A silicone resin anti-icing coating material and its preparation method

Abstract

The present invention belongs to the technical field of chemical coatings, and discloses a silicone resin anti-icing coating material and a preparation method thereof. The anti-icing coating material is composed of the following components in terms of mass percentage: 20% - 50% of silicone resin, 15% - 30% of hydrophobic nano-Al(OH)3, 3% - 6% of hydrophobic nano-SiO2, 25% - 45% of diluent, 0.1% - 5% of coupling agent, and 0.7% - 11.5% of auxiliary agent. The preparation method includes: after preparing the hydrophobic nano-Al(OH)3 material, the silicone resin, diluent, hydrophobic nano-Al(OH)3, hydrophobic nano-SiO2, auxiliary agent, and coupling agent are sequentially mixed, dispersed and ground, and then filtered to obtain the anti-icing coating material. During the preparation process of the present invention, heating is not required, which is environmentally friendly and energy-saving. The component ratio is reasonable, the cost is saved, the preparation method is simple, and large-scale production is easy to achieve.

Description

Technical Field

[0001] The present invention belongs to the technical field of chemical coatings, and relates to a silicone resin anti-icing coating material and a preparation method thereof. Background Art

[0002] Icing on aircraft, wind power equipment, transmission lines, etc. will affect work efficiency, cause property losses, and even threaten life safety. Traditional anti-icing measures include thermal de-icing, mechanical de-icing, chemical de-icing, etc., but they have the disadvantages of low efficiency, high energy consumption, and high maintenance costs. Structural damage may also be caused to the object surface during the mechanical de-icing process. The excellent liquid repellency of superhydrophobic coatings endows the coatings with outstanding self-cleaning characteristics. Using superhydrophobic coatings can effectively curb the surface icing phenomenon, and at the same time has the advantages of low energy consumption and low pollution, making it have broad application prospects in places such as the outer surface of buildings, automobile windshields, solar baffles, etc., and is favored by researchers in the anti-icing field.

[0003] However, in the actual application of existing superhydrophobic coatings, the micro-nano structure and chemical coating of the superhydrophobic surface will cause the failure of ice repellency due to wear and aging, and the lubricating fluid inside the superlubricating surface will also be lost due to factors such as gravity and temperature, resulting in the failure of ice repellency. Moreover, most of the existing bionic anti-icing surfaces can only exhibit good ice repellency under specific conditions in the laboratory. Under low temperature and high humidity conditions, the ice repellency will be greatly reduced and is easily affected by environmental factors. Therefore, it is necessary to enhance the durability and stability of bionic anti-icing surfaces through multiple channels. Summary of the Invention

[0004] In view of the problems and deficiencies of the prior art, the present invention provides a silicone resin anti-icing coating material and a preparation method thereof.

[0005] Based on the above purpose, the present invention adopts the following technical solutions:

[0006] In the first aspect, a preparation method of a hydrophobic nano-Al(OH)3 material includes the following steps:

[0007] Add nano-Al(OH)3 powder into absolute ethanol, mix evenly to obtain a nano-Al(OH)3 sol-gel, then add 1,1,2,2,3,3,4,4,5,5,6,6,7,7,7-heptadecafluorodecyltriethoxysilane and stearic acid into the nano-Al(OH)3 sol-gel and disperse evenly to obtain a nano-Al(OH)3 sol-gel mixture. Dry and grind the nano-Al(OH)3 sol-gel mixture through a sieve to obtain the hydrophobic nano-Al(OH)3 material.

[0008] Preferably, in the nano-Al(OH)3 sol-gel mixture, the content of nano-Al(OH)3 is 31% - 36%, the content of absolute ethanol is 60% - 65%, the content of heptadecafluorodecyltriethoxysilane is 0.5% - 1.5%, and the content of stearic acid is 2% - 3%.

[0009] Further, the dispersion temperature is 25 5 °C.

[0010] Further, the dispersion speed is 1200 - 1500 r / min, and the duration is 1.5 - 2 h.

[0011] Further, the drying temperature is 60 - 100 °C, and the duration is 3 - 6 h.

[0012] In the second aspect, the present invention provides a hydrophobic nano-Al(OH)3 material prepared by the preparation method of the first aspect above.

[0013] In the third aspect, the present invention provides the application of the hydrophobic nano-Al(OH)3 material in coatings.

[0014] In the fourth aspect, the present invention provides a silicone resin anti-icing coating material, which is composed of the following components by mass percentage: silicone resin 20% - 50%, hydrophobic nano-Al(OH)3 15% - 30%, hydrophobic nano-SiO2 3% - 6%, diluent 25% - 45%, coupling agent 0.1% - 5%, and auxiliary agent 0.7% - 11.5%.

[0015] Preferably, the average particle size of the hydrophobic nano-Al(OH)3 and hydrophobic nano-SiO2 is 100 nm.

[0016] Preferably, the silicone resin is SJ-509.

[0017] Preferably, the diluent is RY306.

[0018] Preferably, the coupling agent is BYK173.

[0019] Preferably, the auxiliary agent is a defoaming agent, a dispersing agent, and a smoothing agent.

[0020] Preferably, the silicone resin anti-icing coating material is composed of the following components by mass percentage: silicone resin 20% - 50%, hydrophobic nano-Al(OH)3 15% - 30%, hydrophobic nano-SiO2 3% - 6%, diluent 25% - 45%, coupling agent 0.1% - 5%, defoaming agent 0.1% - 5%, dispersing agent 0.1% - 5%, and smoothing agent 0.5% - 1.5%.

[0021] More preferably, the defoaming agent is a silicone defoaming agent.

[0022] More preferably, the dispersant is BYK163.

[0023] More preferably, the smoothing agent is wax powder.

[0024] Fifthly, the present invention provides a preparation method of a silicone resin anti-icing coating material, comprising the following steps:

[0025] (1) Adding silicone resin into a diluent and dispersing evenly to obtain a first mixture;

[0026] (2) Adding hydrophobic nano-Al(OH)3 and hydrophobic nano-SiO2 into the first mixture and dispersing evenly to obtain a second mixture;

[0027] (3) Adding an auxiliary agent and a coupling agent into the second mixture, dispersing and grinding, and then filtering to obtain the silicone resin anti-icing coating material.

[0028] Further, the dispersion temperature is 25 5 °C.

[0029] Further, in step (1), the dispersion speed is 400-600 r / min and the duration is 10-15 min.

[0030] Further, in step (2), the dispersion speed is 800-1200 r / min and the duration is 30-60 min.

[0031] Further, in step (3), the dispersion speed is 1200-1500 r / min and the duration is 1-2 h.

[0032] Compared with the prior art, the beneficial effects of the present invention are as follows:

[0033] 1. During the modification process of nano-Al(OH)3 in the present invention, the adsorption of the heptadecafluorodecyl group in the organic molecule on the surface of the nano-Al(OH)3 powder, as well as free radical reactions and chelation reactions, etc. are used to coat and modify the particle surface, so that nano-Al(OH)3 obtains hydrophobic properties.

[0034] 2. The silicone resin anti-icing coating material of the present invention, by adding modified hydrophobic nano-Al(OH)3 and a reasonable ratio of other components, greatly increases the contact angle of water on the coating surface, achieving superhydrophobic properties, thereby realizing the anti-icing effect, and having good durability and stability.

[0035] 3. During the preparation process of the present invention, no heating is required, which is environmentally friendly and energy-saving. The component ratio is reasonable, the cost is saved, the preparation method is simple, and it is easy to realize large-scale production. Brief Description of the Drawings

[0036] Figure 1 It is a contact angle diagram of water on the surface of the coating material prepared in Example 2;

[0037] Figure 2 It is a contact angle diagram of water on the surface of the coating material prepared in Comparative Example 7. Detailed Description of the Invention

[0038] Example 1

[0039] A hydrophobic nano - Al(OH)3 material, and its preparation method includes the following steps:

[0040] (1) Add nano - Al(OH)3 powder into absolute ethanol to form a nano - Al(OH)3 sol - gel. Then add 1,1,2,2,3,3,4,4,5,5,6,6,7,7,7 - heptadecafluorodecyltriethoxysilane and stearic acid into the nano - Al(OH)3 sol - gel, and disperse with a disperser for 2 h at a rotation speed of 1500 r / min and a temperature of 25 5 °C to obtain a nano - Al(OH)3 sol - gel mixture. In the nano - Al(OH)3 sol - gel mixture, the content of nano - Al(OH)3 is 32.24%, the content of absolute ethanol is 64.48%, the content of 1,1,2,2,3,3,4,4,5,5,6,6,7,7,7 - heptadecafluorodecyltriethoxysilane is 1.13%, and the content of stearic acid is 2.15%.

[0041] (2) Dry the nano - Al(OH)3 sol - gel mixture at 80 °C for 3 h, then grind and sieve to obtain the hydrophobic nano - Al(OH)3.

[0042] Comparative Example 1

[0043] A hydrophobic nano - Al(OH)3 material, whose composition and preparation method are basically the same as those in Example 1, the difference is that in the nano - Al(OH)3 sol - gel mixture, the content of nano - Al(OH)3 is 31.1%, the content of absolute ethanol is 62.21%, the content of 1,1,2,2,3,3,4,4,5,5,6,6,7,7,7 - heptadecafluorodecyltriethoxysilane is 0.47%, and the content of stearic acid is 6.22%.

[0044] Comparative Example 2

[0045] A hydrophobic nano - Al(OH)3 material, whose composition and preparation method are basically the same as those in Example 1, the difference is that in the nano - Al(OH)3 sol - gel mixture, the content of nano - Al(OH)3 is 32%, the content of absolute ethanol is 64%, the content of 1,1,2,2,3,3,4,4,5,5,6,6,7,7,7 - heptadecafluorodecyltriethoxysilane is 0.8%, and the content of stearic acid is 3.2%.

[0046] Comparative Example 3

[0047] A hydrophobic nano - Al(OH)3 material, its composition and preparation method are basically the same as those of Example 1, the difference is that, among them, in the nano - Al(OH)3 sol - gel mixture, the content of nano - Al(OH)3 is 48.19%, the content of absolute ethanol is 48.19%, the content of heptadecafluorodecyltriethoxysilane is 1.2%, and the content of stearic acid is 2.41%.

[0048] Comparative Example 4

[0049] A hydrophobic nano - Al(OH)3 material, its composition and preparation method are basically the same as those of Example 1, the difference is that, among them, in the nano - Al(OH)3 sol - gel mixture, the content of nano - Al(OH)3 is 24.6%, the content of absolute ethanol is 73.8%, the content of heptadecafluorodecyltriethoxysilane is 0.62%, and the content of stearic acid is 0.98%.

[0050] Example 2

[0051] A silicone resin anti - icing coating material, by mass percentage, consists of the following components: silicone resin SJ - 509 30%, hydrophobic nano - Al(OH)3 20%, hydrophobic nano - SiO2 5%, diluent RY306 42%, organosilicon defoamer 0.5%, dispersant BYK163 0.5%, coupling agent BYK173 0.5%, wax powder 1.5%. Among them, the hydrophobic nano - Al(OH)3 is prepared from Example 1.

[0052] The preparation method of the above - mentioned silicone resin anti - icing coating material includes the following steps:

[0053] (1) Add silicone resin SJ - 509 into diluent RY306, disperse with a disperser for 10 min, the rotation speed is 400 r / min, and the temperature is 25 5 °C, to obtain the first mixture.

[0054] (2) Add hydrophobic nano - Al(OH)3 and hydrophobic nano - SiO2 into the first mixture in sequence, disperse with a disperser for 30 min, the rotation speed is 1200 r / min, and the temperature is 25 5 °C, to obtain the second mixture.

[0055] (3) Add dispersant BYK163, organosilicon defoamer, wax powder, and coupling agent BYK173 into the second mixture in sequence for mixing, then grind and disperse with a grinding disperser for 1 h, the rotation speed is 1200 r / min, and the temperature is 25 5 °C, and then filter to obtain the silicone resin anti - icing coating material.

[0056] Comparative Example 5

[0057] A silicone resin anti-icing coating material, whose composition and preparation method are basically the same as those of Example 2, except that the hydrophobic nano-Al(OH)3 is prepared from Comparative Example 1.

[0058] Comparative Example 6

[0059] A silicone resin anti-icing coating material, whose composition and preparation method are basically the same as those of Example 2, except that the hydrophobic nano-Al(OH)3 is prepared from Comparative Example 2.

[0060] Comparative Example 7

[0061] A silicone resin anti-icing coating material, whose composition and preparation method are basically the same as those of Example 2, except that the hydrophobic nano-Al(OH)3 is prepared from Comparative Example 3.

[0062] Comparative Example 8

[0063] A silicone resin anti-icing coating material, whose composition and preparation method are basically the same as those of Example 2, except that the hydrophobic nano-Al(OH)3 is prepared from Comparative Example 4.

[0064] The hydrophobic properties of the silicone resin anti-icing coating materials prepared in Example 2 and Comparative Examples 5-8 were detected using a contact angle tester, and the test results are shown in Table 1. The contact angle diagram of the coating material surface prepared in Example 2 is shown in Figure 1 , and the contact angle diagram of the coating material surface prepared in Comparative Example 7 is shown in Figure 2 .

[0065]

[0066] It can be seen from Table 1 that for the silicone resin anti-icing coating material prepared in Example 2, the contact angle of water on its surface reached 154°, showing superhydrophobic properties, which is close to the hydrophobic properties of the silicone resin anti-icing coating material prepared in Comparative Example 7. However, the dosage of nano-Al(OH)3 in Comparative Example 7 is 1.5 times that of Example 2, and the raw material cost is too high. For the silicone resin anti-icing coating materials prepared in Comparative Examples 5-6 and Comparative Example 8, the contact angle of water on their surfaces is less than 150°, and they do not show superhydrophobic properties. In summary, the silicone resin anti-icing coating material prepared in Example 2 can not only achieve superhydrophobic properties and realize the anti-icing effect, but also save costs, and its comprehensive performance is the best.

[0067] Comparative Example 9

[0068] A silicone resin anti-icing coating material, whose composition and preparation method are basically the same as those of Example 2, except that, by mass percentage, it is composed of the following components: silicone resin SJ-509 27%, hydrophobic nano-Al(OH)3 25%, hydrophobic nano-SiO2 2%, diluent RY306 43%, silicone defoamer 0.5%, dispersant BYK163 0.5%, coupling agent BYK173 0.5%, wax powder 1.5%.

[0069] Comparative Example 10

[0070] A silicone resin anti-icing coating material, whose composition and preparation method are basically the same as those of Example 2, except that, by mass percentage, it is composed of the following components: silicone resin SJ-509 30.15%, hydrophobic nano-Al(OH)3 22.1%, hydrophobic nano-SiO2 2.51%, diluent RY306 42.24%, silicone defoamer 0.5%, dispersant BYK163 0.5%, coupling agent BYK173 0.5%, wax powder 1.5%.

[0071] Comparative Example 11

[0072] A silicone resin anti-icing coating material, whose composition and preparation method are basically the same as those of Example 2, except that, by mass percentage, it is composed of the following components: silicone resin SJ-509 53.69%, hydrophobic nano-Al(OH)3 5.34%, hydrophobic nano-SiO2 6.61%, diluent RY306 30.85%, silicone defoamer 0.67%, dispersant BYK163 0.67%, coupling agent BYK173 0.67%, wax powder 1.5%.

[0073] Comparative Example 12

[0074] A silicone resin anti-icing coating material, whose composition and preparation method are basically the same as those of Example 2, except that, by mass percentage, it is composed of the following components: silicone resin SJ-509 40%, hydrophobic nano-Al(OH)3 10%, hydrophobic nano-SiO2 2%, diluent RY306 45%, silicone defoamer 0.5%, dispersant BYK163 0.5%, coupling agent BYK173 0.5%, wax powder 1.5%.

[0075] The hydrophobic properties of the silicone resin anti-icing coating materials prepared in Example 2 and Comparative Examples 9 to 12 were detected using a contact angle tester, and the detection results are shown in Table 2.

[0076]

[0077] As can be seen from Table 2, for the silicone resin anti-icing coating materials prepared in Comparative Examples 9 to 12, the contact angles of water on their surfaces are all less than 150°, and they do not exhibit superhydrophobic properties. In summary, the silicone resin anti-icing coating material prepared in Example 2 has the best hydrophobic property and the best anti-icing effect.

[0078] The stability test was carried out on the silicone resin anti-icing coating material prepared in Example 2. Among them, after reciprocating friction 300 times under 1000-mesh sandpaper and 2.3 KPA, the contact angle of water on its surface only decreased by ≤10°; after flushing for 2 min under a water pressure of 50 KPA, the contact angle of water on its surface only decreased by ≤11°; after standing outdoors for 50 days, the contact angle of water on its surface only decreased by ≤5°. In summary, the silicone resin anti-icing coating material prepared by the present invention has good durability and stability.

[0079] The above describes the preferred embodiments of the present invention, but it should be understood that the invention is not limited to the content disclosed herein. As long as non-substantial improvements are made by adopting the method concept and technical solution of the present invention, or the method concept and technical solution of the present invention are applied to other occasions, they are all within the protection scope of the present invention.

Claims

1. A silicone resin anti-icing coating material, characterized in that, It consists of the following components by mass percentage: 20% - 50% silicone resin, 15% - 30% hydrophobic nano - Al(OH)3, 3% - 6% hydrophobic nano - SiO2, 25% - 45% diluent, 0.1% - 5% coupling agent, 0.7% - 11.5% additives; the additives are at least one of defoaming agent, dispersant, and lubricant. The hydrophobic nano - Al(OH)3 is prepared by the following steps: adding nano - Al(OH)3 powder into absolute ethanol, mixing evenly to obtain a nano - Al(OH)3 solution, then adding 1,1,1,2,2,3,3,4,4,5,5,6,6 - heptadecafluorodecyltriethoxysilane and stearic acid into the nano - Al(OH)3 solution and dispersing evenly to obtain a nano - Al(OH)3 mixture, drying and grinding the nano - Al(OH)3 mixture and sieving it to obtain the hydrophobic nano - Al(OH)3 material; in the nano - Al(OH)3 mixture, the content of nano - Al(OH)3 is 31% - 36%, the content of absolute ethanol is 60% - 65%, the content of 1,1,1,2,2,3,3,4,4,5,5,6,6 - heptadecafluorodecyltriethoxysilane is 0.5% - 1.5%, and the content of stearic acid is 2% - 3%.

2. The silicone resin anti-icing coating material according to claim 1, characterized in that, It consists of the following components by mass percentage: 20% - 50% silicone resin, 15% - 30% hydrophobic nano - Al(OH)3, 3% - 6% hydrophobic nano - SiO2, 25% - 45% diluent, 0.1% - 5% coupling agent, 0.1% - 5% defoaming agent, 0.1% - 5% dispersant, 0.5% - 1.5% lubricant.

3. A method for preparing the silicone resin anti-icing coating material according to claim 1 or 2, characterized in that, It includes the following steps: (1) Adding silicone resin into the diluent and dispersing evenly to obtain a first mixture. (2) Adding hydrophobic nano - Al(OH)3 and hydrophobic nano - SiO2 into the first mixture and dispersing evenly to obtain a second mixture. (3) Adding additives and coupling agent into the second mixture, dispersing and grinding, and then filtering to obtain the coating.

4. The preparation method of the silicone resin anti-icing coating material according to claim 3, characterized in that, In step (1), the dispersion speed is 400 - 600 r / min, in step (2), the dispersion speed is 800 - 1200 r / min, and in step (3), the dispersion speed is 1200 - 1500 r / min.

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