WO2018223781A1 - Anti-icing coating and preparation method thereof - Google Patents

Abstract

A preparation method of an anti-icing coating comprises: mixing a vinyl-terminated silicone oil, a hydrogen-terminated silicone oil, a methyl silicone oil, Karstedt's catalyst, and silica nanoparticles, and removing bubbles to obtain a mixture (S1); making the mixture into a coating (S2); curing the coating to obtain an anti-icing coating (S3).

Description

Anti-icing coating and preparation method thereof Technical field

The invention relates to the field of composite materials, in particular to an anti-icing coating and a preparation method thereof.

Background technique

The phenomenon of ice coating such as precipitation and ice coating, sublimation and ice coating will bring great inconvenience to people's production and life, and will cause huge economic losses. Especially for the power system, not only will the transmission line be interrupted, but the tower will collapse and be broken. Etc. Even the transmission line will cause serious damage to the safe operation of the power system. China is one of the countries with serious ice-covered transmission lines, and the probability of line ice-covered accidents is among the highest in the world. In addition, railway line icing, wing icing, etc. may also pose a huge threat to people's lives and property. Therefore, the research on anti-icing materials has great social and economic value.

technical problem

So far, there have been some researches on anti-icing coatings in China. Most of the existing technologies are realized by preparing a superhydrophobic anti-icing coating. The superhydrophobic anti-icing coating refers to a coating having a surface contact angle of water of more than 150° and a falling angle of less than 10°. When the contact angle of the water droplet on the surface of the coating is large and the rolling angle is relatively small, the adhesion between the water droplet and the coating is much smaller than the adhesion between the water droplet and the general coating, and the water droplet is affected by the gravity. Automatically rolls off the surface of the coating to prevent ice from freezing on the surface of the coating. However, in a humid environment, when the superhydrophobic anti-icing coating is frozen, it will lose its original superhydrophobic property, and the adhesion strength of ice tends to be relatively large, making the difficulty of deicing more difficult. At the same time, after the anti-icing material is used for many times, the anti-icing performance is greatly reduced. Therefore, the existing anti-icing materials often have the disadvantages of poor anti-icing effect and poor durability.

Technical solution

In order to solve the problem that the existing anti-icing coating is difficult to remove after icing and the durability of the coating is poor, the present invention provides an anti-icing coating having low ice adhesion strength and a preparation method thereof.

The method for preparing an anti-icing coating provided by the invention comprises: mixing a terminal vinyl silicone oil, a terminal hydrogen silicone oil, a methyl silicone oil, a Custer catalyst, a silica nano particle uniformly and removing bubbles to prepare a mixture; A coating is formed; the coating is cured to provide an anti-icing coating.

In the above preparation method, 10 to 100 parts of the terminal vinyl silicone oil, 1-10 parts of the terminal hydrogen silicone oil, 10-500 parts of the methyl silicone oil, 0.01-1 part of the Castell catalyst, and 1 to 50 parts by mass. The silica nanoparticles are uniformly mixed and the bubbles are removed.

In the above preparation method, the terminal vinyl silicone oil, the terminal hydrogen silicone oil, the methyl silicone oil, the Custer catalyst, and the silica nanoparticles are stirred at a stirring rate of 4000 to 6000 rpm for 25 to 35 minutes to be uniformly mixed.

In the above preparation method, the terminal vinyl silicone oil, the terminal hydrogen silicone oil, the methyl silicone oil, the Custer catalyst, and the silica nanoparticles were stirred at a stirring rate of 5000 rpm for 30 minutes to be uniformly mixed.

In the above preparation method, air bubbles are removed by vacuuming.

In the above preparation method, the viscosity of the terminal vinyl silicone oil is 10,000 to 50,000 lis, the viscosity of the terminal hydrogen silicone oil is 10 to 200 lis, and the viscosity of the methyl silicone oil is 1000 to 5000 ris.

In the above preparation method, the mixture is formed into a coating by a doctor blade method, a roll coating method, a spray method, or a sputtering method.

In the above preparation method, in the step of forming the mixture into a coating layer, the thickness of the coating layer is 1 to 5 mm.

In the above preparation method, the coating is cured at a temperature of 60 to 80 ° C for 20 to 28 hours, and then cooled to room temperature to obtain an ice-proof coating.

In the above preparation method, the coating is cured at a temperature of 70 ° C for 24 hours, and then cooled to room temperature to obtain an ice-proof coating.

In the above preparation method, the water contact angle of the anti-icing coating is 110° to 150°, the rolling angle is 5° to 10°, and the ice adhesion strength is 30 to 80 kPa.

An anti-icing coating prepared according to the above preparation method.

Beneficial effect

The preparation method of the anti-icing coating provided by the invention is prepared by mixing the terminal vinyl silicone oil, the terminal hydrogen silicone oil, the methyl silicone oil, the Custer catalyst, the silica nano particles in proportion and defoaming, thereby forming a coating layer, It is then cured to prepare an anti-icing coating. In the present invention, a suitable ratio of terminal vinyl silicone oil, terminal hydrogen silicone oil and methyl silicone oil is mixed to ensure that the prepared coating has suitable shear strength, and a suitable proportion of Cartes catalytic component is added to control The curing time of the coating, in addition, by adding a suitable proportion of silica nanoparticles to ensure that the prepared coating has good hydrophobicity and good mechanical properties. Therefore, the preparation method of the anti-icing coating has low cost and simple production process, and the prepared anti-icing coating has low ice adhesion strength, good anti-icing performance and good durability, and can be widely used as an active anti-icing system. In the fields of aerospace, high-speed locomotives, transmission lines, wind power generation, etc.

DRAWINGS

In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings to be used in the embodiments will be briefly described below. Obviously, the drawings in the following description are only some of the present invention. For the embodiments, those skilled in the art can obtain other drawings according to the drawings without any creative work.

1 is a process flow diagram of a method of making an ice resistant coating in accordance with an embodiment of the present invention.

2 is a schematic view showing the structure of an anti-icing coating according to an embodiment of the present invention.

Embodiments of the invention

The technical solutions in the embodiments of the present invention are clearly and completely described in the following with reference to the accompanying drawings in the embodiments of the present invention. It is obvious that the described embodiments are only a part of the embodiments of the present invention, but not all embodiments. All other embodiments obtained by those of ordinary skill in the art based on the embodiments of the present invention are within the scope of the present invention.

The preparation method of the anti-icing coating provided by the invention, as shown in FIG. 1 , comprises the following steps:

S1: mixing a terminal vinyl silicone oil, a terminal hydrogen silicone oil, a methyl silicone oil, a Custer catalyst, and silica nanoparticles to form a mixture. In this step, 10-100 parts of terminal vinyl silicone oil, 1-10 parts of terminal hydrogen silicone oil, 10-500 parts of methyl silicone oil, 0.01-1 part of Castell catalyst, 1-50 parts of two parts by mass. The silica nanoparticles are placed in a glassware and vigorously stirred at a stirring rate of 4000 to 6000 rpm for 25 to 35 minutes, preferably, vigorously stirred at a stirring rate of 5000 rpm for 30 minutes to uniformly mix, and then evacuated to remove air bubbles. Among them, the change of the proportion of the terminal vinyl silicone oil, the terminal hydrogen silicone oil and the methyl silicone oil will change the degree of crosslinking of the product, thereby affecting the shear strength of the coating. In this step, the ratio of the terminal vinyl silicone oil, The terminal hydrogen silicone oil and methyl silicone oil can make the obtained product have a suitable degree of crosslinking, thereby ensuring the coating has a suitable shear strength. The change of the catalytic component of the Custer directly affects the curing cross-linking time. By controlling the proportion of the catalyst, the curing time of the coating is not too long or too short in the case of ensuring that the coating can be sufficiently cross-linked. In addition, in this step, since the composition change of the silica nanoparticles affects the hydrophobic property and the mechanical properties of the coating, selecting the silica nanoparticles of the ratio can ensure good hydrophobicity of the prepared coating. It also has good mechanical properties. Therefore, in this process, it is necessary to strictly control the amount and proportion of each component. The viscosity of the terminal vinyl silicone oil is 10,000 to 50,000 lis (cst), the viscosity of the terminal hydrogen silicone oil is 10 to 200 lis, and the viscosity of the methyl silicone oil is 1000 to 5000 lis. Preferably, the viscosity of the terminal vinyl silicone oil is 20,000 lis, The terminal hydrogen silicone oil has a viscosity of 50 lis and the methyl silicone oil has a viscosity of 1000 ris.

S2: The mixture is made into a coating. In this step, a coating having a thickness of 1 to 5 mm is prepared by knife coating, roll coating, spraying, sputtering, and the mixture can be subjected to blade coating, roll coating, spraying, sputtering on the substrate 1 to prepare. Coating 2 (shown in Figure 2), the substrate can be selected from substrates commonly used in the art.

S3: Curing the coating to obtain an anti-icing coating. In this step, the coating is cured in an oven at a temperature of 60-80 ° C for 20 to 28 hours, and then cooled to room temperature to obtain an anti-icing coating. Preferably, the coating is cured at a temperature of 70 ° C. After 24 hours, it was cooled to room temperature to prepare an anti-icing coating.

The water contact angle, rolling angle, ice adhesion strength and durability test were performed on the prepared anti-icing coating. The test results were as follows: the water contact angle of the anti-icing coating was 110° to 150°, and the rolling angle was 5°. ~10°, the ice adhesion strength is 30 to 80 kPa, and therefore, the anti-icing coating of the present invention has good anti-icing performance. After 100 freeze/de-icing cycles, the ice adhesion strength of the anti-icing coating decreased by only 15% to 20%. It can be seen that the anti-icing coating has good durability.

The preparation method of the anti-icing coating provided by the invention is prepared by mixing the terminal vinyl silicone oil, the terminal hydrogen silicone oil, the methyl silicone oil, the Custer catalyst, the silica nano particles in proportion and defoaming, thereby forming a coating layer, It is then cured to prepare an anti-icing coating. The preparation method of the anti-icing coating has low cost and simple production process, and the prepared anti-icing coating has low ice adhesion strength, good anti-icing performance and good durability, and can be widely used as an active anti-icing system for aviation. Aerospace, high-speed locomotives, transmission lines, wind power and other fields.

Example 1

100 parts of terminal vinyl silicone oil with a viscosity of 10,000 lis, 10 parts of hydrogen silicone oil with a viscosity of 100 lis, 200 parts of methyl silicone oil with a viscosity of 3,500 lis, 0.01 parts of Castell catalyst and 50 parts by mass, respectively. The silica nanoparticles were placed in a glassware, stirred vigorously for 30 minutes at a stirring rate of 5000 rpm to uniformly mix, and evacuated to remove air bubbles. A coating having a thickness of 2 mm was then prepared by knife coating. It was cured in an oven at 60 ° C for 26 hours and cooled to room temperature to obtain an ice-resistant coating having low ice adhesion strength. The obtained anti-icing coating has a water contact angle of 110°, a rolling angle of 8°, and an ice adhesion strength of 50 kPa. After 100 freeze/de-icing cycles, the ice adhesion strength of the anti-icing coating only decreases. 20%.

Example 2

10 parts of terminal vinyl silicone oil with a viscosity of 50,000 lis, 1 part of terminal hydrogen silicone oil with a viscosity of 10 lis, 100 parts of methyl silicone oil with a viscosity of 1500 lis, 0.1 part of Caster catalyst and 5 parts by mass, respectively. The silica nanoparticles were placed in a glassware, stirred vigorously at a stirring rate of 4000 rpm for 35 minutes to uniformly mix, and evacuated to remove air bubbles. A coating having a thickness of 1 mm was then prepared by roll coating. It was cured in an oven at 70 ° C for 24 hours and cooled to room temperature to obtain an ice-resistant coating having low ice adhesion strength. The obtained anti-icing coating has a water contact angle of 120°, a rolling angle of 10°, and an ice adhesion strength of 30 kPa. After 100 freeze/de-icing cycles, the ice adhesion strength of the anti-icing coating only decreases. 20%.

Example 3

According to the parts by mass, weigh 50 parts of vinyl acetate with a viscosity of 20,000 lis, 4 parts of hydrogen silicone oil with a viscosity of 50 lis, 500 parts of methyl silicone oil with a viscosity of 1000 ris, 0.5 parts of Custer catalyst and 1 The silica nanoparticles were placed in a glassware, stirred vigorously for 25 minutes at a stirring rate of 6000 rpm to uniformly mix, and evacuated to remove air bubbles. A coating having a thickness of 4 mm was then prepared by sputtering. It was cured in an oven at 80 ° C for 20 hours and cooled to room temperature to obtain an ice-resistant coating having low ice adhesion strength. The obtained anti-icing coating has a water contact angle of more than 140°, a rolling angle of 5°, and an ice adhesion strength of 80 kPa. After 100 freeze/de-icing cycles, the ice adhesion strength of the anti-icing coating only decreases. 20%.

Example 4

According to the parts by mass, 35 parts of terminal vinyl silicone oil with a viscosity of 12000 lis, 8 parts of terminal hydrogen silicone oil with a viscosity of 200 lis, 300 parts of methyl silicone oil with a viscosity of 2500 lis, 0.7 parts of Custer catalyst and 20 parts were weighed separately. The silica nanoparticles were placed in a glassware, stirred vigorously for 33 minutes at a stirring rate of 4500 rpm to uniformly mix, and evacuated to remove air bubbles. Then, a coating having a thickness of 3 mm was prepared by spraying. It was cured in an oven at 65 ° C for 28 hours and cooled to room temperature to obtain an ice-resistant coating having low ice adhesion strength. The prepared anti-icing coating has a water contact angle of more than 120°, a rolling angle of 9°, and an ice adhesion strength of 30 kPa. After 100 freeze/de-icing cycles, the ice adhesion strength of the anti-icing coating only decreases. 15%.

Example 5

According to the parts by mass, 75 parts of the terminal vinyl silicone oil with a viscosity of 35000 lis, 3 parts of the terminal hydrogen silicone oil with a viscosity of 150 lis, 10 parts of methyl silicone oil with a viscosity of 5000 lis, 1 part of the Custer catalyst and 15 parts were weighed. The silica nanoparticles were placed in a glassware, stirred vigorously at a stirring rate of 5,500 rpm for 28 minutes to uniformly mix, and evacuated to remove air bubbles. A coating having a thickness of 5 mm was then prepared by knife coating. It was cured in an oven at 75 ° C for 23 hours and cooled to room temperature to obtain an ice-resistant coating having low ice adhesion strength. The obtained anti-icing coating has a water contact angle of more than 130°, a rolling angle of 6°, and an ice adhesion strength of 30 kPa. After 100 ice/de-icing cycles, the ice adhesion strength of the anti-icing coating only decreases. 18%.

The above are only the preferred embodiments of the present invention, and are not intended to limit the present invention. Any modifications, equivalents, improvements, etc., which are within the spirit and scope of the present invention, should be included in the scope of the present invention. within.

Claims (12)

A method for preparing an anti-icing coating, comprising: Mixing the terminal vinyl silicone oil, the terminal hydrogen silicone oil, the methyl silicone oil, the Custer catalyst, the silica nanoparticles, and removing the bubbles to prepare a mixture; Forming the mixture into a coating; The coating was cured to produce an anti-icing coating. The preparation method according to claim 1, wherein 10 to 100 parts of the terminal vinyl silicone oil, 1-10 parts of the terminal hydrogen silicone oil, 10 to 500 parts of the methyl silicone oil, and 0.01 to 1 part of the card are used in parts by mass. The Ster catalyst, 1-50 parts of silica nanoparticles are uniformly mixed and bubbles are removed. The preparation method according to claim 1, wherein the terminal vinyl silicone oil, the terminal hydrogen silicone oil, the methyl silicone oil, the Custer catalyst, and the silica nanoparticles are stirred at a stirring rate of 4000 to 6000 rpm for 25~. Mix for 35 min. The preparation method according to claim 1, wherein the terminal vinyl silicone oil, the terminal hydrogen silicone oil, the methyl silicone oil, the Custer catalyst, and the silica nanoparticles are stirred at a stirring rate of 5000 rpm for 30 minutes to be uniformly mixed. . The preparation method according to claim 1, wherein the bubble is removed by a vacuuming method. The preparation method according to claim 1, wherein the terminal vinyl silicone oil has a viscosity of 10,000 to 50,000 lis, the terminal hydrogen silicone oil has a viscosity of 10 to 200 rissia, and the methyl silicone oil has a viscosity of 1000 Å. ~5000 ris. The preparation method according to claim 1, wherein the mixture is formed into the coating by a method of blade coating, roll coating, spraying, sputtering. The preparation method according to claim 1, wherein in the step of forming the mixture into the coating layer, the coating layer has a thickness of 1 to 5 mm. The preparation method according to claim 1, wherein the coating is cured at a temperature of 60 to 80 ° C for 20 to 28 hours, and then cooled to room temperature to obtain the anti-icing coating. The preparation method according to claim 1, wherein the coating is cured at a temperature of 70 ° C for 24 hours and then cooled to room temperature to obtain the anti-icing coating. The preparation method according to claim 1, wherein the anti-icing coating has a water contact angle of 110° to 150°, a rolling angle of 5° to 10°, and an ice adhesion strength of 30 to 80 kPa. The anti-icing coating produced by the preparation method according to any one of claims 1 to 12.