CN115537076A - Fluoride-free super-hydrophobic coating composition and super-hydrophobic coating - Google Patents
Fluoride-free super-hydrophobic coating composition and super-hydrophobic coating Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING 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
- C09D125/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring; Coating compositions based on derivatives of such polymers
- C09D125/02—Homopolymers or copolymers of hydrocarbons
- C09D125/04—Homopolymers or copolymers of styrene
- C09D125/06—Polystyrene
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D5/00—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures
- B05D5/08—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures to obtain an anti-friction or anti-adhesive surface
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
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- C09D—COATING 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
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/08—Anti-corrosive paints
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D2202/00—Metallic substrate
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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Abstract
The invention provides a fluorine-free super-hydrophobic coating composition and a super-hydrophobic coating, belonging to the field of coatings. The super-hydrophobic coating not only has excellent hydrophobic effect, but also has excellent corrosion resistance and weather resistance. The method for preparing the super-hydrophobic coating does not use strong acid, strong alkali and fluorine-containing silane coupling agent, is green, nontoxic, simple and feasible, and is suitable for industrial expanded production.
Description
Technical Field
The invention belongs to the field of coatings, and particularly relates to a fluorine-free super-hydrophobic coating composition and a super-hydrophobic coating.
Background
Icing of an aircraft is one of the major hazards that lead to flight safety accidents. In the flight process, the icing on the surfaces of components such as the front edge of the wing and the like not only increases the weight of the airplane, but also destroys the aerodynamic appearance and influences the aerodynamic characteristics of the airplane, thereby influencing the flight safety, and the serious icing can cause the death of the airplane and the people. Studies have shown that the probability of a global aircraft crash due to icing exceeds 15%.
Currently, conventional anti/de-icing methods include mechanical de-icing, solution de-icing, and thermal de-icing, but these methods are energy intensive, inefficient, short in anti-icing duration, and can have environmental consequences. The novel deicing method achieves the purpose of deicing by mainly designing the special shape structure and chemical composition of the surface of the material, and has the characteristics of low energy consumption and high efficiency. The super-hydrophobic coating is an ideal anti-icing/deicing material and has the advantages of zero energy consumption, no complex control system and the like; the low surface energy and the micro-nano structure of the coating are mainly utilized to reduce the adhesion of water drops on the surface of the coating, so that the water drops slide off the surface of the airplane before the icing, and the icing on the surface of the airplane is delayed.
Chinese patent application publication No. CN112359356A discloses a method for preparing a superhydrophobic zinc-aluminum hydrotalcite-like coating on an aluminum alloy surface: mechanically polishing and ultrasonically cleaning an aluminum alloy sample to remove an oxide film and impurities on the surface of the aluminum alloy sample; then, dissolving a proper amount of zinc sulfate and urea in deionized water, fully stirring to uniformly mix the solution, placing the aluminum alloy sample subjected to surface treatment and the mixed solution in a hydrothermal reaction kettle, reacting for a period of time at a certain temperature, taking out, drying by cold air, and obtaining a zinc-aluminum hydrotalcite-like coating with a sheet or sheet-needle structure on the surface of the aluminum alloy; and finally, soaking the sample in an absolute ethyl alcohol solution of stearic acid for modification to obtain the zinc-aluminum hydrotalcite coating with the super-hydrophobic function. The method is simple to operate and environment-friendly, and the contact angle of deionized water on the surface of the coating exceeds 150 degrees, and the rolling angle is lower than 10 degrees. However, the hydrothermal reaction is not beneficial to controlling the uniformity of the coating, and the preparation method of the coating needs to use a hydrothermal reaction kettle, so that the method is not suitable for industrial expanded production.
An embodiment 4 of chinese patent application with publication number CN110734700A discloses a super-hydrophobic coating composite material for preventing/removing ice, the preparation method is as follows: dissolving 50mg of Polydimethylsiloxane (PDMS) and 5mg of a curing agent in n-hexane, adding 20mg of hydrophobic ring cross-linked polyphosphazene microspheres (namely PHC microspheres), dispersing for 15min by ultrasonic waves, and stirring for 1h on a magnetic stirrer to obtain a PDMS/PHC dispersion liquid. And uniformly spraying the dispersion liquid on the surface of the pretreated steel by adopting a spraying process, and then placing the pretreated steel in a physicochemical drying oven for curing reaction for 3 hours at 60 ℃ to obtain the PDMS/PHC coating composite material. The contact angle of the liquid drop on the surface of the coating is 164 degrees, the rolling angle is 3.7 degrees, and the icing delay time is 1472s. However, the PHC microspheres used in the superhydrophobic coating have a complex preparation method, which increases the process cost and difficulty.
The development of the super-hydrophobic coating which is low in process cost, easy to prepare, and excellent in corrosion resistance and weather resistance is of great significance.
Disclosure of Invention
It is an object of the present invention to provide a fluorine-free superhydrophobic coating composition.
The invention also aims to provide a fluorine-free environment-friendly super-hydrophobic coating with excellent corrosion resistance and weather resistance and a preparation method thereof.
The invention provides a fluorine-free super-hydrophobic coating composition, which comprises the following components: the silicone rubber-polystyrene microsphere comprises silicone rubber, polystyrene microspheres and a solvent, wherein the weight ratio of the silicone rubber to the polystyrene microspheres is (0.10-1.1): (0.5-4.0).
Further, the weight ratio of the silicone rubber to the polystyrene microspheres is 0.22:3.0.
further, the concentration of the polystyrene microspheres is (0.5-4.0): 40g/ml, preferably 3.0:40g/ml.
Further, the silicone rubber is SYLGARD 184silicone rubber.
Further, the SYLGARD 184silicon rubber is a Dow chemical SYLGARD TM 184Silicone Elastomer Kit。
Further, the particle size of the polystyrene microsphere is 1-10 μm, preferably 5 μm; and/or the solvent is petroleum ether.
The invention also provides a method for preparing the fluorine-free super-hydrophobic coating, which comprises the following steps:
(1) Pretreating the surface of the base material: polishing with sand paper, and cleaning with organic solvent;
(2) Preparing the fluorine-free super-hydrophobic coating composition as a spraying liquid;
(3) And (2) spraying the spraying liquid on the surface of the base material pretreated in the step (1), and curing to obtain the fluorine-free super-hydrophobic coating.
Further, in the step (1), the substrate is a metal substrate, preferably an aluminum alloy substrate; and/or the organic solvent is one or the mixture of ethanol and acetone.
Further, in the step (3), the number of sprayed layers is 2-10, the spraying pressure is 0.1-1.0 MPa, and the distance from the nozzle to the base material is 5-20 cm during spraying; the curing temperature is 100-140 ℃, and the curing time is 2-4 h;
preferably, in the step (3), the number of the coating layers is 8, the spraying pressure is 0.2MPa, and the distance from the nozzle to the substrate is 10cm during spraying; the curing temperature is 120 ℃ and the curing time is 3h.
The invention also provides the fluorine-free super-hydrophobic coating prepared by the method.
The invention also provides a fluorine-free super-hydrophobic material which comprises the fluorine-free super-hydrophobic coating.
Compared with the prior art, the invention has the following beneficial effects:
(1) The super-hydrophobic coating obtained by the invention has excellent hydrophobic effect;
(2) The super-hydrophobic coating improves the corrosion resistance of the surface of the aluminum alloy;
(3) The super-hydrophobic coating obtained by the invention has excellent weather resistance;
(3) The method for preparing the super-hydrophobic coating does not use strong acid, strong alkali and fluorine-containing silane coupling agent, is green, nontoxic, simple and feasible, and is suitable for industrial expanded production.
Obviously, many modifications, substitutions, and variations are possible in light of the above teachings of the invention, without departing from the basic technical spirit of the invention, as defined by the following claims.
The present invention will be described in further detail with reference to the following examples. This should not be understood as limiting the scope of the above-described subject matter of the present invention to the following examples. All the technologies realized based on the above contents of the present invention belong to the scope of the present invention.
Drawings
FIG. 1: the process schematic diagram for preparing the super-hydrophobic PS/PDMS coating is shown in the specification.
FIG. 2: the invention relates to a surface topography of a super-hydrophobic PS/PDMS coating.
In FIG. 3: (a, b) schematic contact angle diagram; (c) water flow rebound photos; (d) The state of the coating in water and the surface adhesion condition after lifting; (e, f) horizontally dragging and vertically pulling the water drop on the surface of the coating layer, and detecting the adhesion condition of the water drop; (g) A video snapshot of the rolling behavior of a 10 μ L drop of water on the PS/PDMS coating.
FIG. 4: and testing results of electrochemical experiments.
FIG. 5 is a schematic view of: the morphology of water drops with different pH values on the coating surface is tested.
FIG. 6: and testing the water contact angle and the rolling angle of the coating after the coating is soaked in solutions with different pH values for 1h.
FIG. 7: and (5) high temperature resistance test results.
FIG. 8: TG test results.
FIG. 9: and (5) soaking in rain water to test results.
FIG. 10: DSC icing temperature test results.
FIG. 11: (a) Contact angles of the obtained coating samples at different amounts of SYLGARD 184silicone rubber added; (b) Contact angles of the obtained coating samples under different spraying times; (c) Contact angle and rolling angle of the obtained coating sample under different PS microsphere adding amount.
Detailed Description
The raw materials and equipment used in the invention are known products and are obtained by purchasing commercial products.
Commercially available SYLGARD 184silicone rubber (Dow chemical SYLGARD) TM 184Silicone Elastomer Kit) consists of the following two parts: polydimethylsiloxane (PDMS) and a curing agent, wherein the weight ratio of the PDMS to the curing agent is 10:1.
polystyrene microspheres (PS microspheres), available from Suzhou knoyi microsphere science and technology, are uniform in spherical shape (CV < 3%) and have a particle size of 5 μm.
EXAMPLE 1 preparation of fluorine-free Superhydrophobic coatings
(1) Pretreating the surface of the aluminum alloy: polishing with 1200# abrasive paper, and then cleaning with acetone;
(2) Weighing 0.22g SYLGARD 184silicone rubber, 3.0g PS microspheres and 40ml petroleum ether, performing ultrasonic treatment for 5min, and magnetically stirring for 10min to obtain a spraying liquid;
(3) Spraying the spraying liquid onto the surface of the pretreated aluminum alloy by using a spray gun, wherein the number of spraying layers is 8, the spraying pressure is 0.2MPa, and the distance from a nozzle to an aluminum alloy sample plate is 10cm; curing for 3h at 120 ℃ to obtain the super-hydrophobic PS/PDMS coating.
The process is schematically shown in FIG. 1, and the surface topography of the coating is shown in FIG. 2.
The beneficial effects of the present invention are demonstrated by the following experimental examples.
Experimental example 1 contact Angle and Rolling Angle test
1. Test sample
Example 1 made superhydrophobic PS/PDMS coating.
2. Experimental methods
The water Contact Angle (CA) and the rolling angle (SA) of the superhydrophobic PS/PDMS coating surface of example 1 were measured by the sitting drop method using a KrussDSA30 contact angle system (Germany) with a fitting method of Young-Laplace using water drops with volumes of 3. Mu.L and 10. Mu.L, respectively. The contact angle of water on the surface of the coating measured by the contact angle measuring instrument reflects the hydrophobicity of the coating, and each sample is measured 3 times at different positions and averaged.
3. Results of the experiment
As can be seen from FIG. 3, the surface contact angle of the superhydrophobic coating of example 1 reaches 158 degrees, and the rolling angle is 5.9 degrees, indicating that the coating has excellent hydrophobicity.
Experimental example 2 Corrosion resistance test
1. Test sample
Super hydrophobic PS/PDMS coating prepared in example 1.
2. Experimental methods
Drawing Tafel curves of the aluminum alloy without the coating and the aluminum alloy test plate coated with the PS/PDMS coating through an electrochemical experiment, and testing the improvement condition of the coating on the corrosion performance of the aluminum alloy; the electrolyte is 3.5 percent NaCl solution, and the saturated calomel electrode and the platinum electrode are respectively used as a reference electrode and an auxiliary electrode.
3. Results of the experiment
Electrochemical test results are shown in FIG. 4, and it can be seen that E of the aluminum alloy coated with the PS/PDMS coating is compared with the aluminum alloy not coated with the coating corr from-1.69V to-0.79V, and i corr From 1.99X 10 -7 A/cm 2 Becomes to 1.78 × 10 -8 A/cm 2 . The super-hydrophobic PS/PDMS coating has excellent corrosion resistance.
Example 3 weather resistance test
1. Test sample
Super hydrophobic PS/PDMS coating prepared in example 1.
2. Experimental methods
(1) The pH resistance test method comprises the following steps:
observing the shapes of water drops with different pH values on the surface of the coating; after immersing the coating in solutions of different pH for 1h, the water Contact Angle (CA) and the rolling angle (SA) of the coating were measured.
(2) The high temperature resistance test method comprises the following steps: and heating the oven to a set temperature, wherein the treatment time is 1h. The water contact angle and the sliding angle of the coating were measured after treatment at different temperatures.
TG test method: the instrument comprises: german stass 449F5, atmosphere: air; the heating rate is 5 ℃/min.
(3) The method for testing the soaked rainwater comprises the following steps: the coating was immersed in rain water in the Sichuan area using a conventional glass vessel and the water contact angle and the sliding angle of the coating were measured.
(4) DSC icing temperature test method: german relaxation resistant DSC214, atmosphere: nitrogen gas; the temperature change rate is 10 ℃/min.
3. Results of the experiment
(1) Results of pH resistance test
The results of the morphological tests of water drops of different pH on the coating surface are shown in fig. 5. The results of the water contact angle and the sliding angle test after the coating is soaked in the solutions with different pH values for 1h are shown in FIG. 6. It can be seen that the liquid drops with different pH values can keep good contact state on the surface of the coating, and can still keep excellent hydrophobicity and good stability after being soaked.
(2) Results of high temperature test and TG test
The results of the high temperature test are shown in fig. 7, and it can be seen that the coating can still maintain excellent hydrophobicity at a temperature as high as 240 ℃.
The TG test results are shown in fig. 8, and it can be seen that the initial failure temperature of the coating is as high as 277.2 ℃.
(3) Test results of soaking in rain
The test result of the soaked rainwater is shown in fig. 9, and it can be seen that the rolling angle of the coating is larger than 10 degrees after the coating is soaked in rainwater for 2 days in the Sichuan area; after 20 days of soaking, the contact angle is still more than 150 degrees.
(4) DSC icing temperature test results
The DSC icing temperature test result is shown in figure 10, and the crystallization temperature is changed from-20.01 ℃ to-23.04 ℃ after the aluminum dry pot is coated with the coating, which shows that the coating can effectively prolong the icing time on the surface.
The experimental results show that the super-hydrophobic PS/PDMS coating can keep excellent hydrophobicity after being soaked in solutions with different pH values and being soaked in rainwater at the temperature of 240 ℃; in addition, the super-hydrophobic PS/PDMS coating can effectively prolong the icing time on the surface. The super-hydrophobic PS/PDMS coating has excellent weather resistance.
Experimental example 4 screening experiment for preparing super-hydrophobic coating
1. Experimental methods
With reference to the method of example 1, 20 coating samples were prepared according to table 1 with varying PS microsphere addition, SYLGARD 184silicone rubber addition and spray times: PS-PDMS1-PS-PDMS20.
The surfaces of PS-PDMS1-PS-PDMS20 were tested for water Contact Angle (CA) and rolling angle (SA) according to the method of Experimental example 1.
TABLE 1.20 formulation and spray times for the coating samples
2. Results of the experiment
The test results are shown in fig. 11. Fig. 11 (a) shows the contact angle of the PS-PDMS coating samples obtained with different amounts of SYLGARD 184silicone rubber added, and it can be seen that when the amount of SYLGARD 184silicone rubber added is 0.22g, the contact angle of the coating sample obtained is the largest and the hydrophobicity is the most excellent. Fig. 11 (b) shows the contact angle of the PS-PDM coating samples obtained at different spraying times, and it can be seen that the contact angle of the coating sample obtained is the largest and the hydrophobicity is the most excellent when the spraying times are 8. Fig. 11 (c) shows the contact angle and the rolling angle of the PS-PDMS coating samples obtained under different PS microsphere addition amounts, and it can be seen that when the PS microsphere addition amount is 3.0g, the contact angle of the obtained coating sample is the largest, the rolling angle is the smallest, and the hydrophobicity is the best.
The results show that when the raw material formula is 0.22g SYLGARD 184silicon rubber, 3.0g PS microspheres and 40ml petroleum ether, and the spraying times are 8 times, the hydrophobic property of the obtained PS-PDMS coating is optimal.
In conclusion, the invention provides a fluorine-free super-hydrophobic coating composition and a super-hydrophobic coating. The super-hydrophobic coating not only has excellent hydrophobic effect, but also has excellent corrosion resistance and weather resistance. The method for preparing the super-hydrophobic coating does not use strong acid, strong alkali and fluorine-containing silane coupling agent, is green, nontoxic, simple and feasible, and is suitable for industrial expanded production.
Claims (10)
1. A fluorine-free super-hydrophobic coating composition is characterized in that: it comprises the following components: the silicone rubber-polystyrene microsphere comprises silicone rubber, polystyrene microspheres and a solvent, wherein the weight ratio of the silicone rubber to the polystyrene microspheres is (0.10-1.1): (0.5-4.0).
2. The fluorine-free superhydrophobic coating composition according to claim 1, characterized in that: the weight ratio of the silicon rubber to the polystyrene microspheres is 0.22:3.0.
3. the fluorine-free superhydrophobic coating composition according to claim 1, characterized in that: the content of the polystyrene microspheres is (0.5-4.0): 40g/ml, preferably 3.0:40g/ml.
4. The fluorine-free superhydrophobic coating composition according to any one of claims 1-4, characterized in that: the silicone rubber is SYLGARD 184silicone rubber.
5. The fluorine-free superhydrophobic coating composition according to any one of claims 1-4, characterized in that: the particle size of the polystyrene microsphere is 1-10 μm, preferably 5 μm; and/or the solvent is petroleum ether.
6. A method for preparing a fluorine-free super-hydrophobic coating is characterized by comprising the following steps: the method comprises the following steps:
(1) Pretreating the surface of the base material: polishing with sand paper, and cleaning with organic solvent;
(2) Formulating the fluorine-free superhydrophobic coating composition of any one of claims 1-5 as a spray coating liquid;
(3) And (3) spraying the spraying liquid on the surface of the base material pretreated in the step (1), and curing to obtain the fluorine-free super-hydrophobic coating.
7. The method of claim 6, wherein: in the step (1), the base material is a metal base material, preferably an aluminum alloy base material; and/or the organic solvent is one or the mixture of two of ethanol and acetone.
8. The method according to any one of claims 6 to 7, wherein: in the step (3), the number of sprayed layers is 2-10, the spraying pressure is 0.1-1.0 MPa, and the distance from the nozzle to the base material is 5-20 cm during spraying; the curing temperature is 100-140 ℃, and the curing time is 2-4 h;
preferably, in the step (3), the number of the coating layers is 8, the spraying pressure is 0.2MPa, and the distance from the nozzle to the substrate is 10cm during spraying; the curing temperature is 120 ℃ and the curing time is 3h.
9. The fluorine-free super-hydrophobic coating prepared by the method of any one of claims 6 to 8.
10. A fluorine-free super-hydrophobic material is characterized in that: comprising the fluorine-free superhydrophobic coating of claim 9.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103570251A (en) * | 2012-08-01 | 2014-02-12 | 青岛大学 | Preparation method of insulating super-hydrophobic coating |
| CN104231916A (en) * | 2014-09-30 | 2014-12-24 | 东南大学 | Transparent super-hydrophobic nano-coating and spraying and preparation method thereof |
| US20190256722A1 (en) * | 2016-09-06 | 2019-08-22 | The Regents Of The University Of Michigan | Durable superhydrophobic surfaces |
| CN114276751A (en) * | 2021-12-24 | 2022-04-05 | 中国大唐集团科学技术研究院有限公司中南电力试验研究院 | Preparation method and application of substrate-unlimited super-hydrophobic coating |
| CN114686076A (en) * | 2022-04-08 | 2022-07-01 | 哈尔滨工业大学 | Super-hydrophobic nano composite material coating with excellent mechanical stability and preparation method thereof |
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- 2022-09-27 CN CN202211182856.6A patent/CN115537076A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103570251A (en) * | 2012-08-01 | 2014-02-12 | 青岛大学 | Preparation method of insulating super-hydrophobic coating |
| CN104231916A (en) * | 2014-09-30 | 2014-12-24 | 东南大学 | Transparent super-hydrophobic nano-coating and spraying and preparation method thereof |
| US20190256722A1 (en) * | 2016-09-06 | 2019-08-22 | The Regents Of The University Of Michigan | Durable superhydrophobic surfaces |
| CN114276751A (en) * | 2021-12-24 | 2022-04-05 | 中国大唐集团科学技术研究院有限公司中南电力试验研究院 | Preparation method and application of substrate-unlimited super-hydrophobic coating |
| CN114686076A (en) * | 2022-04-08 | 2022-07-01 | 哈尔滨工业大学 | Super-hydrophobic nano composite material coating with excellent mechanical stability and preparation method thereof |
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