CN108997888B - Preparation method of super-hydrophobic anti-drag coating - Google Patents
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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Abstract
The invention relates to a preparation method of a super-hydrophobic anti-drag coating, which is characterized in that the super-hydrophobic anti-drag coating is prepared on the surface of a substrate by alternately spraying an epoxy matrix and hydrophobic particles, and has excellent super-hydrophobic performance, the static water contact angle reaches more than 150 degrees, and the rolling angle is less than 10 degrees. The coating is prepared on a rheometer rotor for resistance reduction performance test, and the resistance reduction rate can reach over 25 percent. The super-hydrophobic coating has good super-hydrophobic performance and can be used for drag reduction and speed acceleration of an offshore aircraft; the preparation method is simple, the preparation period is short, the coating can be coated on any substrate to keep the super-hydrophobic performance, and the coating has better cohesiveness; the super-hydrophobic coating has better wear resistance, and can still maintain the super-hydrophobic performance after being repeatedly polished by abrasive paper.
Description
Technical Field
The invention belongs to the technical field of organic composite coating materials, and relates to a preparation method of a super-hydrophobic anti-drag coating.
Background
With the continuous promotion of global integration, the communication and cooperation in the fields of economy, culture, military and the like among countries are increasingly tight, the marine transportation gradually becomes the main mode of the transportation of the big countries, the countries begin to enhance the development and utilization of water resources, the energy consumption is serious, the reserves are reduced increasingly, and meanwhile, the development of new energy is difficult, so how to effectively utilize the existing energy and reduce the energy consumption becomes very important.
When large-scale water vehicles such as cargo ships, aircraft carriers, research ships and the like and underwater vehicles such as submarines, torpedoes and the like are sailed in the ocean, the sailing speed and the energy consumption rate are important parameters for evaluating the performance of the large-scale water vehicles, and the operation speed and the energy consumption are mainly determined by the resistance except for the influence of the performance of a ship engine. The friction resistance of the ship is reduced, and the ship has very important significance for improving the navigation speed of the ship, strengthening the fighting capacity of the ship and reducing energy consumption.
The reduction of the frictional resistance between the ship body and the water flow can save fuel and energy firstly, and can increase the navigation speed secondly, thereby having important significance in the military field. In addition, the energy consumption generated in the sailing process is accompanied by corresponding noise and vibration, and the application of the anti-drag material can also bring a positive effect on vibration and noise reduction. Currently, underwater vehicles are influenced by bionics in recent years, and people begin to prefer a bionic design thinking in aspects of appearance design and material application of various traffic carriers. Scientists in the area of underwater vehicle drag reduction have focused their research primarily on superhydrophobic drag reduction.
The super-hydrophobic surface drag reduction technology is derived from the research on the self-cleaning function of the lotus leaf surface. A biologist and a material scientist observe and research the surface microstructures of plant leaves such as lotus leaves, taro leaves and the like, and find that the micron-sized convex structures on the surfaces of the plant leaves and the taro leaves and the nano-sized waxy villi generate a synergistic effect to form uneven papilla or microcolumns and the like with extremely large surface coarse-grained structures, and the papilla surface structures are not smooth and are covered by long-chain hydrophobic alkane structures to form waxy surfaces. According to the observation structure of a scanning electron microscope, on the surfaces of the leaves with the multilevel structure, water drops drop to the tops of the convex microstructures, most of the water drops are in contact with air, only a small part of the solid surface of the leaf is in contact with the water drops, under the condition, the small solid-liquid contact surface causes insufficient adhesion, the water drops are difficult to stay on the surface, and therefore rolling occurs, and because the water molecules belong to strong polar molecules, pollutant particles on the surfaces of the lotus leaves can be taken away in the rolling process to achieve the self-cleaning effect. People prepare various hydrophobic/super-hydrophobic materials by simulating the lotus leaf surface, and apply the hydrophobic/super-hydrophobic materials to the surface drag reduction field, thereby forming a new drag reduction method for drag reduction by simulating a hydrophobic/super-hydrophobic water meter. In 1999, Watanabe et al prepared a fluoroalkane (Fluid Mech,1999,38(1),225) from modified acrylic acid, applied it as a hydrophobic material to the wall of a pipe and studied its drag reduction effect, and experimentally found that the surface drag reduction of the pipe wall in laminar flow was 14%. The subject group also carried out the work of preparing superhydrophobic coatings. Zhang Qiongyu et al designed a fluorosilicone resin to prepare a super-hydrophobic/amphiphobic coating (CN 2017107386707) by utilizing a mercapto-alkene click chemistry method, and obtained a better self-cleaning effect when applied to fabrics, but did not research on the aspect of super-hydrophobic drag reduction on a planar substrate.
Disclosure of Invention
Technical problem to be solved
In order to avoid the defects of the prior art, the invention provides a preparation method of a super-hydrophobic anti-drag coating, which is a preparation method of a super-hydrophobic anti-drag coating based on a composite coating technology and mainly applies the composite coating technology to realize the super-hydrophobic anti-drag performance on a substrate.
Technical scheme
A preparation method of a super-hydrophobic drag reduction coating is characterized by comprising the following steps:
step 1, preparation of epoxy prepolymer: under the protection of nitrogen, sequentially adding a multifunctional thiol compound, an alkenyl epoxy mixture, a solvent A and an alkali catalyst into a reactor, carrying out a mercapto-alkene addition reaction at normal temperature, and obtaining an epoxy prepolymer after 6-10 hours; the mass ratio of the multifunctional thiol compound to the alkenyl epoxy mixture, the solvent A and the base catalyst is 1: 1-5: 0.01-0.05; in the mixture of the multifunctional thiol compound and the alkenyl epoxy, the multifunctional thiol compound and the alkenyl epoxy are mixed according to the molar ratio of 1:1 of sulfydryl to epoxy group;
the alkenyl epoxy is glycidyl methacrylate;
step 2, preparation of a resin matrix: mixing the epoxy prepolymer and the amino curing agent according to the mass ratio of 100: 20-50, and stirring to obtain a resin matrix;
step 3, preparing the super-hydrophobic drag reduction coating: spraying the resin matrix and the hydrophobic particle suspension liquid at intervals in a layered manner for 6-10 times, and placing the resin matrix and the hydrophobic particle suspension liquid in a blast oven at the temperature of 100-180 ℃ for curing for 2-6 h to obtain a super-hydrophobic anti-drag coating;
when spraying, the first layer on the substrate is a resin matrix, and the last layer is a hydrophobic particle suspension; after the resin matrix or the hydrophobic particle suspension is sprayed, the next layer is sprayed after the solvent is completely volatilized;
the hydrophobic particle suspension is as follows: mixing hydrophobic particles and a solvent B according to a mass ratio of 1: 10-20, and mixing to obtain the hydrophobic particle suspension.
The solvent A is acetone, tetrahydrofuran, N-methyl pyrrolidone or N, N-dimethyl acetamide.
The multifunctional thiol compound is glycerol trimercapto propionate, trimethylolpropane trimercapto propyl ester, isocyanuric acid trimercapto carboxylate, pentaerythritol tetramercaptopropionate or dipentaerythritol hexamercapto propionate.
The alkali catalyst is dimethyl phenyl phosphine, tributyl phosphine or a diethylenetriamine basic compound.
The amino curing agent is one or a combination of more of 4,4' -dithiodiphenylamine, dicyandiamide, modified dicyandiamide, urea derivatives and imidazole derivatives.
The hydrophobic particles are fluorinated silica with the particle size of 100-2000 nm, polytetrafluoroethylene micro powder and polyvinylidene fluoride micro powder.
The solvent B is absolute ethyl alcohol, acetone, tetrahydrofuran or N, N-dimethylacetamide.
Advantageous effects
The invention provides a preparation method of a super-hydrophobic anti-drag coating, which prepares the super-hydrophobic anti-drag coating on the surface of a substrate by alternately spraying an epoxy matrix and hydrophobic particles, and has excellent super-hydrophobic performance, a static water contact angle of more than 150 degrees and a rolling angle of less than 10 degrees. The coating is prepared on a rheometer rotor for resistance reduction performance test, and the resistance reduction rate can reach over 25 percent.
The invention has the advantages that:
1. the super-hydrophobic coating has good super-hydrophobic performance and can be used for drag reduction and speed acceleration of an offshore aircraft;
2. the super-hydrophobic coating has the advantages of simple preparation method and short preparation period, can be coated on any substrate to keep super-hydrophobic performance, and has better cohesiveness;
3. the super-hydrophobic coating has better wear resistance, and can still maintain the super-hydrophobic performance after being repeatedly polished by abrasive paper.
Drawings
FIG. 1: an electron microscope photograph of the surface microstructure of the super-hydrophobic anti-drag coating;
FIG. 2: and the contact angle of the super-hydrophobic drag reduction coating after friction.
Detailed Description
The invention will now be further described with reference to the following examples and drawings:
the invention relates to a preparation method of a super-hydrophobic drag reduction coating, which comprises the steps of preparing an epoxy prepolymer, preparing a resin matrix and preparing the super-hydrophobic drag reduction coating, and is characterized in that: the preparation method of the epoxy prepolymer comprises the following steps: under the protection of nitrogen, sequentially adding a solvent A, a multifunctional thiol compound, alkenyl epoxy and an alkali catalyst into a reactor to perform a mercapto-alkene addition reaction at normal temperature for 6-10 hours to obtain an epoxy prepolymer, wherein the multifunctional thiol compound and the alkenyl epoxy are mixed according to the molar ratio of mercapto to epoxy groups of 1:1, and the mass ratio of the multifunctional thiol compound to the alkenyl epoxy mixture, the organic solvent and the alkali catalyst is 1: 1-5: 0.01-0.05; the preparation method of the resin matrix comprises the following steps: mixing the epoxy prepolymer and the amino curing agent according to the mass ratio of 100: 20-50, and uniformly stirring to obtain a resin matrix; the preparation method of the super-hydrophobic drag reduction coating comprises the following steps: uniformly spraying a resin matrix on a substrate, spraying a hydrophobic particle suspension once after the solvent is completely volatilized, spraying a layer of resin matrix after the solvent of the suspension is completely volatilized, repeatedly spraying the resin matrix and the hydrophobic particle suspension for 6 to 10 times in this way, and placing the resin matrix and the hydrophobic particle suspension in a blowing oven at 100 to 180 ℃ for curing for 2 to 6 hours to obtain the super-hydrophobic anti-drag coating.
The preparation method of the super-hydrophobic drag reduction coating is characterized by comprising the following steps: the solvent A is acetone, tetrahydrofuran, N, N-methyl pyrrolidone and N, N-dimethylacetamide;
the preparation method of the super-hydrophobic drag reduction coating is characterized by comprising the following steps: the multifunctional thiol compound is glycerol trimercapto propionate, trimethylolpropane trimercapto propyl ester, isocyanuric acid trimercapto carboxylate, pentaerythritol tetramercaptopropionate, and dipentaerythritol hexamercapto propionate.
The preparation method of the super-hydrophobic drag reduction coating is characterized by comprising the following steps: the alkenyl epoxy is glycidyl methacrylate.
The preparation method of the super-hydrophobic drag reduction coating is characterized by comprising the following steps: the alkali catalyst is alkaline compounds such as dimethyl phenyl phosphine, tributyl phosphine, diethylenetriamine and the like.
The preparation method of the super-hydrophobic drag reduction coating is characterized by comprising the following steps: the amino curing agent is one or a combination of more of 4,4' -dithiodiphenylamine, dicyandiamide, modified dicyandiamide, urea derivatives and imidazole derivatives.
The preparation method of the super-hydrophobic drag reduction coating is characterized by comprising the following steps: the preparation method of the hydrophobic particle suspension comprises the following steps of mixing hydrophobic particles and a solvent B according to a mass ratio of 1: 10-20, and ultrasonically dispersing the mixture uniformly.
The preparation method of the hydrophobic particle suspension is characterized by comprising the following steps: the hydrophobic particles are fluorinated silica with the particle size of 100-2000 nm, polytetrafluoroethylene micro powder and polyvinylidene fluoride micro powder.
The preparation method of the hydrophobic particle suspension is characterized by comprising the following steps: the solvent B is absolute ethyl alcohol, acetone, tetrahydrofuran, N-dimethylacetamide and the like.
Comparative example 1
A common hydrophobic coating (polyurethane coating) was chosen with a contact angle of 105 °.
And (3) resistance reduction test: a BROOKFIELD R/S type rheometer is selected for resistance reduction test. The hydrophobic coating was coated on a rotor disc of 50mm diameter, the gap 0.2mm from the base plate was filled with water and the torque was tested at 1000 rpm/min.
The results for the hydrophobic coating of comparative example 1 show a torque of 1.18 μ N · m. The plain rotor disk without any coating applied had a torque of 1.22 μ N · m under the same test conditions according to the formula for drag reduction:
DR＝1-Msu/Msm，
wherein M issuAnd MsmRepresenting the torque value of the coating and the torque value of the bare rotor, respectively. The drag reduction of a conventional hydrophobic coating is thus 3.2%.
Example 1
Under the protection of nitrogen, 50g of acetone, 24.2g of trimethylolpropane tri (3-mercaptopropionate), 25.8g of glycidyl methacrylate and 0.5g of dimethyl phenylphosphine were sequentially added into a reactor to perform mercapto-ene addition reaction at normal temperature for 6 hours, and then an epoxy prepolymer solution was obtained. And then mixing the epoxy prepolymer solution with 25g of 4,4' -dithiodiphenylamine according to the mass ratio, and uniformly stirring to obtain a resin matrix. Then 10g of fluorine-containing silica (100nm) was mixed with 100g of ethanol and dispersed uniformly by ultrasonic waves. And finally, uniformly spraying a resin matrix on a glass sheet, spraying a hydrophobic particle suspension once after the solvent is completely volatilized, spraying a layer of resin matrix again after the solvent of the suspension is completely volatilized, repeatedly spraying the resin matrix and the hydrophobic particle suspension for 6 times, and curing in a blowing oven at the temperature of 140 ℃ for 4 hours to obtain the super-hydrophobic anti-drag coating.
And (3) resistance reduction test: a BROOKFIELD R/S type rheometer is selected for resistance reduction test. The super-hydrophobic coating is coated on a rotor disc with the diameter of 50mm, a gap with the distance of 0.2mm from the bottom plate is filled with water, and the torque is tested at the rotating speed of 1000 rpm/min.
The test results for the superhydrophobic coating of example 1 show a torque of 0.96 μ N · m and a torque of 1.22 μ N · m for the plain rotor disc without any coating under the same test conditions, according to the calculation formula for the drag reduction:
DR＝1-Msu/Msm，
wherein M issuAnd MsmRespectively representing the torque value and light of the coatingTorque value of the face rotor. The drag reduction of a conventional hydrophobic coating is thus 21.3%.
Example 2
Under the protection of nitrogen, 125g of tetrahydrofuran, 23.1g of pentaerythritol tetramercaptopropionate, 26.9g of glycidyl methacrylate and 1.25g of tributylphosphine were sequentially added into a reactor to perform mercapto-ene addition reaction at normal temperature, and an epoxy prepolymer solution was obtained after 8 hours. And then mixing the epoxy prepolymer solution with 20g of modified dicyandiamide, and uniformly stirring to obtain the resin matrix. Then 10g of polytetrafluoroethylene micropowder (1000nm) was mixed with 150g of tetrahydrofuran and dispersed uniformly by ultrasonic. And finally, uniformly spraying a resin matrix on a glass sheet, spraying a hydrophobic particle suspension once after the solvent is completely volatilized, spraying a layer of resin matrix again after the solvent of the suspension is completely volatilized, repeatedly spraying the resin matrix and the hydrophobic particle suspension for 8 times in the way, and curing in a blowing oven at 180 ℃ for 2 hours to obtain the super-hydrophobic anti-drag coating.
And (3) resistance reduction test: a BROOKFIELD R/S type rheometer is selected for resistance reduction test. The super-hydrophobic coating is coated on a rotor disc with the diameter of 50mm, a gap with the distance of 0.2mm from the bottom plate is filled with water, and the torque is tested at the rotating speed of 1000 rpm/min.
The test results for the superhydrophobic coating of example 1 show a torque of 0.92 μ N · m and a torque of 1.22 μ N · m for the plain rotor disc without any coating under the same test conditions, according to the calculation formula for the drag reduction:
DR＝1-Msu/Msm，
wherein M issuAnd MsmRepresenting the torque value of the coating and the torque value of the bare rotor, respectively. The drag reduction of a conventional hydrophobic coating is thus 24.6%.
Example 3
Under the protection of nitrogen, 250g N N-dimethylacetamide, 23.9g dipentaerythritol hexamercaptopropionate, 26.1g glycidyl methacrylate and 2.5g diethylenetriamine are sequentially added into a reactor to carry out mercapto-alkene addition reaction at normal temperature, and an epoxy prepolymer solution is obtained after 10 hours. Then, the epoxy prepolymer solution was mixed with 10g of an imidazole derivative and uniformly stirred to obtain a resin matrix. Then 10g polyvinylidene fluoride micropowder (2000nm) was mixed with 200g N, N-dimethylacetamide and dispersed uniformly by ultrasound. And finally, uniformly spraying a resin matrix on a glass sheet, spraying a hydrophobic particle suspension once after the solvent is completely volatilized, spraying a layer of resin matrix again after the solvent of the suspension is completely volatilized, repeatedly spraying the resin matrix and the hydrophobic particle suspension for 10 times in the way, and curing in a blast oven at 100 ℃ for 6 hours to obtain the super-hydrophobic anti-drag coating.
And (3) resistance reduction test: a BROOKFIELD R/S type rheometer is selected for resistance reduction test. The super-hydrophobic coating is coated on a rotor disc with the diameter of 50mm, a gap with the distance of 0.2mm from the bottom plate is filled with water, and the torque is tested at the rotating speed of 1000 rpm/min.
The test results for the superhydrophobic coating of example 1 show a torque of 0.88 μ N · m and a torque of 1.22 μ N · m for the plain rotor disc without any coating under the same test conditions, according to the formula for calculation of the drag reduction:
DR＝1-Msu/Msm，
wherein M issuAnd MsmRepresenting the torque value of the coating and the torque value of the bare rotor, respectively. The drag reduction of a conventional hydrophobic coating is thus 27.9%.
Claims (5)
1. A preparation method of a super-hydrophobic drag reduction coating is characterized by comprising the following steps:
step 1, preparation of epoxy prepolymer: under the protection of nitrogen, sequentially adding a multifunctional thiol compound, an alkenyl epoxy mixture, a solvent A and an alkali catalyst into a reactor, carrying out a mercapto-alkene addition reaction at normal temperature, and obtaining an epoxy prepolymer after 6-10 hours; the mass ratio of the multifunctional thiol compound to the alkenyl epoxy mixture, the solvent A and the base catalyst is 1: 1-5: 0.01-0.05; in the mixture of the multifunctional thiol compound and the alkenyl epoxy, the multifunctional thiol compound and the alkenyl epoxy are mixed according to the molar ratio of 1:1 of sulfydryl to epoxy group;
the alkenyl epoxy is glycidyl methacrylate;
step 2, preparation of a resin matrix: mixing the epoxy prepolymer and the amino curing agent according to the mass ratio of 100: 20-50, and stirring to obtain a resin matrix;
step 3, preparing the super-hydrophobic drag reduction coating: spraying the resin matrix and the hydrophobic particle suspension liquid at intervals in a layered manner for 6-10 times, and placing the resin matrix and the hydrophobic particle suspension liquid in a blast oven at the temperature of 100-180 ℃ for curing for 2-6 h to obtain a super-hydrophobic anti-drag coating;
when spraying, the first layer on the substrate is a resin matrix, and the last layer is a hydrophobic particle suspension; after the resin matrix or the hydrophobic particle suspension is sprayed, the next layer is sprayed after the solvent is completely volatilized;
the hydrophobic particle suspension is as follows: mixing hydrophobic particles and a solvent B according to a mass ratio of 1: 10-20, mixing to obtain a hydrophobic particle suspension;
the solvent A is acetone, tetrahydrofuran, N-methyl pyrrolidone or N, N-dimethyl acetamide;
the multifunctional thiol compound is glycerol trimercapto propionate, trimethylolpropane trimercapto propyl ester, isocyanuric acid trimercapto carboxylate, pentaerythritol tetramercaptopropionate or dipentaerythritol hexamercapto propionate.
2. The method of preparing a superhydrophobic drag reducing coating of claim 1, characterized in that: the alkali catalyst is dimethyl phenyl phosphine, tributyl phosphine or a diethylenetriamine basic compound.
3. The method of preparing a superhydrophobic drag reducing coating of claim 1, characterized in that: the amino curing agent is one or a combination of more of 4,4' -dithiodiphenylamine, dicyandiamide, modified dicyandiamide, urea derivatives and imidazole derivatives.
4. The method of preparing a superhydrophobic drag reducing coating of claim 1, characterized in that: the hydrophobic particles are fluorinated silica, polytetrafluoroethylene micro powder or polyvinylidene fluoride micro powder, and the particle size of the particles is 100-2000 nm.
5. The method of preparing a superhydrophobic drag reducing coating of claim 1, characterized in that: the solvent B is absolute ethyl alcohol, acetone, tetrahydrofuran or N, N-dimethylacetamide.
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