CN115558415A - Novel marine antifouling coating based on polydopamine ball oil storage and preparation method thereof - Google Patents

Novel marine antifouling coating based on polydopamine ball oil storage and preparation method thereof Download PDF

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Publication number
CN115558415A
CN115558415A CN202211367768.3A CN202211367768A CN115558415A CN 115558415 A CN115558415 A CN 115558415A CN 202211367768 A CN202211367768 A CN 202211367768A CN 115558415 A CN115558415 A CN 115558415A
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polydopamine
ball
marine antifouling
oil
template
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CN202211367768.3A
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Inventor
李中
范白涛
任美鹏
王名春
王秀通
杨向前
郭华
陈宏举
王彬
张会增
殷志明
普佳艳
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Beijing Research Center of CNOOC China Ltd
CNOOC China Ltd
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Beijing Research Center of CNOOC China Ltd
CNOOC China Ltd
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Priority to CN202211367768.3A priority Critical patent/CN115558415A/en
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D183/00Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Coating compositions based on derivatives of such polymers
    • C09D183/04Polysiloxanes
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D5/00Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/16Antifouling paints; Underwater paints
    • C09D5/1656Antifouling paints; Underwater paints characterised by the film-forming substance
    • C09D5/1662Synthetic film-forming substance
    • C09D5/1675Polyorganosiloxane-containing compositions
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D5/00Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/16Antifouling paints; Underwater paints
    • C09D5/1687Use of special additives

Abstract

The invention discloses a novel marine antifouling coating based on polydopamine ball oil storage and a preparation method thereof. The preparation method comprises the following steps: preparing dopamine hydrochloride into a polydopamine ball with cracks on the surface, and then soaking the polydopamine ball in excessive silicone oil to obtain an oil-storing polydopamine ball; mixing the prepolymer A forming the polydimethylsiloxane with the curing agent B, adding the oil-stored polydopamine balls, uniformly dispersing, and removing bubbles to obtain a homogeneous marine antifouling composite material; and then, coating the template with the micro-nano structure by scraping, drying and then stripping the template to obtain the nano-composite material. The marine antifouling coating can effectively prevent marine organisms from attaching and has good resistance reducing performance, so that fouling organisms are not easy to attach or not firmly attached on the surface of a material, and an antifouling effect can be achieved.

Description

Novel marine antifouling coating based on polydopamine ball oil storage and preparation method thereof
Technical Field
The invention relates to a novel marine antifouling coating based on polydopamine ball oil storage and a preparation method thereof, and belongs to the technical field of marine antifouling.
Background
The marine biofouling is one of the problems which plague the global marine economic development, and the adsorption of marine biofouling organisms can cause serious damage to offshore operation equipment, thereby bringing huge economic loss to marine engineering. In the marine environment, the surface of any material inevitably suffers from the adhesion of marine fouling organisms, which not only affects the normal operation of equipment, but also increases energy consumption, therefore, the development of a novel marine antifouling material is urgent, and the application of an antifouling paint is an important way for solving the problem.
Most of coatings which are made of antifouling agents and seep out to prevent fouling have the problem that cavities are formed inside coatings after seepage to influence the mechanical property of the coatings and the seepage speed control, so that the existing antifouling materials need to be improved, marine organisms are difficult to attach or not firmly attached on the surfaces of the coatings, and the coatings are easy to fall off under the action of water flow or external force, and the aim of preventing the attachment of fouling organisms is fulfilled.
Disclosure of Invention
The invention aims to provide a polydopamine ball oil storage-based marine antifouling coating, and aims to solve the problems of complex preparation method and high cost of marine fouling organism adhesion and antifouling coatings; the method has the advantages of simple process, low cost, excellent self-cleaning performance, long-term antifouling effect and suitability for widely applied marine antifouling composite materials, so that the antifouling performance of the coating is improved.
The invention provides a preparation method of a marine antifouling coating based on polydopamine ball oil storage, which comprises the following steps:
s1, preparing dopamine hydrochloride into a polydopamine ball with a crack on the surface, and then soaking the polydopamine ball in excessive silicone oil to obtain an oil-storage polydopamine ball;
s2, mixing the prepolymer A forming the polydimethylsiloxane with a curing agent B, adding the polydopamine ball for oil storage, and uniformly dispersing and removing bubbles to obtain a homogeneous marine antifouling composite material;
and S3, scraping the marine antifouling composite material on a template with a micro-nano structure, drying and peeling the template to obtain the marine antifouling coating based on the polydopamine ball oil storage.
In the above preparation method, in step S1, the polydopamine sphere is prepared according to the following steps:
in the presence of ammonia water, in a mixed solution of water and ethanol, dopamine hydrochloride is subjected to self polymerization to obtain a polydopamine ball, and then cracks are generated on the surface of the polydopamine ball after calcination;
the particle size of the polydopamine sphere is 230 nm-270 nm.
In the preparation method, the mass concentration of the dopamine hydrochloride in the mixed solution is 3.5-4 mg/ml;
in the mixed solution, the volume concentration of the water is 77-79%, and the volume concentration of the ethanol is 21-23%;
the calcination conditions were as follows:
an inert atmosphere;
the temperature is 880-900 ℃;
the time is 1.5 to 2 hours;
the calcination is preceded by a wash: sequentially using deionized water and absolute ethyl alcohol to carry out ultrasonic treatment for 3-5 min, then centrifuging for 3-5 min by a centrifugal machine, and alternately washing for 3-5 times.
In the preparation method, in the step S1, the silicone oil is dimethyl silicone oil with the viscosity of 50-350 mm 2 /s;
The mass ratio of the polydopamine ball to the silicone oil is 1:5 to 6;
the soaking conditions were as follows:
drying the mixture in a vacuum drying oven for 3 to 5 hours at normal temperature.
In the above preparation method, in step S2, bubbles are removed as follows: and placing the mixture in a vacuum drying oven for vacuum treatment for 30-40 min at room temperature.
In the preparation method, in step S2, the mass ratio of the oil-storing polydopamine spheres to the polydimethylsiloxane is 1:18 to 20.
In the above preparation method, in step S3, the template is prepared according to the following method:
spraying the ground salt powder (such as adopting a pneumatic self-suction sand-blasting gun) on an aluminum plate to obtain the aluminum plate with the surface uniformly attached with the salt powder; then carrying out ultrasonic treatment on the template by using deionized water to obtain a clean template with a micro-nano structure;
the particle size of the salt powder is 5-10 microns, and the salt powder can be obtained by grinding commercial edible salt by adopting a grinder.
In the preparation method, in the step S3, the drying is carried out in a vacuum drying oven, and the drying is carried out for 70 to 72 hours at the temperature of between 25 and 30 ℃ under the atmospheric pressure condition.
The novel ocean antifouling coating based on polydopamine sphere oil storage provided by the invention has a micro-nano structure on the surface.
According to the invention, the PDMS is doped with the polydopamine sphere for storing oil, and the gap on the surface of the polydopamine sphere is used as an oil storage space, so that the doping effectively reduces the formation of an internal cavity of the coating after oil seepage and has a slow release effect on oil, the oil seepage time is prolonged, and the influence of the oil seepage on the coating structure is reduced; the coating surface has a micro-nano structure, and is matched with the seepage of oil, so that marine organisms are effectively prevented from attaching, and the coating has good resistance reducing performance, so that fouling organisms are not easy to attach or not firmly attached to the material surface, and an antifouling effect can be achieved.
Compared with the prior art, the invention has the following beneficial effects:
in terms of materials, the polydimethylsiloxane is a non-toxic and stable material, the polydopamine is a biological bionic material, and the polydopamine has the characteristics of environmental friendliness, simplicity in preparation and the like, and is fully utilized in the aspect of marine antifouling; on the surface structure of the coating, a microstructure imitating the marine organism skin is processed, so that fouling organisms are difficult to attach to the surface of the coating, and the aim of preventing the biofouling is achieved by utilizing the slow seepage of silicone oil.
Drawings
Fig. 1 is an SEM image of polydopamine spheres before calcination prepared in example 1 of the present invention.
Fig. 2 is an SEM image of calcined polydopamine spheres prepared in example 1 of the present invention.
Fig. 3 is a schematic structural diagram of a novel marine antifouling coating based on polydopamine ball oil storage prepared in example 1 of the invention.
Fig. 4 is a contact angle test chart of the novel marine antifouling coating based on polydopamine ball oil storage prepared in example 1 of the invention.
Fig. 5 is a contact angle test chart of the novel marine antifouling coating based on polydopamine ball oil storage prepared in example 2 of the invention.
FIG. 6 shows the results of soaking the novel PABA coating prepared in example 1 in a concentration of 130350000cfu/ml for three days.
FIG. 7 shows the results of soaking the novel PABA coating prepared in example 2 in a concentration of 130350000cfu/ml for three days.
Fig. 8 shows the anti-algae adhesion results of the novel marine anti-fouling coating based on polydopamine ball oil storage prepared in example 1 of the present invention.
Fig. 9 shows the anti-algae adhesion results of the novel marine anti-fouling coating based on polydopamine ball oil storage prepared in example 2 of the present invention.
FIG. 10 shows the results of three days after soaking the PDMS in the chlorella solution with a concentration of 130350000 cfu/ml.
FIG. 11 shows a polydimethylsiloxane doping viscosity of 350mm 2 Results of anti-algal adhesion of dimethicone/s.
FIG. 12 shows a polydimethylsiloxane doping viscosity of 50mm 2 The result of soaking the microspherical algae solution in 130350000cfu/ml for three days is obtained.
FIG. 13 shows a polydimethylsiloxane doping viscosity of 50mm 2 Anti-algae adhesion results of dimethicone/s.
Detailed Description
The experimental procedures used in the following examples are all conventional procedures unless otherwise specified.
Materials, reagents and the like used in the following examples are commercially available unless otherwise specified.
EXAMPLE 1 novel Marine antifouling coatings based on Polydopamine ball oil storage
(1) Preparation of polydopamine spheres
Dissolving 0.5g of dopamine hydrochloride in 90ml of deionized water, adding 40ml of absolute ethyl alcohol after full dissolution, mixing and stirring for 30min to obtain a dopamine mixed solution with the concentration of 3.8 mg/ml;
adding 2ml of ammonia water into the solution, stirring and reacting for 7 hours at room temperature, sequentially using deionized water and absolute ethyl alcohol for ultrasonic treatment for 4 minutes, centrifuging for 5 minutes by a centrifugal machine, alternately washing for 4 times, and drying for 5 hours at 80 ℃ in a vacuum drying oven under a vacuum condition to obtain the polydopamine spheres with smooth surfaces.
Calcining the mixture for 2 hours at 900 ℃ in a tubular furnace in Ar atmosphere to obtain the poly-dopamine ball with cracks distributed on the surface.
(2) Preparation of the template
The method comprises the steps of grinding commercial salt by a grinder to obtain salt powder with the diameter of about 10 micrometers, spraying the edible salt powder on an aluminum plate by using a pneumatic self-suction sand blasting gun to obtain the aluminum plate with the surface uniformly attached with the edible salt powder, carrying out ultrasonic treatment on the aluminum plate with the surface uniformly attached with the edible salt powder by using deionized water for 25 minutes, and replacing the deionized water every 5 minutes to obtain the clean aluminum template with the micro-nano structure.
(3) Preparation of the coating
0.1g of polydopamine ball obtained in the step (1) is weighed and soaked in 0.5g of polydopamine ball with the viscosity of 350mm 2 Mixing dimethyl silicone oil/s in a vacuum drying oven at normal temperature for 4 hours to obtain oil-stored polydopamine balls for later use;
prepolymer A (SYLGARD 184Silicone Elastomer Base) forming polydimethylsiloxane (SYLGARD 184) and Curing agent B (SYLGARD 184Silicone Elastomer Curing) were mixed in the following 10:1, and then, dispersing and stirring the mixture and the obtained oil-storage polydopamine ball until the mixture is uniform, wherein the mass ratio of the oil-storage polydopamine ball to polydimethylsiloxane is 1:20, placing the marine antifouling composite material in a vacuum drying oven, and vacuumizing to remove bubbles to obtain the marine antifouling composite material for later use;
fixing the aluminum template obtained in the step (2) at the bottom of a culture dish, pouring the marine antifouling composite material into the culture dish, then placing the culture dish in a vacuum drying oven, firstly placing the culture dish in a vacuum condition for 30min, then placing the culture dish in an atmospheric pressure condition, and drying the culture dish for 70h at the temperature of 25-30 ℃ to obtain the novel marine antifouling coating.
Fig. 1 is an SEM image of the poly-dopamine sphere prepared in this example before calcination, the diameter of the poly-dopamine sphere is 240nm to 270nm, and the surface is smooth.
Fig. 2 is an SEM image of the calcined polydopamine sphere prepared in this example, the diameter of the polydopamine sphere is 240nm to 270nm, the volume change is not generated after calcination, but cracks appear on the surface.
Fig. 3 is a schematic structural diagram of the novel marine antifouling coating based on polydopamine ball oil storage prepared in this embodiment.
Fig. 4 is a contact angle test chart of the novel marine antifouling coating based on polydopamine sphere oil storage prepared in this embodiment, and it can be seen that the novel marine antifouling coating based on polydopamine sphere oil storage has a better hydrophobic effect.
FIG. 10 shows a polydimethylsiloxane doping viscosity of 350mm 2 The result of soaking the microspherical algae solution in 130350000cfu/ml for three days is obtained.
FIG. 11 shows a polydimethylsiloxane doping viscosity of 350mm 2 Anti-algae adhesion results of dimethicone/s.
FIG. 6 shows the results of the novel PABA coating prepared in this example and based on oil storage of poly-dopamine beads soaked in the chlorella solution with a concentration of 130350000cfu/ml for three days.
Fig. 8 shows the anti-algae adhesion result of the novel marine antifouling coating based on polydopamine sphere oil storage prepared in the embodiment, and compared with fig. 6, it can be seen that the novel marine antifouling coating based on polydopamine sphere oil storage has good antifouling performance.
EXAMPLE 2 novel Marine antifouling coatings based on Polydopamine ball oil storage
(1) Preparation of polydopamine spheres
Dissolving 0.5g of dopamine hydrochloride in 90ml of deionized water, adding 40ml of absolute ethyl alcohol after full dissolution, mixing and stirring for 30min to obtain a dopamine mixed solution with the concentration of 3.8 mg/ml;
adding 2ml of ammonia water into the solution, stirring and reacting for 8 hours at room temperature, sequentially performing ultrasonic treatment on the solution by using deionized water and absolute ethyl alcohol for 5 minutes, centrifuging the solution by using a centrifugal machine for 4 minutes, alternately washing the solution for 5 times, and drying the solution in a vacuum drying oven for 5 hours at 80 ℃ under a vacuum condition to obtain polydopamine spheres with smooth surfaces;
calcining the mixture for 2 hours at 900 ℃ in a tubular furnace in Ar atmosphere to obtain the poly-dopamine ball with cracks distributed on the surface.
(2) Preparation of the template
The method comprises the steps of grinding commercial salt by a grinder to obtain salt powder with the diameter of about 10 micrometers, spraying the edible salt powder on an aluminum plate by using a pneumatic self-suction sand blasting gun to obtain the aluminum plate with the surface uniformly attached with the edible salt powder, carrying out ultrasonic treatment on the aluminum plate with the surface uniformly attached with the edible salt powder by using deionized water for 25 minutes, and replacing the deionized water every 5 minutes to obtain the clean aluminum template with the micro-nano structure.
(3) Preparation of the coating
0.1g of polydopamine ball obtained in the step (1) is weighed and soaked in 0.5g of polydopamine ball with the viscosity of 50mm 2 Mixing dimethyl silicone oil/s in a vacuum drying oven at normal temperature for 4 hours to obtain oil-stored polydopamine balls for later use;
prepolymer A (SYLGARD 184Silicone Elastomer Base) forming polydimethylsiloxane (SYLGARD 184) was mixed with Curing agent B (SYLGARD 184Silicone Elastomer Curing) in a 10:1, and then uniformly mixing the oil-stored polydopamine spheres with the oil-stored polydopamine spheres in a dispersing and stirring manner until the oil-stored polydopamine spheres and polydimethylsiloxane are uniformly mixed, wherein the mass ratio of the oil-stored polydopamine spheres to the polydimethylsiloxane is 1:20, placing the marine antifouling composite material in a vacuum drying oven, and vacuumizing to remove bubbles to obtain the marine antifouling composite material for later use;
fixing the aluminum template obtained in the step (2) at the bottom of a culture dish, pouring the marine antifouling composite material into the culture dish, then placing the culture dish into a vacuum drying oven, firstly placing the culture dish under a vacuum condition for 40min, then placing the culture dish under an atmospheric pressure condition, and drying the culture dish for 70-72 h at 25-30 ℃.
Fig. 5 is a contact angle test chart of the novel marine antifouling coating based on polydopamine sphere oil storage prepared in this embodiment, and it can be seen that the novel marine antifouling coating based on polydopamine sphere oil storage has better hydrophobic property, is favorable for forming a super-hydrophobic surface, inhibits adhesion of bacteria, and makes fouling organisms more difficult to attach to the coating surface.
FIG. 12 shows a polydimethylsiloxane doping viscosity of 50mm 2 The result of three days after soaking the chlorella in the simethicone solution with the concentration of 130350000 cfu/ml.
FIG. 13 shows a polydimethylsiloxane doping viscosity of 50mm 2 Anti-algae adhesion results of dimethicone/s.
FIG. 7 shows the results of the novel PABA coating prepared in this example and based on oil storage of poly-dopamine beads soaked in the chlorella solution with a concentration of 130350000cfu/ml for three days.
Fig. 9 shows the anti-algae adhesion result of the novel marine antifouling coating based on polydopamine sphere oil storage prepared in the embodiment, and compared with fig. 7, it can be seen that the novel marine antifouling coating based on polydopamine sphere oil storage has good antifouling performance.
Wherein, the steps of the algae adhesion resisting experiment are as follows:
according to the national standard, the prepared antifouling sample plate is hung and soaked in chlorella liquid with the concentration of 130350000cfu/ml and is placed in a warm position with sufficient sunlight for three days. The sample plate was then placed under a fluorescent microscope to observe the attachment of chlorella. Then at a flow velocity of 61.571m 3 The anti-fouling sample plate was washed for 3 seconds under water flow, and the anti-fouling sample plate was placed under a fluorescence microscope again to observe the adhesion of chlorella.

Claims (10)

1. A preparation method of a marine antifouling coating based on polydopamine ball oil storage comprises the following steps:
s1, preparing dopamine hydrochloride into a polydopamine ball with cracks on the surface, and then soaking the polydopamine ball in excessive silicone oil to obtain an oil-storage polydopamine ball;
s2, mixing the prepolymer A forming the polydimethylsiloxane with a curing agent B, adding the polydopamine ball for oil storage, and uniformly dispersing and removing bubbles to obtain a homogeneous marine antifouling composite material;
and S3, scraping the marine antifouling composite material on a template with a micro-nano structure, drying and peeling the template to obtain the marine antifouling coating based on the polydopamine ball oil storage.
2. The production method according to claim 1, characterized in that: in step S1, the polydopamine sphere is prepared according to the following steps:
carrying out self-polymerization on dopamine hydrochloride in a mixed solution of water and ethanol in the presence of ammonia water to obtain a polydopamine ball, and then calcining to show that a crack is generated;
the particle size of the polydopamine sphere is 230 nm-270 nm.
3. The method of claim 2, wherein: in the mixed solution, the mass concentration of the dopamine hydrochloride is 3.5-4.0 mg/ml;
in the mixed solution, the volume concentration of the water is 77-79%, and the volume concentration of the ethanol is 21-23%;
the calcination conditions were as follows:
an inert atmosphere;
the temperature is 880-900 ℃;
the time is 1.5 to 2 hours.
4. The production method according to any one of claims 1 to 3, characterized in that: in the step S1, the silicone oil is dimethyl silicone oil;
the mass ratio of the polydopamine ball to the silicone oil is 1:5 to 6
The soaking conditions were as follows:
drying the mixture in a vacuum drying oven for 3 to 5 hours at normal temperature.
5. The production method according to any one of claims 1 to 4, characterized in that: in step S2, bubbles are removed as follows: and placing the mixture in a vacuum drying oven for vacuum treatment for 30-40 min at room temperature.
6. The production method according to any one of claims 1 to 5, characterized in that: in the step S2, the mass ratio of the polydopamine ball storing the oil to the polydimethylsiloxane is 1:18 to 20.
7. The production method according to any one of claims 1 to 6, characterized in that: in step S3, the template is prepared according to the following method:
spraying the ground salt powder on an aluminum plate to obtain the aluminum plate with the surface uniformly attached with the salt powder; then carrying out ultrasonic treatment on the template by using deionized water to obtain a clean template with a micro-nano structure;
the particle size of the salt powder is 5-10 microns.
8. The production method according to any one of claims 1 to 7, characterized in that: in the step S3, the drying is carried out in a vacuum drying oven and is dried for 70 to 72 hours at the temperature of between 25 and 30 ℃ under the atmospheric pressure condition.
9. A marine antifouling coating prepared by the process of any of claims 1 to 8.
10. Use of a marine antifouling coating according to claim 9 for preventing the attachment of marine fouling organisms to a man-made structure.
CN202211367768.3A 2022-11-03 2022-11-03 Novel marine antifouling coating based on polydopamine ball oil storage and preparation method thereof Pending CN115558415A (en)

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CN111534190A (en) * 2020-03-12 2020-08-14 复旦大学 Double-response self-repairing super-hydrophobic coating material and preparation method thereof
CN113663891A (en) * 2021-08-13 2021-11-19 苏州大学 PDMS (polydimethylsiloxane) repairable super-hydrophobic coating and preparation method thereof
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CN110277563A (en) * 2019-06-10 2019-09-24 北京科技大学 A kind of preparation method of N doping hollow carbon sphere elctro-catalyst
CN111534190A (en) * 2020-03-12 2020-08-14 复旦大学 Double-response self-repairing super-hydrophobic coating material and preparation method thereof
CN113663891A (en) * 2021-08-13 2021-11-19 苏州大学 PDMS (polydimethylsiloxane) repairable super-hydrophobic coating and preparation method thereof
CN114907766A (en) * 2022-03-14 2022-08-16 中海石油(中国)有限公司 Novel marine antifouling material based on biochar micro-nano structure and preparation method and application thereof
CN114806397A (en) * 2022-03-21 2022-07-29 昆明理工大学 Green self-repairing type super-smooth surface marine antifouling coating and preparation method thereof

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