating is enhanced, the coating is wide in application range, and can be used on various outdoor anti-icing and anti-skid base materials.
Drawings
FIG. 1 is a sample diagram of an anti-icing type electrothermal hydrophobic coating prepared by examples 1-4 of the present invention and a schematic structural diagram of the coating; wherein, the leftmost side in the graph is a sample electrothermal graph; the far right side of the figure is the sample superhydrophobicity map;
FIG. 2 is a contact angle diagram of an anti-icing type electrothermal hydrophobic coating prepared in example 3 of the present invention;
FIG. 3 is a thermal image of an anti-icing type electrothermal hydrophobic coating prepared in example 3 of the present invention;
FIG. 4 is an SEM image of an electric heating layer of the anti-icing type electric heating hydrophobic coating prepared in example 3 of the invention;
FIG. 5 is an SEM image of a super-hydrophobic layer of the anti-icing type electrothermal hydrophobic coating prepared in example 3 of the present invention;
FIG. 6 is a graph showing the results of testing the conductivity and resistivity of an anti-icing type electrothermal hydrophobic coating prepared from copper-clad silver powder of different components in comparative example 32;
FIG. 7 is an SEM image of an anti-icing type electrothermal hydrophobic coating prepared by carbon black and carbon nanotubes of different compositions in comparative example 34.
Detailed Description
The present invention will be further explained with reference to examples, but the present invention is not limited to the examples.
Copper-clad silver powder (DK-Ag-CU-3um, more than or equal to 99.95%): beijing Dekoku island gold technologies, Inc.; carbon nanotubes (MWCNTs, 15-30um, 97% or more): shenzhen Tuling evolution technology Limited.
Example 1
An anti-icing type electric heating hydrophobic coating comprises the following raw materials in percentage by mass:
20 parts of epoxy resin, 50 parts of copper-clad silver powder, 4 parts of carbon black, 4 parts of boron nitride powder, 4 parts of carbon nano tube and SiO 2 2 parts of nano particles, 3 parts of triethylene tetramine, 4 parts of defoaming agent (polydimethylsiloxane), 4 parts of dispersing agent (sodium dodecyl sulfate), 3 parts of adhesive (polyvinyl alcohol) and 2 parts of thickening agent (propylene glycol sodium alginate).
The preparation method of the anti-icing type electric heating hydrophobic coating specifically comprises the following steps:
(1) adding 20 parts of epoxy resin, 50 parts of copper-coated silver powder, 4 parts of carbon black and 2 parts of dispersing agent into a planetary stirrer, stirring for 40-50 minutes at the rotating speed of 800-;
(2) adding 4 parts of boron nitride powder into the grinding machine, grinding for 40-60 minutes at the rotation speed of 1200-2000 r/min to obtain slurry B;
(3) continuously adding 4 parts of carbon nano tube and SiO into the slurry B in the step (2) 2 2 parts of nano particles, 2 parts of dispersing agent, grinding for 30-50 minutes, and fully grinding at the rotating speed of the grinding machine of 1500-Obtaining slurry C after homogenizing;
(4) adding 4 parts of defoaming agent into the slurry C prepared in the step (3), fully mixing, and then putting into an ultrasonic dispersion machine for dispersion for 30-40 minutes to obtain slurry D which is uniformly dispersed and is in a wire-drawing sticky state;
(5) adding the slurry A prepared in the step (1) and the slurry D prepared in the step (4) into a planetary stirrer at the same time, stirring for 20-30 minutes at the rotation speed of the stirrer of 500-800 rpm, and simultaneously adding 3 parts of triethylene tetramine, 3 parts of adhesive and 2 parts of thickening agent to obtain slurry E;
(6) and (4) adding the slurry E prepared in the step (5) into a spraying machine, spraying the slurry E on a base material, and heating and curing to obtain the anti-icing type electric heating hydrophobic coating.
Example 2
An anti-icing type electric heating hydrophobic coating comprises the following raw materials in percentage by mass:
30 parts of epoxy resin, 60 parts of copper-clad silver powder, 6 parts of carbon black, 6 parts of boron nitride powder, 6 parts of carbon nano tube and SiO 2 4 parts of nano particles, 3 parts of triethylene tetramine, 5 parts of defoaming agent (polydimethylsiloxane), 4 parts of dispersing agent (sodium dodecyl sulfate), 3 parts of adhesive (polyvinyl alcohol) and 3 parts of thickening agent (propylene glycol sodium alginate).
A preparation method of an anti-icing type electric heating hydrophobic coating specifically comprises the following steps:
(1) adding 30 parts of epoxy resin, 60 parts of copper-coated silver powder, 6 parts of carbon black and 2 parts of dispersing agent into a planetary stirrer, stirring for 40-50 minutes at the rotating speed of 800-;
(2) adding 6 parts of boron nitride powder into the grinding machine, grinding for 40-60 minutes at the rotation speed of 1200-2000 r/min to obtain slurry B;
(3) continuously adding 6 parts of carbon nano tube and SiO into the slurry B in the step (2) 2 4 parts of nano particles and 2 parts of dispersing agent, grinding for 30-50 minutes at a grinding machine rotation speed of 1500-2000 r/min, and fully and uniformly grinding to obtain slurry C;
(4) adding 5 parts of defoaming agent into the slurry C obtained in the step (3), fully mixing, and then placing into an ultrasonic dispersion machine for dispersion for 30-40 minutes to obtain slurry D which is uniformly dispersed and is in a wire-drawing sticky state;
(5) adding the slurry A prepared in the step (1) and the slurry D prepared in the step (4) into a planetary stirrer at the same time, stirring for 20-30 minutes at the rotation speed of the stirrer of 500-800 rpm, and simultaneously adding 3 parts of triethylene tetramine, 3 parts of adhesive and 3 parts of thickening agent to obtain slurry E;
(6) and (4) adding the slurry E prepared in the step (5) into a spraying machine, spraying the slurry E on a base material, and heating and curing to obtain the anti-icing type electric heating hydrophobic coating.
Example 3
An anti-icing type electric heating hydrophobic coating comprises the following raw materials in percentage by mass:
40 parts of epoxy resin, 70 parts of copper-clad silver powder, 8 parts of carbon black, 8 parts of boron nitride powder, 8 parts of carbon nano tube and SiO 2 6 parts of nano particles, 4 parts of triethylene tetramine, 6 parts of defoaming agent (polydimethylsiloxane), 5 parts of dispersing agent (sodium dodecyl sulfate), 4 parts of adhesive (polyvinyl alcohol) and 4 parts of thickening agent (propylene glycol sodium alginate).
A preparation method of an anti-icing type electric heating hydrophobic coating specifically comprises the following steps:
(1) adding 40 parts of epoxy resin, 70 parts of copper-coated silver powder, 8 parts of carbon black and 3 parts of dispersing agent into a planetary stirrer, stirring for 40-50 minutes at the rotating speed of 800-;
(2) adding 8 parts of boron nitride powder into the grinding machine, grinding for 40-60 minutes at the rotation speed of 1200-2000 r/min to obtain slurry B;
(3) continuously adding 8 parts of carbon nano tube and SiO into the mixture obtained in the step (2) 2 Grinding for 30-50 minutes at the rotation speed of 1500-2000 r/min of a grinding machine to obtain slurry C after fully and uniformly grinding, wherein 6 parts of nano particles and 2 parts of a dispersing agent are used for grinding;
(4) adding 6 parts of defoaming agent into the slurry C prepared in the step (3), fully mixing, and then placing into an ultrasonic dispersion machine for dispersion for 30-40 minutes to obtain slurry D which is uniformly dispersed and is in a wire-drawing sticky state;
(5) adding the slurry A prepared in the step (1) and the slurry D prepared in the step (4) into a planetary stirrer at the same time, stirring for 20-30 minutes at the rotation speed of the stirrer of 500-800 rpm, and simultaneously adding 4 parts of triethylene tetramine, 4 parts of adhesive and 4 parts of thickening agent to obtain slurry E;
(6) and (4) adding the slurry E prepared in the step (5) into a spraying machine, spraying the slurry E on a base material, and heating and curing to obtain the anti-icing type electric heating hydrophobic coating.
Example 4
An anti-icing type electric heating hydrophobic coating comprises the following raw materials in percentage by mass:
50 parts of epoxy resin, 80 parts of copper-clad silver powder, 10 parts of carbon black, 10 parts of boron nitride powder, 10 parts of carbon nano tube and SiO 2 8 parts of nano particles, 4 parts of triethylene tetramine, 7 parts of defoaming agent (polydimethylsiloxane), 5 parts of dispersing agent (sodium dodecyl sulfate), 5 parts of adhesive (polyvinyl alcohol) and 5 parts of thickening agent (propylene glycol sodium alginate).
A preparation method of an anti-icing type electric heating hydrophobic coating specifically comprises the following steps:
(1) adding 50 parts of epoxy resin, 80 parts of copper-coated silver powder, 10 parts of carbon black and 3 parts of dispersing agent into a planetary stirrer, stirring for 40-50 minutes at the rotating speed of 800-;
(2) adding 10 parts of boron nitride powder into a grinding machine, grinding for 40-60 minutes at the rotation speed of 1200-2000 r/min to obtain slurry B;
(3) continuously adding 10 parts of carbon nano tube and SiO into the slurry B in the step (2) 2 8 parts of nano particles and 2 parts of dispersing agent, grinding for 30-50 minutes at a grinder rotation speed of 1500-2000 r/min, and fully and uniformly grinding to obtain slurry C;
(4) adding 7 parts of defoaming agent into the slurry C prepared in the step (3), fully mixing, and then putting into an ultrasonic dispersion machine for dispersion for 30-40 minutes to obtain slurry D which is uniformly dispersed and is in a wire-drawing sticky state;
(5) adding the slurry A prepared in the step (1) and the slurry D prepared in the step (4) into a planetary stirrer at the same time, stirring for 20-30 minutes at the rotation speed of the stirrer of 500-800 rpm, and simultaneously adding 4 parts of triethylene tetramine, 5 parts of adhesive and 5 parts of thickening agent to obtain slurry E;
(6) and (4) adding the slurry E prepared in the step (5) into a spraying machine, spraying the slurry E on a base material, and heating and curing to obtain the anti-icing type electric heating hydrophobic coating.
Comparative example 1
The only difference from example 3 is that no copper-clad silver powder is added; the preparation method of the anti-icing type electrothermal hydrophobic coating is the same as that of the example 3.
Comparative example 2
Only differs from example 3 in that no carbon black is added; the preparation method of the anti-icing type electrothermal hydrophobic coating is the same as that of the example 3.
Comparative example 3
Only differs from example 3 in that no boron nitride powder was added; the preparation method of the anti-icing type electrothermal hydrophobic coating is the same as that of the example 3.
Comparative example 4
Only the difference from example 3 is that no carbon nanotubes are added; the preparation method of the anti-icing type electrothermal hydrophobic coating is the same as that of the example 3.
Comparative example 5
The only difference from example 3 is that no SiO addition is made 2 A nanoparticle; the preparation method of the anti-icing type electrothermal hydrophobic coating is the same as that of the example 3.
Comparative example 6
Only differs from example 3 in that copper-clad silver powder and carbon black are not added; the preparation method of the anti-icing type electrothermal hydrophobic coating is the same as that of example 3.
Comparative example 7
Only the difference from example 3 is that copper-clad silver powder and boron nitride powder are not added; the preparation method of the anti-icing type electrothermal hydrophobic coating is the same as that of the example 3.
Comparative example 8
Only the difference from example 3 is that copper-clad silver powder and carbon nanotubes are not added; the preparation method of the anti-icing type electrothermal hydrophobic coating is the same as that of the example 3.
Comparative example 9
The difference from example 3 is only that no copper-clad silver powder is addedAnd SiO 2 A nanoparticle; the preparation method of the anti-icing type electrothermal hydrophobic coating is the same as that of the example 3.
Comparative example 10
Only differs from example 3 in that no carbon black and boron nitride powder are added; the preparation method of the anti-icing type electrothermal hydrophobic coating is the same as that of the example 3.
Comparative example 11
Only the difference from example 3 is that no carbon black and carbon nanotubes are added; the preparation method of the anti-icing type electrothermal hydrophobic coating is the same as that of the example 3.
Comparative example 12
The only difference from example 3 is that no carbon black and no SiO were added 2 A nanoparticle; the preparation method of the anti-icing type electrothermal hydrophobic coating is the same as that of the example 3.
Comparative example 13
Only the difference from example 3 is that boron nitride powder and carbon nanotubes are not added; the preparation method of the anti-icing type electrothermal hydrophobic coating is the same as that of the example 3.
Comparative example 14
The only difference from example 3 is that no boron nitride powder and no SiO were added 2 A nanoparticle; the preparation method of the anti-icing type electrothermal hydrophobic coating is the same as that of the example 3.
Comparative example 15
The only difference from example 3 is that no carbon nanotubes and no SiO were added 2 A nanoparticle; the preparation method of the anti-icing type electrothermal hydrophobic coating is the same as that of the example 3.
Comparative example 16
Only differs from example 3 in that no copper-clad silver powder, carbon black and boron nitride powder were added; the preparation method of the anti-icing type electrothermal hydrophobic coating is the same as that of the example 3.
Comparative example 17
The only difference from example 3 is that copper-clad silver powder, carbon black and carbon nanotubes are not added; the preparation method of the anti-icing type electrothermal hydrophobic coating is the same as that of the example 3.
Comparative example 18
Differences from example 3Only in that copper-clad silver powder, carbon black and SiO are not added 2 A nanoparticle; the preparation method of the anti-icing type electrothermal hydrophobic coating is the same as that of the example 3.
Comparative example 19
Only the difference from example 3 is that copper-clad silver powder, boron nitride powder and carbon nanotubes are not added; the preparation method of the anti-icing type electrothermal hydrophobic coating is the same as that of example 3.
Comparative example 20
The only difference from example 3 is that no copper-clad silver powder, no boron nitride powder and no SiO were added 2 A nanoparticle; the preparation method of the anti-icing type electrothermal hydrophobic coating is the same as that of the example 3.
Comparative example 21
The only difference from example 3 is that copper-clad silver powder, carbon nanotubes and SiO were not added 2 A nanoparticle; the preparation method of the anti-icing type electrothermal hydrophobic coating is the same as that of the example 3.
Comparative example 22
Only the difference from example 3 is that no carbon black, boron nitride powder and carbon nanotubes are added; the preparation method of the anti-icing type electrothermal hydrophobic coating is the same as that of the example 3.
Comparative example 23
The only difference from example 3 is that no carbon black, boron nitride powder and SiO were added 2 A nanoparticle; the preparation method of the anti-icing type electrothermal hydrophobic coating is the same as that of the example 3.
Comparative example 24
The only difference from example 3 is that no carbon black, carbon nanotubes and SiO were added 2 A nanoparticle; the preparation method of the anti-icing type electrothermal hydrophobic coating is the same as that of the example 3.
Comparative example 25
The only difference from example 3 is that no boron nitride powder, carbon nanotubes and SiO were added 2 A nanoparticle; the preparation method of the anti-icing type electrothermal hydrophobic coating is the same as that of the example 3.
Comparative example 26
Only the difference from example 3 is that copper-clad silver powder, carbon black, boron nitride powder and carbon nanotubes are not added; the preparation method of the anti-icing type electrothermal hydrophobic coating is the same as that of the example 3.
Comparative example 27
The only difference from example 3 is that no copper-clad silver powder, carbon black, boron nitride powder and SiO were added 2 A nanoparticle; the preparation method of the anti-icing type electrothermal hydrophobic coating is the same as that of the example 3.
Comparative example 28
The only difference from example 3 is that no carbon black, boron nitride powder, carbon nanotubes and SiO were added 2 A nanoparticle; the preparation method of the anti-icing type electrothermal hydrophobic coating is the same as that of the example 3.
Comparative example 29
The only difference from example 3 is that copper-clad silver powder, boron nitride powder, carbon nanotube and SiO were not added 2 A nanoparticle; the preparation method of the anti-icing type electrothermal hydrophobic coating is the same as that of the example 3.
Comparative example 30
The only difference from example 3 is that copper-coated silver powder, carbon black, carbon nanotubes and SiO were not added 2 A nanoparticle; the preparation method of the anti-icing type electrothermal hydrophobic coating is the same as that of the example 3.
Comparative example 31
The only difference from example 3 is that copper-clad silver powder, carbon black, boron nitride powder, carbon nanotube and SiO were not added 2 A nanoparticle; the preparation method of the anti-icing type electrothermal hydrophobic coating is the same as that of the example 3.
Comparative example 32 (determination of copper-clad silver powder composition)
An anti-icing type electric heating hydrophobic coating comprises the following raw materials in percentage by mass:
40 parts of epoxy resin, 40 parts of copper-coated silver powder, 50 parts of copper-coated silver powder, 60 parts of copper-coated silver powder, 70 parts of copper-coated silver powder, 80 parts of copper-coated silver powder, 90 parts of copper-coated silver powder, 8 parts of carbon black, 8 parts of boron nitride powder, 8 parts of carbon nano tube and 8 parts of SiO 2 6 parts of nano particles, 4 parts of triethylene tetramine, 6 parts of a defoaming agent (polydimethylsiloxane), 5 parts of a dispersing agent (sodium dodecyl sulfate), 4 parts of a binding agent (polyvinyl alcohol) and 4 parts of a thickening agent (propylene glycol sodium alginate).
A preparation method of an anti-icing type electric heating hydrophobic coating specifically comprises the following steps:
(1) adding 40 parts of epoxy resin, 40 parts of copper-coated silver powder, 50 parts of copper-coated silver powder, 60 parts of copper-coated silver powder, 70 parts of copper-coated silver powder, 90 parts of carbon black and 3 parts of dispersing agent into a planetary stirrer respectively, stirring for 40-50 minutes at a rotating speed of the stirrer of 800 plus 1200 revolutions per minute, and fully and uniformly mixing the raw materials to obtain slurry A;
(2) adding 8 parts of boron nitride powder into the grinding machine, grinding for 40-60 minutes at the rotation speed of 1200-2000 r/min to obtain slurry B;
(3) continuously adding 8 parts of carbon nano tube and SiO into the solution obtained in the step (2) 2 Grinding for 30-50 minutes at the rotation speed of 1500-2000 r/min of a grinding machine to obtain slurry C after fully and uniformly grinding, wherein 6 parts of nano particles and 2 parts of a dispersing agent are used for grinding;
(4) adding 6 parts of defoaming agent into the slurry C prepared in the step (3), fully mixing, and then placing into an ultrasonic dispersion machine for dispersion for 30-40 minutes to obtain slurry D which is uniformly dispersed and is in a wire-drawing sticky state;
(5) adding the slurry A prepared in the step (1) and the slurry D prepared in the step (4) into a planetary stirrer at the same time, stirring for 20-30 minutes at the rotation speed of the stirrer of 500-800 rpm, and simultaneously adding 4 parts of triethylene tetramine, 4 parts of adhesive and 4 parts of thickening agent to obtain slurry E;
(6) and (4) adding the slurry E prepared in the step (5) into a spraying machine, spraying the slurry E on a base material, and heating and curing to obtain the anti-icing type electric heating hydrophobic coating.
Comparative example 33 (replacement of triethylene tetramine by diethylenetriamine)
An anti-icing type electric heating hydrophobic coating comprises the following raw materials in percentage by mass:
40 parts of epoxy resin, 70 parts of copper-clad silver powder, 8 parts of carbon black, 8 parts of boron nitride powder, 8 parts of carbon nano tube and SiO 2 6 parts of nano particles, 4 parts of diethylenetriamine, 6 parts of defoaming agent (polydimethylsiloxane), 5 parts of dispersing agent (sodium dodecyl sulfate), 4 parts of adhesive (polyvinyl alcohol) and 4 parts of thickening agent (propylene glycol sodium alginate).
A preparation method of an anti-icing type electric heating hydrophobic coating specifically comprises the following steps:
(1) adding 40 parts of epoxy resin, 70 parts of copper-coated silver powder, 8 parts of carbon black and 3 parts of dispersing agent into a planetary stirrer, stirring for 40-50 minutes at the rotation speed of the stirrer of 800-1200 revolutions per minute, and fully and uniformly mixing the raw materials to obtain slurry A;
(2) adding 8 parts of boron nitride powder into the grinding machine, grinding for 40-60 minutes at the rotation speed of 1200-2000 r/min to obtain slurry B;
(3) continuously adding 8 parts of carbon nano tube and SiO into the mixture obtained in the step (2) 2 Grinding for 30-50 minutes at the rotation speed of 1500-2000 r/min of a grinding machine to obtain slurry C after fully and uniformly grinding, wherein 6 parts of nano particles and 2 parts of a dispersing agent are used for grinding;
(4) adding 6 parts of defoaming agent into the slurry C prepared in the step (3), fully mixing, and then placing into an ultrasonic dispersion machine for dispersion for 30-40 minutes to obtain slurry D which is uniformly dispersed and is in a wire-drawing sticky state;
(5) adding the slurry A prepared in the step (1) and the slurry D prepared in the step (4) into a planetary stirrer at the same time, stirring for 20-30 minutes at a rotating speed of 500-;
(6) and (4) adding the slurry E prepared in the step (5) into a spraying machine, spraying the slurry E on a base material, and heating and curing to obtain the anti-icing type electric heating hydrophobic coating.
Comparative example 34 (adjustment of the ratio of carbon black to carbon nanotube)
An anti-icing type electric heating hydrophobic coating comprises the following raw materials in percentage by mass:
40 parts of epoxy resin, 70 parts of copper-clad silver powder, 12 parts of carbon black, 8 parts of boron nitride powder, 4 parts of carbon nano tube and SiO 2 6 parts of nano particles, 4 parts of triethylene tetramine, 6 parts of a defoaming agent (polydimethylsiloxane), 5 parts of a dispersing agent (sodium dodecyl sulfate), 4 parts of a binding agent (polyvinyl alcohol) and 4 parts of a thickening agent (propylene glycol sodium alginate).
A preparation method of an anti-icing type electric heating hydrophobic coating specifically comprises the following steps:
(1) adding 40 parts of epoxy resin, 70 parts of copper-coated silver powder, 12 parts of carbon black and 3 parts of dispersing agent into a planetary stirrer, stirring for 40-50 minutes at the rotating speed of 800 plus 1200 revolutions per minute of the stirrer, and fully and uniformly mixing the raw materials to obtain slurry A
(2) Adding 8 parts of boron nitride powder into a grinding machine, grinding for 40-60 minutes at the rotation speed of 1200-2000 rpm of the grinding machine to obtain slurry B;
(3) continuously adding 4 parts of carbon nano tube and SiO into the mixture obtained in the step (2) 2 Grinding for 30-50 minutes at the rotation speed of 1500-2000 r/min of a grinding machine to obtain slurry C after fully and uniformly grinding, wherein 6 parts of nano particles and 2 parts of a dispersing agent are used for grinding;
(4) adding 6 parts of defoaming agent into the slurry C prepared in the step (3), fully mixing, and then placing into an ultrasonic dispersion machine for dispersion for 30-40 minutes to obtain slurry D which is uniformly dispersed and is in a wire-drawing sticky state;
(5) adding the slurry A prepared in the step (1) and the slurry D prepared in the step (4) into a planetary stirrer at the same time, stirring for 20-30 minutes at the rotation speed of the stirrer of 500-800 rpm, and simultaneously adding 4 parts of triethylene tetramine, 4 parts of adhesive and 4 parts of thickening agent to obtain slurry E;
(6) and (4) adding the slurry E prepared in the step (5) into a spraying machine, spraying the slurry E on a base material, and heating and curing to obtain the anti-icing type electric heating hydrophobic coating.
And (3) testing results:
43(4 examples and 34 comparative examples, wherein 6 coatings are contained in 32) composite coatings with completely consistent shapes, sizes and thicknesses prepared in the examples 1-4 and the comparative examples 1-34 are subjected to performance tests: wherein, FIG. 1 is a sample diagram of the anti-icing type electric heating hydrophobic coating prepared in the embodiments 1-4 and a structural schematic diagram of the coating.
The test method comprises the following steps:
1. the conductive performance test was performed on 43 composite coatings (6 coatings in comparative example 32), the resistivity of the sample was measured by a four-corner probe resistivity tester, and the formula k ρ ═ ρ -1 To obtain corresponding conductivity to characterize the conductivity of the sample, wherein the results of the detailed data of 38 blocks are shown in table 1.
2. The heat transfer performance of the coating is shown by carrying out surface heat transfer performance test on 38 composite coatings (4 examples and 34 comparative examples, wherein one coating is taken in the comparative example 32), applying a constant current of 1A to two ends of the coating, and testing a surface temperature distribution graph of the coating surface at the same time and the same current by using an infrared thermal imager, wherein the detailed results are shown in Table 1; wherein FIG. 3 is a thermal image of the anti-icing type electrothermal hydrophobic coating prepared in example 3; fig. 4 is an SEM image of an electric heating layer of the anti-icing type electric heating hydrophobic coating prepared in example 3.
3. The test adopts a circling method used in a paint film inspection standard for evaluation, the evaluation is carried out according to the integrity degree of the paint film in the scratch range of the thread line, the evaluation is expressed by grades and can be divided into 0, 1, 2, 3, 4, 5, 6 and 7, and the larger the grade, the worse the adhesive force of the coating is.
The 38 samples of the composite coating were placed on a test bed, pressed tightly with a press plate, weighted to bring the needle point into contact with the paint film, the hand wheel was shaken uniformly clockwise, the samples were then taken out, the paint chips on the scratches were removed with a paint brush, the scratches were observed under a magnifying glass and rated, and the detailed results are shown in table 1.
And fourthly, putting the 38 pieces of composite coating samples into a contact angle tester, and testing the contact angle of the treated composite coating by dripping water drops. The data are measured for multiple times at different positions of the same composite coating and then averaged, the values are compared, the larger the contact angle is, the better the hydrophobicity is, and the detailed results are shown in table 1; wherein FIG. 2 is a contact angle diagram of the anti-icing type electrothermal hydrophobic coating prepared in example 3; fig. 5 is an SEM image of the super-hydrophobic layer of the anti-icing type electrothermal hydrophobic coating prepared in example 3.
TABLE 1
Figure BDA0003741943620000131
Figure BDA0003741943620000141
In the comparative example 1, no copper-clad silver powder is added, so that the conductivity is poor, the heating efficiency is poor, the heat transfer effect is good, the adhesive force is good, and the hydrophobic property is good.
The comparative example 2 has no carbon black, and has good conductivity, good heating efficiency, good heat transfer effect, good adhesive force and good hydrophobic property.
Comparative example 3, in which no boron nitride powder was added, had good conductivity, general heating efficiency, good heat transfer effect, general adhesion, and good hydrophobic property.
Comparative example 4 has no carbon nanotube added, and has good conductivity, general heating efficiency, good heat transfer effect, good adhesion, and good hydrophobic property.
Comparative example 5 No SiO addition 2 The nano particles have the advantages of good conductivity, good heating efficiency, good heat transfer effect, good adhesive force and poor hydrophobic property.
Comparative example 6 does not add copper-clad silver powder and carbon black, and has general electric conductivity, general heating efficiency, good heat transfer effect, general adhesive force and good hydrophobic property.
Comparative example 7 does not add copper-clad silver powder and boron nitride powder, and has a general electric conductivity, a general heating efficiency, a general heat transfer effect, a general adhesive force and a good hydrophobic property.
In the comparative example 8, copper-clad silver powder and carbon nanotubes are not added, so that the conductivity is general, the heating efficiency is general, the heat transfer effect is general, the adhesive force is good, and the hydrophobic property is good.
Comparative example 9 No copper-clad silver powder and SiO 2 The nano particles have the advantages of common conductivity, heat generation efficiency, heat transfer effect, adhesive force and poor hydrophobic property.
Comparative example 10, in which carbon black and boron nitride powder were not added, had good conductivity, good heat generation efficiency, poor heat transfer effect, general adhesion, and good hydrophobic property.
In the comparative example 11, carbon black and carbon nanotubes are not added, so that the conductivity is general, the heating efficiency is general, the heat transfer effect is poor, the adhesive force is general, and the hydrophobic property is good.
Comparative example 12 No addition of carbon Black and SiO 2 The nano particles have the advantages of common conductivity, common heating efficiency, common adhesive force and poor hydrophobic property.
In comparative example 13, boron nitride powder and carbon nanotubes were not added, resulting in poor conductivity, general heat generation efficiency, poor heat transfer effect, general adhesion, and good hydrophobic property.
Comparative example 14 in which boron nitride powder and SiO were not added 2 The nano particles have poor conductivity, general heating efficiency, poor heat transfer effect, general adhesive force and good hydrophobic property.
Comparative example 15 No carbon nanotube and SiO 2 The nano particles have poor conductivity, general heating efficiency, poor heat transfer effect, general adhesive force and poor hydrophobic property.
Comparative example 16, in which copper-clad silver powder, carbon black and boron nitride powder were not added, had poor conductivity, poor heating efficiency, poor heat transfer effect, poor adhesion and good hydrophobicity.
Comparative example 17, in which copper-clad silver powder, carbon black and carbon nanotubes were not added, had poor conductivity, poor heating efficiency, general heat transfer effect, poor adhesion, and good hydrophobicity.
Comparative example 18 No copper-clad silver powder, carbon black and SiO 2 The nano particles have poor conductivity, poor heating efficiency, general heat transfer effect, poor adhesive force and poor hydrophobic property.
Comparative example 19, in which copper-clad silver powder, boron nitride powder, and carbon nanotubes were not added, had poor conductivity, poor heat generation efficiency, general heat transfer effect, poor adhesion, and good hydrophobicity.
Comparative example 20 No copper-clad silver powder, boron nitride powder and SiO 2 The nano particles have poor conductivity, poor heating efficiency, general heat transfer effect, poor adhesive force and poor hydrophobic property.
Comparative example 21 without adding copper-clad silver powder, carbon nanotube and SiO 2 The nano particles have poor conductivity, poor heating efficiency, general heat transfer effect, poor adhesive force and poor hydrophobic property.
Comparative example 22, in which carbon black, boron nitride powder and carbon nanotubes were not added, had good conductivity, poor heat generation efficiency, poor heat transfer effect, general adhesion, and good hydrophobicity.
Comparative example 23 No carbon Black, boron nitride powder and SiO 2 Nanoparticles, electrically conductiveBetter rate, poor heating efficiency, poor heat transfer effect, general adhesive force and poor hydrophobic property.
Comparative example 24 in which carbon black, carbon nanotube and SiO were not added 2 The nano particles have the advantages of good conductivity, poor heating efficiency, general heat transfer effect, general adhesive force and poor hydrophobic property.
Comparative example 25 in which boron nitride powder, carbon nanotube and SiO were not added 2 The nano particles have the advantages of good conductivity, poor heating efficiency, general heat transfer effect, general adhesive force and poor hydrophobic property.
Comparative example 26, in which copper-clad silver powder, carbon black, boron nitride powder, and carbon nanotubes were not added, had poor conductivity, poor heat generation efficiency, poor heat transfer effect, poor adhesion, and good hydrophobicity.
Comparative example 27 No addition of copper-clad silver powder, carbon black, boron nitride powder and SiO 2 The nano particles have poor conductivity, poor heating efficiency, poor heat transfer effect, poor adhesive force and poor hydrophobic property.
Comparative example 28 No carbon Black, boron nitride powder, carbon nanotube and SiO 2 The nano particles have the advantages of good conductivity, poor heating efficiency, poor heat transfer effect, general adhesive force and poor hydrophobic property.
Comparative example 29 No copper-clad silver powder, boron nitride powder, carbon nanotube and SiO 2 The nano particles have poor conductivity, poor heating efficiency, poor heat transfer effect, poor adhesive force and poor hydrophobic property.
Comparative example 30 No addition of copper-clad silver powder, carbon black, carbon nanotube and SiO 2 The nano particles have poor conductivity, poor heating efficiency, poor heat transfer effect, poor adhesive force and poor hydrophobic property.
Comparative example 31 was conducted without adding copper-clad silver powder, carbon black, boron nitride powder, carbon nanotube and SiO 2 The nano particles have poor conductivity, poor heating efficiency, poor heat transfer effect, poor adhesive force and poor hydrophobic property.
Comparative example 32 the data in table 1 is that the coating prepared when 40 parts of copper-clad silver powder is added has poor conductivity, poor heating efficiency and poor heat transfer effect;
in order to determine the appropriate addition amount of the copper-clad silver powder, the conductivity and the resistivity of the anti-icing type electrothermal hydrophobic coating respectively prepared from the copper-clad silver powder with different components in the comparative example 32 were tested, and the test results are shown in fig. 6:
from fig. 6, it can be seen that the conductivity increases with the increase of the content of copper-clad silver powder, and when reaching a certain peak value, the conductivity decreases; when the adding amount of the copper-clad silver powder is 70 parts, the resistivity of the prepared coating is the minimum, and the electrical conductivity is the best; this is because when the content of copper-clad silver powder in the system is too large, part of the copper-clad silver powder is not bonded with the epoxy resin but is dissociated outside the whole system, so that the impedance of the whole conductive system is increased, and the conductivity is also reduced.
Comparative example 33 differs from example 3 only in that triethylene tetramine is replaced with diethylene triamine, and the prepared coating layer has better hydrophobic property, but the conductivity, heat generation efficiency and adhesion are significantly reduced compared to example 3.
In comparative example 34, 12 parts of carbon black and 4 parts of carbon nanotubes were added, and the hydrophobic property was extremely poor. The added carbon black and the carbon nano tubes not only have the effect of heat conduction and heat transfer, but also have certain influence on the structure of the micro-nano structure on the surface of the coating.
Comparative example 34 a coating was prepared by adjusting the ratio of carbon black to carbon nanotubes; and as shown in the attached figure 7, the scanning electron microscope observation of the coating surface shows that after the components of the carbon black and the carbon nano tube are adjusted, the micro-nano structure on the surface of the super-hydrophobic coating is damaged and covered, and the result is shown in table 1 by measuring the contact angle: when the carbon black in the coating is adjusted to be 12 parts and the carbon nano tube is adjusted to be 4 parts, the contact angle of the prepared coating can only reach 72.6 degrees, compared with the coatings prepared in the embodiments 1-4, the contact angle is greatly reduced, and the hydrophobic effect is extremely poor; the analysis reason is that a large amount of carbon black or carbon nano tubes can wrap the micro-nano structure formed on the surface of the coating by the SiO2 nano particles, and the structure of the micro-nano structure is damaged, so that the contact angle of the surface of the coating is suddenly reduced.
The above results show that: the anti-icing type electric heating hydrophobic coating prepared by the invention, especially the coating prepared in the embodiment 3, has better conductivity, heat transfer effect and hydrophobic property, and plays a good role in preventing the icing/icing of outdoor base materials.
The embodiments described herein are merely illustrative of the spirit and some of the experiments performed. Various modifications or additions may be made to the described embodiments, or alternatives may be employed, by those skilled in the art, without departing from the spirit or scope of the invention as defined in the appended claims.

Claims (10)

1. An anti-icing type electricity hydrophobic coating that generates heat which characterized in that: the coating comprises the following raw materials in parts by weight: 20-50 parts of epoxy resin, 50-80 parts of copper-clad silver powder, 4-10 parts of carbon black, 4-10 parts of boron nitride powder, 4-10 parts of carbon nano tube and SiO 2 2-8 parts of nano particles, 3-4 parts of triethylene tetramine, 4-7 parts of a defoaming agent, 4-5 parts of a dispersing agent, 3-5 parts of an adhesive and 2-5 parts of a thickening agent.
2. The anti-icing type electrothermal hydrophobic coating of claim 1, wherein: the epoxy resin comprises one or more of bisphenol A epoxy resin, bisphenol F epoxy resin, polyphenol glycidyl ether epoxy resin, aliphatic glycidyl ether epoxy resin and glycidyl ester epoxy resin.
3. The anti-icing type electrothermal hydrophobic coating of claim 1, wherein: the dispersing agent comprises one or more of triethyl hexyl phosphoric acid, sodium dodecyl sulfate, sodium tripolyphosphate and polyacrylamide.
4. The anti-icing type electrothermal hydrophobic coating of claim 1, wherein: the defoaming agent comprises one or more of polydimethylsiloxane, isopropanol and fatty acid amide.
5. The anti-icing type electrothermal hydrophobic coating of claim 1, wherein: the thickening agent comprises one or more of myristyl alcohol, propylene glycol sodium alginate, polyurethane and diallyl phthalate.
6. The anti-icing type electrothermal hydrophobic coating of claim 1, wherein: the adhesive comprises one or more of polyvinyl alcohol, polystyrene and polyacrylate.
7. The anti-icing type electrothermal hydrophobic coating according to any one of claims 1 to 6, wherein: the coating comprises the following raw materials in parts by weight: 40 parts of epoxy resin, 70 parts of copper-clad silver powder, 8 parts of carbon black, 8 parts of boron nitride powder, 8 parts of carbon nano tube and SiO 2 6 parts of nano particles, 4 parts of triethylene tetramine, 6 parts of defoaming agent, 5 parts of dispersing agent, 5 parts of adhesive and 4 parts of thickening agent.
8. The preparation method of the anti-icing type electrothermal hydrophobic coating according to any one of claims 1 to 7, characterized by comprising the following steps: the method comprises the following steps:
(1) adding epoxy resin, copper-coated silver powder, carbon black and a dispersing agent into a planetary stirrer, and uniformly stirring and mixing to obtain slurry A;
(2) adding boron nitride powder into the grinding machine, and grinding to obtain slurry B;
(3) continuously adding the carbon nano tube and SiO into the slurry B prepared in the step (2) 2 Fully and uniformly grinding the nano particles and the dispersing agent to obtain slurry C;
(4) adding a defoaming agent into the slurry C prepared in the step (3), fully mixing, and then putting into an ultrasonic dispersion machine for ultrasonic dispersion to obtain a slurry D in a wire-drawing viscous state;
(5) adding the slurry A prepared in the step (1) and the slurry D prepared in the step (4) into a planetary stirrer at the same time, continuously stirring, and then adding triethylene tetramine, an adhesive and a thickening agent to obtain slurry E;
(6) and (4) adding the slurry E prepared in the step (5) into a spraying machine, spraying the slurry E on a base material, and heating and curing to obtain the anti-icing type electric heating hydrophobic coating.
9. The method for preparing the anti-icing type electrothermal hydrophobic coating according to claim 8, wherein the method comprises the following steps: the temperature of the heating and curing in the step (6) is 100-150 ℃.
10. Use of an anti-icing type electrothermal hydrophobic coating according to any one of claims 1 to 7 for anti-icing/anti-icing of outdoor substrates.
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CN115612378A (en) * 2022-10-21 2023-01-17 东北林业大学 Preparation method of environment-friendly durable photothermal promotion anti-icing coating of wood-based material

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CN111073574A (en) * 2019-12-04 2020-04-28 北京氦舶科技有限责任公司 Single-component normal-temperature curing conductive adhesive and preparation method thereof
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