Preparation method of anti-icing super-hydrophobic material

By using blast furnace slag powder and steel slag powder to prepare superhydrophobic coatings, the problems of expensive equipment and poor coating stability in existing technologies have been solved, realizing low-cost and simple preparation of superhydrophobic coatings and improving the anti-icing performance and mechanical stability of wind turbine blades.

CN118359985BActive Publication Date: 2026-04-28XINJIANG UNIVERSITY
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Patent Information

Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
XINJIANG UNIVERSITY
Filing Date
2024-04-19
Publication Date
2026-04-28

AI Technical Summary

Technical Problem

Existing technologies for preparing superhydrophobic coatings suffer from problems such as expensive equipment, complex procedures, serious environmental pollution, and poor mechanical stability of the coatings, making it difficult to apply them on a large scale in practical engineering. Furthermore, icing on wind turbine blades affects the stability and efficiency of the system.

Method used

Superhydrophobic coatings were prepared by using blast furnace slag powder and steel slag powder as superhydrophobic fillers, through modification treatment and spraying method. Two-component polyurea was used as a binder to simplify the preparation process, reduce costs and improve the wear resistance of the coating.

Benefits of technology

A low-cost and simple superhydrophobic coating preparation method has been achieved, which has excellent wear resistance, effectively prevents icing of wind turbine blades, and improves system stability and efficiency.

✦ Generated by Eureka AI based on patent content.

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Abstract

The application discloses a kind of anti-icing super-hydrophobic material preparation methods, with aluminum plate as substrate;First, blast furnace slag powder and steel slag powder are treated with hydrophobic modification, blast furnace slag powder and steel slag powder are mixed according to certain mass ratio, mixed powder and organic solvent A absolute ethyl alcohol are stirred in round bottom flask, after solution is fully mixed, organic solvent B seventeen fluorine decyl triethoxysilane is added and transferred to water bath heating tank water bath heating and stirring;Modified blast furnace slag-steel slag powder, organic solvent C butyl acetate are uniformly mixed according to 3:8 ratio, after reaction ten minutes, two-component polyurea is added drop by drop, and super-hydrophobic coating is obtained by drying.The present application uses blast furnace slag waste as main raw material, adds a small amount of steel slag to improve the wear resistance of coating, uses two-component polyurea as adhesive, uses modified-spraying two-step method, without large instrument equipment, and super-hydrophobic coating with excellent wear resistance is prepared simply and quickly.
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Description

Technical Field

[0001] This invention relates to the field of superhydrophobic functional materials technology, and in particular to a method for preparing an anti-icing superhydrophobic material. Background Technology

[0002] Wind power, as a clean and renewable energy source, has seen significant development in China in recent years. Wind power is characterized by its green and environmentally friendly nature and wide distribution. As a key component of my country's clean energy development, it possesses significant advantages and a clear development trend. However, in extreme cold winter weather, ice can form on the surface of wind turbine blades. Icing can affect the stability of the entire wind power system, causing mechanical vibration and damage. Icing also reduces the aerodynamic efficiency of the wind turbine, lowering its power generation efficiency.

[0003] As a major energy producer, my country generates a huge amount of blast furnace slag waste from mineral smelting. Blast furnace slag and steel slag are rich in many components such as titanium oxide, silicon oxide, aluminum oxide, magnesium oxide, and iron oxide. In addition, steel slag powder has excellent wear resistance and has certain utilization value. Without a suitable method to utilize it, it will lead to resource waste.

[0004] Currently, laser processing technology is commonly used to construct micro- and nano-rough structures, and chemical etching, magnetron sputtering, and electrospinning are used to prepare superhydrophobic coatings. However, these methods are complex, and equipment such as electrospinning machines and femtosecond lasers are expensive, requiring harsh preparation environments and lengthy procedures. Moreover, chemical etching causes serious environmental pollution. These factors limit the large-scale application of superhydrophobic self-cleaning coatings in practical engineering.

[0005] Conventional superhydrophobic coatings use modified silica as filler and epoxy resin and PDMS as binders. These coatings have poor mechanical stability, and after wear, the contact angle decreases significantly, thus losing their superhydrophobic properties. Summary of the Invention

[0006] The technical problem to be solved by the present invention is to overcome the defects of the prior art and provide a method for preparing anti-icing superhydrophobic materials.

[0007] To address the aforementioned technical problems, the present invention provides the following technical solution:

[0008] This invention discloses a method for preparing an anti-icing superhydrophobic material, the specific steps of which are as follows:

[0009] Step 1: Preparation of hydrophobic modified blast furnace slag powder: Blast furnace slag powder and steel slag powder are used as superhydrophobic fillers. After mixing the blast furnace slag powder and steel slag powder, the mixed powder and organic solvent A (anhydrous ethanol) are added to a round-bottom flask and stirred for 10 minutes. After the solution is fully mixed, organic solvent B (heptadecyltriethoxysilane) is added, and the mixture is transferred to a water bath for heating and stirring to allow it to react fully. After the reaction is completed, the modified blast furnace slag-steel slag powder is obtained by filtration.

[0010] Step 2: Drying treatment: Place the modified blast furnace slag-steel slag powder obtained in Step 1 in an oven to ensure complete drying, and take it out for later use. During the drying process, avoid any moisture entering in order to maintain the hydrophobicity of the powder.

[0011] Step 3: Preparation of coating mixture: The dried modified blast furnace slag-steel slag powder obtained in step 2 is mixed with organic solvent C butyl acetate in a ratio of 3:8 at room temperature. After the reaction, the two-component polyurea is added dropwise and stirred until completely mixed to obtain a mixed liquid.

[0012] Step 4: Spraying and drying: Transfer the mixed liquid obtained in step 3 to a spray bottle and spray it onto the substrate. After spraying, dry it in an oven to obtain a superhydrophobic coating.

[0013] As a preferred embodiment of the present invention, in step 1, the mixed powder formed by mixing blast furnace slag powder and steel slag powder is mixed with anhydrous ethanol of organic solvent A in a ratio of 1:5, and the ratio of anhydrous ethanol of organic solvent A to organic solvent B heptadecafluorodecyltriethoxysilane is 2:1.

[0014] As a preferred embodiment of the present invention, the water bath temperature of the water bath heating tank in step 1 is 45°C, and the reaction time is 3 hours.

[0015] As a preferred embodiment of the present invention, the oven temperature in steps 2 and 4 is set to 70°C and the drying time is set to 6 hours.

[0016] As a preferred technical solution of the present invention, in step 4, the substrate is an aluminum plate, and the aluminum plate is polished with sandpaper of 300 grit or higher to remove dirt and clean the surface residue. It can be used after being completely dried.

[0017] Compared with the prior art, the beneficial effects of the present invention are as follows:

[0018] This invention uses blast furnace slag waste as the main raw material, adds a small amount of steel slag to improve the wear resistance of the coating, uses two-component polyurea as a binder, and adopts a two-step modification-spraying method. It can easily and quickly prepare a superhydrophobic coating with excellent wear resistance without the need for large-scale instruments and equipment, which saves costs and promotes resource recycling. Attached Figure Description

[0019] The accompanying drawings are provided to further illustrate the invention and form part of the specification. They are used in conjunction with embodiments of the invention to explain the invention and do not constitute a limitation thereof. In the drawings:

[0020] Figure 1 This is a flowchart of the steps of the present invention;

[0021] Figure 2 This is a comparison diagram of the contact angle of the coating and the contact angle after friction in Example 1;

[0022] Figure 3 This is a comparison diagram of the coating contact angle and the contact angle after friction in Example 2;

[0023] Figure 4 This is a comparison diagram of the coating contact angle and the contact angle after friction in Example 3;

[0024] Figure 5 This is a comparison diagram of the coating contact angle and the contact angle after friction in Example 4;

[0025] Figure 6 This is a comparison diagram of the coating contact angle and the contact angle after friction in Example 5;

[0026] Figure 7 This is a comparison chart of contact angles before and after friction in each embodiment; Detailed Implementation

[0027] The preferred embodiments of the present invention will be described below with reference to the accompanying drawings. It should be understood that the preferred embodiments described herein are for illustration and explanation only and are not intended to limit the present invention.

[0028] Example 1

[0029] like Figure 1 , 2 As shown in Figure 7, this invention provides a method for preparing an anti-icing superhydrophobic material, based on blast furnace slag powder and steel slag powder as superhydrophobic materials. The specific steps are as follows:

[0030] Step 1: Weigh 5g of blast furnace slag powder and 25ml of anhydrous ethanol into a round-bottom flask A1. Stir for 10 minutes until the solution is completely mixed. Place the round-bottom flask A1 into a constant temperature water bath, set the water bath temperature to 45℃ and stir continuously. During this process, add 10g of heptadecafluorodecyltriethoxysilane dropwise and react for 3 hours.

[0031] Step 2: Filter the product after the reaction and dry it in a 70℃ oven for 6 hours. After complete drying, modified blast furnace slag powder is obtained. Organic solvent A (anhydrous ethanol) and organic solvent B...

[0032] Step 3: Weigh 5g of modified blast furnace slag powder and 13.3g of butyl acetate solution into beaker A1, stir at room temperature for 10 minutes until the solution is completely mixed, and add 5g of two-component polyurea dropwise. The mass ratio of component A (anhydrous ethanol) to component B (heptadecyltriethoxysilane) is 2:1. After the solution is completely mixed, transfer it to the spray gun's spray bottle, set the air compressor pressure to 0.6MPa, and the distance between the spray gun and the aluminum plate to about 15cm for spraying.

[0033] Step 4: Transfer the coated aluminum plate to an oven, set the temperature to 70℃, and dry for 6 hours. Remove it after it is completely dry.

[0034] The superhydrophobic coating prepared in Example 1 was tested, and the contact angle was measured using an optical contact angle meter. The droplet volume was set to 3 μL. Figure 2 (a) clearly shows a contact angle of 159.5°, indicating that the coating has extremely strong hydrophobic properties. A friction test was conducted by pressing a 500g weight onto an aluminum plate coated with the superhydrophobic layer and dragging it back and forth on 300-grit sandpaper 50 times. The results after the abrasion resistance test showed that... Figure 2 As can be seen from (b), the average contact angle is 141.6°; no obvious icing phenomenon was observed when the aluminum plate was placed at -10°C.

[0035] Example 2

[0036] like Figure 1 , 3 As shown in Figure 7, this invention provides a method for preparing an anti-icing superhydrophobic material, based on blast furnace slag powder and steel slag powder as superhydrophobic materials. The specific steps are as follows:

[0037] Step 1: Weigh 4g of blast furnace slag powder, 1g of steel slag powder, and 25ml of anhydrous ethanol into a round-bottom flask A2. Stir for 10 minutes until the solution is completely mixed. Place the round-bottom flask A2 into a constant temperature water bath, set the water bath temperature to 45℃ and stir continuously. During this process, add 10g of heptadecafluorodecyltriethoxysilane dropwise and react for 3 hours.

[0038] Step 2: Filter the product after the reaction is complete and dry it in an oven at 70℃ for 6 hours. After it is completely dried, the modified blast furnace slag-steel slag powder is obtained.

[0039] Step 3: Weigh 5g of modified blast furnace slag-steel slag powder and 13.3g of butyl acetate solution into beaker A, stir at room temperature for 10 minutes until the solution is completely mixed, and add 5g of two-component polyurea dropwise. The mass ratio of component A (anhydrous ethanol) to component B (heptadecyltriethoxysilane) is 2:1. After the solution is completely mixed, transfer it to the spray gun's spray bottle, set the air compressor pressure to 0.6MPa, and the distance between the spray gun and the aluminum plate to about 15cm for spraying.

[0040] Step 4: Transfer the coated aluminum plate to an oven, set the temperature to 70℃, and dry for 6 hours. Remove it after it is completely dry.

[0041] The superhydrophobic coating prepared in Example 2 was tested under the same test conditions as in Example 1. The contact angle was measured before friction as follows: Figure 3 (a) shows 157.6°; an aluminum plate with a superhydrophobic coating was compacted using a 500g weight and dragged back and forth on 300-grit sandpaper 50 times for a friction test. The results after the abrasion test were obtained. Figure 3 As can be seen from (e), the average contact angle is 141.9°; no obvious icing phenomenon was observed when the aluminum plate was placed at -10°C.

[0042] Example 3

[0043] like Figure 1 , 4 As shown in Figure 7, this invention provides a method for preparing an anti-icing superhydrophobic material, based on blast furnace slag powder and steel slag powder as superhydrophobic materials. The specific steps are as follows:

[0044] Step 1: Weigh 3g of blast furnace slag powder, 2g of steel slag powder, and 25ml of anhydrous ethanol into a round-bottom flask A3. Stir for 10 minutes until the solution is completely mixed. Place the round-bottom flask A3 into a constant temperature water bath, set the water bath temperature to 45℃ and stir continuously. During this process, add 10g of heptadecafluorodecyltriethoxysilane dropwise and react for 3 hours.

[0045] Step 2: Filter the product after the reaction is complete and dry it in an oven at 70℃ for 6 hours. After it is completely dried, the modified blast furnace slag-steel slag powder is obtained.

[0046] Step 3: Weigh 5g of modified blast furnace slag-steel slag powder and 13.3g of butyl acetate solution into beaker A, stir at room temperature for 10 minutes until the solution is completely mixed, and add 5g of two-component polyurea dropwise. The mass ratio of component A (anhydrous ethanol) to component B (heptadecyltriethoxysilane) is 2:1. After the solution is completely mixed, transfer it to the spray gun's spray bottle, set the air compressor pressure to 0.6MPa, and the distance between the spray gun and the aluminum plate to about 15cm for spraying.

[0047] Step 4: Transfer the coated aluminum plate to an oven, set the temperature to 70℃, and dry for 6 hours. Remove it after it is completely dry.

[0048] The superhydrophobic coating prepared in Example 3 was tested under the same test conditions as in Example 1. The contact angle was measured before friction as follows: Figure 4(b) shows 152.6°; an aluminum plate with a superhydrophobic coating was compacted using a 500g weight and dragged back and forth on 300-grit sandpaper 50 times for a friction test. The results after the abrasion test were measured. Figure 4 As can be seen from (f), the average contact angle is 149.7°; no obvious icing phenomenon was observed when the aluminum plate was placed at -10℃.

[0049] Example 4

[0050] like Figure 1 , 5 As shown in Figure 7, this invention provides a method for preparing an anti-icing superhydrophobic material, based on blast furnace slag powder and steel slag powder as superhydrophobic materials. The specific steps are as follows:

[0051] Step 1: Weigh 1g of blast furnace slag powder, 4g of steel slag powder, and 25ml of anhydrous ethanol into a round-bottom flask A4. Stir for 10 minutes until the solution is completely mixed. Place the round-bottom flask A4 into a constant temperature water bath, set the water bath temperature to 45℃ and stir continuously. During this process, add 10g of heptadecafluorodecyltriethoxysilane dropwise and react for 3 hours.

[0052] Step 2: Filter the product after the reaction is complete and dry it in an oven at 70℃ for 6 hours. After it is completely dried, the modified blast furnace slag-steel slag powder is obtained.

[0053] Step 3: Weigh 5g of modified blast furnace slag-steel slag powder and 13.3g of butyl acetate solution into beaker A, stir at room temperature for 10 minutes until the solution is completely mixed, and add 5g of two-component polyurea dropwise. The mass ratio of component A (anhydrous ethanol) to component B (heptadecyltriethoxysilane) is 2:1. After the solution is completely mixed, transfer it to the spray gun's spray bottle, set the air compressor pressure to 0.6MPa, and the distance between the spray gun and the aluminum plate to about 15cm for spraying.

[0054] Step 4: Transfer the coated aluminum plate to an oven, set the temperature to 70℃, and dry for 6 hours. Remove it after it is completely dry.

[0055] The superhydrophobic coating prepared in Example 4 was tested under the same test conditions as in Example 1. The contact angle was measured before friction as follows: Figure 5 (c) shows 98°; an aluminum plate with a superhydrophobic coating was compacted using a 500g weight and dragged back and forth on 300-grit sandpaper 50 times for a friction test. The results after the abrasion test were measured. Figure 5 As can be seen from (g), the average contact angle is 94.8°. Obviously, the coating prepared at this ratio does not have superhydrophobic properties, and the aluminum plate will freeze severely when placed at -10°C.

[0056] Example 5

[0057] like Figure 6 and 7 As shown, as a comparative group, this embodiment provides a method for preparing a hydrophobic silica superhydrophobic self-cleaning material based on silica as a superhydrophobic material, including the following steps:

[0058] Step 1: Weigh 5g of silica powder with a particle size of 500nm and 25ml of anhydrous ethanol into a round-bottom flask A5. Stir for 10 minutes until the solution is completely mixed. Place the round-bottom flask A5 into a constant temperature water bath, set the water bath temperature to 45℃ and stir continuously. During this process, add 10g of heptadecafluorodecyltriethoxysilane dropwise and react for 3 hours.

[0059] Step 2: Filter the product after the reaction is complete and dry it in an oven at 70°C for 6 hours. After it is completely dried, the modified silica powder is obtained.

[0060] Step 3: Weigh 5g of modified silica powder and 13.3g of butyl acetate solution into beaker A, stir at room temperature for 10 minutes until the solution is completely mixed, add 5g of PDMS curing agent drop by drop, and after the solution is completely mixed, transfer it to the spray bottle of the spray gun. Set the air compressor pressure to 0.6Mpa, and the distance between the spray gun and the aluminum plate to about 15cm, and carry out the spraying operation.

[0061] Step 4: Transfer the coated aluminum plate to an oven, set the temperature to 70℃, and dry for 6 hours. Remove it after it is completely dry.

[0062] The hydrophobic coating prepared in Example 5 was tested under the same test conditions as in Example 1. The contact angle was measured before friction as follows: Figure 6 (d) shows 156.6°; an aluminum plate with a superhydrophobic coating was compacted using a 500g weight and dragged back and forth on 300-grit sandpaper 50 times for a friction test. The results after the abrasion resistance test were obtained. Figure 6 As can be seen from (h), the average contact angle is only 76.2°. Obviously, the coating does not have superhydrophobic properties, and the aluminum plate will freeze severely when placed at -10°C.

[0063] The results of the above five implementation examples show that, as Figure 7 As shown, the friction resistance is optimal when the mass ratio of blast furnace slag powder to steel slag powder is 3:2, with almost no impact on the anti-icing effect. The friction resistance is partially affected when the mass ratio is 4:1 or when there is no steel slag powder, but the anti-icing effect is still achieved. Both hydrophobicity and friction resistance are affected when the mass ratio is 1:4. While superhydrophobic coatings using silica as filler and PDMS as curing agent have a high contact angle, their wear resistance is extremely poor and they cannot maintain mechanical stability for long.

[0064] Finally, it should be noted that the above descriptions are merely preferred embodiments of the present invention and are not intended to limit the present invention. Although the present invention has been described in detail with reference to the foregoing embodiments, those skilled in the art can still modify the technical solutions described in the foregoing embodiments or make equivalent substitutions for some of the technical features. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present invention should be included within the protection scope of the present invention.

Claims

1. A method for preparing an anti-icing superhydrophobic material, characterized in that, The specific steps are as follows: Step 1: Preparation of modified blast furnace slag-steel slag powder: Blast furnace slag powder and steel slag powder are used as superhydrophobic fillers. After mixing blast furnace slag powder and steel slag powder in a mass ratio of 3:2, the mixed powder and organic solvent A (anhydrous ethanol) are added to a round bottom flask and stirred for 10 minutes. After the solution is fully mixed, organic solvent B (heptadecyltriethoxysilane) is added, and the mixture is transferred to a water bath for heating and stirring to allow it to react fully. After the reaction is completed, the modified blast furnace slag-steel slag powder is obtained by filtration. Step 2: Drying treatment: Place the modified blast furnace slag-steel slag powder obtained in Step 1 in an oven to ensure complete drying, and take it out for later use. During the drying process, avoid any moisture entering in order to maintain the hydrophobicity of the powder. Step 3: Preparation of coating mixture: The dried modified blast furnace slag-steel slag powder obtained in step 2 is mixed with organic solvent C butyl acetate in a ratio of 3:8 at room temperature. After the reaction, the two-component polyurea is added dropwise and stirred until completely mixed to obtain a mixed liquid. Step 4: Spraying and drying: Transfer the mixed liquid obtained in step 3 to a spray bottle and spray it onto the substrate. After spraying, dry it in an oven to obtain the anti-icing superhydrophobic material. In step 1, the mixed powder formed by mixing blast furnace slag powder and steel slag powder is mixed with anhydrous ethanol of organic solvent A in a ratio of 1:5, and the ratio of anhydrous ethanol of organic solvent A to organic solvent B heptadecafluorodecyltriethoxysilane is 2:

1. In step 1, the water bath temperature of the water bath heating tank is 45°C, and the reaction time is 3 hours. The oven temperature is set to 70℃ and the drying time is 6 hours in both steps 2 and 4.

2. The method for preparing an anti-icing superhydrophobic material according to claim 1, characterized in that, In step 4, the substrate is an aluminum plate, which is sanded with sandpaper of 300 grit or higher to remove dirt and clean the surface residue. It is then used after being completely dry.

Citation Information

Patent Citations

  • Wear-resisting super-hydrophobic coating composition as well as preparation method and application thereof

    CN107987675A