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WO2018223781A1 - 一种防冰涂层及其制备方法 - Google Patents

一种防冰涂层及其制备方法 Download PDF

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Publication number
WO2018223781A1
WO2018223781A1 PCT/CN2018/083680 CN2018083680W WO2018223781A1 WO 2018223781 A1 WO2018223781 A1 WO 2018223781A1 CN 2018083680 W CN2018083680 W CN 2018083680W WO 2018223781 A1 WO2018223781 A1 WO 2018223781A1
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WIPO (PCT)
Prior art keywords
coating
silicone oil
preparation
icing
parts
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/CN2018/083680
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English (en)
French (fr)
Inventor
刘若鹏
赵治亚
李自东
杨鸿帆
白雪
胡宇
曾元强
张运湘
李雪
刘光烜
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Luoyang Institute of Cutting Edge Technology
Luoyang Cutting Edge Equipment Technology Ltd
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Luoyang Institute of Cutting Edge Technology
Luoyang Cutting Edge Equipment Technology Ltd
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Publication of WO2018223781A1 publication Critical patent/WO2018223781A1/zh
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L83/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
    • C08L83/04—Polysiloxanes
    • 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
    • C09D183/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Coating compositions based on derivatives of such polymers
    • C09D183/04—Polysiloxanes
    • 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
    • C09D183/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Coating compositions based on derivatives of such polymers
    • 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
    • C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
    • C08G77/04—Polysiloxanes
    • C08G77/12—Polysiloxanes containing silicon bound to hydrogen
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
    • C08G77/04—Polysiloxanes
    • C08G77/20—Polysiloxanes containing silicon bound to unsaturated aliphatic groups
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00—Specific properties of additives
    • C08K2201/011—Nanostructured additives
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00—Polymer mixtures characterised by other features
    • C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
    • C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00—Polymer mixtures characterised by other features
    • C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00—Polymer mixtures characterised by other features
    • C08L2205/05—Polymer mixtures characterised by other features containing polymer components which can react with one another
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2312/00—Crosslinking

Definitions

  • the invention relates to the field of composite materials, in particular to an anti-icing coating and a preparation method thereof.
  • 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°.
  • 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.
  • 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 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.
  • 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.
  • 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.
  • 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
  • the viscosity of the methyl silicone oil is 1000 to 5000 ris.
  • the mixture is formed into a coating by a doctor blade method, a roll coating method, a spray method, or a sputtering method.
  • the thickness of the coating layer is 1 to 5 mm.
  • 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.
  • 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.
  • the water contact angle of the anti-icing coating is 110° to 150°
  • the rolling angle is 5° to 10°
  • the ice adhesion strength is 30 to 80 kPa.
  • 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.
  • 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.
  • 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.
  • FIG. 1 is a process flow diagram of a method of making an ice resistant coating in accordance with an embodiment of the present invention.
  • FIG. 2 is a schematic view showing the structure of an anti-icing coating according to an embodiment of the present invention.
  • the preparation method of the anti-icing coating provided by the invention 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.
  • 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.
  • 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.
  • 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.
  • 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
  • the viscosity of the methyl silicone oil is 1000 to 5000 lis.
  • 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.
  • 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.
  • 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.
  • 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.
  • 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%.
  • 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%.
  • 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%.
  • terminal vinyl silicone oil with a viscosity of 12000 lis 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%.
  • the terminal vinyl silicone oil with a viscosity of 35000 lis 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%.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Wood Science & Technology (AREA)
  • Health & Medical Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Paints Or Removers (AREA)
  • Materials Applied To Surfaces To Minimize Adherence Of Mist Or Water (AREA)

Abstract

防冰涂层的制备方法，包括：将端乙烯基硅油、端氢硅油、甲基硅油、卡斯特催化剂、二氧化硅纳米微粒混合均匀并去除气泡，制得混合物(S1)；将混合物制成涂层(S2)；固化涂层，制得防冰涂层(S3)。

Description

一种防冰涂层及其制备方法 技术领域
本发明涉及复合材料领域，具体而言，一种防冰涂层及其制备方法。
 背景技术
降水覆冰、升华覆冰等覆冰现象给人们的生产和生活带来极大的不便，并且会造成巨大的经济损失，特别是对于电力系统，不仅会导致输电线路中断，杆塔倒塌、断线等，甚至会导致输电线路瘫痪，对电力系统的安全运营产生严重的危害，我国是输电线路覆冰严重的国家之一，线路覆冰事故发生的概率居于世界前列。此外，铁路线路覆冰、机翼覆冰等也可能对人们的生命财产造成巨大的威胁。因此，开展防覆冰材料的研究，具有重大的社会意义和经济价值。
 技术问题
目前为止，国内在防覆冰涂料方面也有一定研究。现有的技术大都通过制备超疏水防覆冰涂料来实现，超疏水防覆冰涂料是指涂膜的表面对水的接触角大于150°，同时滚落角小于10°的涂料。当水滴在涂层表面的接触角较大且滚落角相对较小时，水滴和涂层之间的粘附力远远小于其和一般涂层间的粘附力，水滴受重力的影响就会自动滚落涂层表面，从而达到了防止水滴在涂层表面结冰的目的。但是，在潮湿的环境中，当超疏水防覆冰涂料结冰后，会使其失去原有的超疏水性质，而且冰的粘附强度往往比较大，使得除冰难度增加。同时，防覆冰材料在使用多次后，防冰性能大大下降，因此，现有的防冰材料往往存在防冰效果差以及耐久性差的缺点。
 技术解决方案
本发明为了解决现有防冰涂层在结冰后不易除去以及涂层耐久性差的问题，提供了一种具有低冰粘附强度的防冰涂层及其制备方法。
本发明提供的防冰涂层的制备方法，包括：将端乙烯基硅油、端氢硅油、甲基硅油、卡斯特催化剂、二氧化硅纳米微粒混合均匀并去除气泡，制得混合物；将混合物制成涂层；固化涂层，制得防冰涂层。
在上述制备方法中，按质量份数，将10-100份端乙烯基硅油、1-10份端氢硅油、10-500份甲基硅油、0.01-1份卡斯特催化剂、1-50份二氧化硅纳米微粒混合均匀并去除气泡。
在上述制备方法中，将端乙烯基硅油、端氢硅油、甲基硅油、卡斯特催化剂、二氧化硅纳米微粒在4000~6000rpm的搅拌速率下，搅拌25~35min以混合均匀。
在上述制备方法中，将端乙烯基硅油、端氢硅油、甲基硅油、卡斯特催化剂、二氧化硅纳米微粒在5000rpm的搅拌速率下，搅拌30min以混合均匀。
在上述制备方法中，采用抽真空的方法去除气泡。
在上述制备方法中，端乙烯基硅油的粘度为10000~50000里斯，端氢硅油的粘度为10~200里斯以及甲基硅油的粘度为1000~5000里斯。
在上述制备方法中，采用刮涂、辊涂、喷射、溅射的方法将混合物制成涂层。
在上述制备方法中，在将混合物制成涂层的步骤中，涂层的厚度为1~5毫米。
在上述制备方法中，将涂层在60~80℃温度下，固化20~28小时，然后冷却至室温，制得防冰涂层。
在上述制备方法中，将涂层在70℃温度下，固化24小时，然后冷却至室温，制得防冰涂层
在上述制备方法中，防冰涂层的水接触角为110°~150°，滚动角为5°~10°，冰粘附强度为30~80 kPa。
根据上述制备方法制得的防冰涂层。
 有益效果
本发明提供的防冰涂层的制备方法，通过将端乙烯基硅油、端氢硅油、甲基硅油、卡斯特催化剂、二氧化硅纳米微粒按比例进行混合并且去气泡，制成涂层，然后固化以制备防冰涂层。在本发明中通过将合适比例的端乙烯基硅油、端氢硅油和甲基硅油进行混合，来保证所制备的涂层具有合适的剪切强度，加入合适比例的卡特斯催化组分，来控制涂层的固化时间，此外，通过加入合适比例的二氧化硅纳米微粒来保证所制备的涂层具有良好的疏水性和良好的力学性能。因此，该防冰涂层的制备方法成本低、生产工艺简单，并且制备的防冰涂层具有低冰粘附强度，防冰性能好且耐久性好，可作为主动防冰系统，广泛地应用于航空航天、高速机车、输电线、风力发电等领域。
 附图说明
为了更清楚地说明本发明实施例或现有技术中的技术方案，下面将对实施例中所需要使用的附图作简单地介绍，显而易见地，下面描述中的附图仅仅是本发明的一些实施例，对于本领域普通技术人员来讲，在不付出创造性劳动的前提下，还可以根据这些附图获得其他的附图。
图1是根据本发明的实施例的制备防冰涂层的方法的工艺流程图。
图2是根据本发明的实施例的防冰涂层的结构示意图。
 本发明的实施方式
下面将结合本发明实施例中的附图，对本发明实施例中的技术方案进行清楚、完整地描述，显然，所描述的实施例仅仅是本发明一部分实施例，而不是全部的实施例。基于本发明中的实施例，本领域普通技术人员所获得的所有其他实施例，都属于本发明保护的范围。
本发明提供的防冰涂层的制备方法,如图1所示，包括以下步骤：
S1：将端乙烯基硅油、端氢硅油、甲基硅油、卡斯特催化剂、二氧化硅纳米微粒混合均匀并去除气泡，制得混合物。在该步骤中，按质量份数，将10-100份端乙烯基硅油、1-10份端氢硅油、10-500份甲基硅油、0.01-1份卡斯特催化剂、1-50份二氧化硅纳米微粒，放入玻璃器皿中，在4000~6000rpm的搅拌速率下剧烈搅拌25~35min，优选地，在5000rpm的搅拌速率下剧烈搅拌30min，以混合均匀，然后抽真空除去气泡。其中，端乙烯基硅油、端氢硅油和甲基硅油三者比例的变化，会改变产品的交联度，从而影响涂层的剪切强度，该步骤中，选用该比例的端乙烯基硅油、端氢硅油和甲基硅油可以使制得的产品具有合适的交联度，从而保证涂层具有合适的剪切强度。卡斯特催化组分的变化会直接影响固化交联的时间，通过控制催化剂的比例，在保证涂层能够充足交联的情况下，使涂层的固化时间不会过长或过短。此外，在该步骤中，由于二氧化硅纳米微粒的组分变化会影响疏水性能和涂层的力学性能，因此选择该比例的二氧化硅纳米微粒可以在保证制得的涂层具有良好疏水性的同时也兼具良好的力学性能。因此，在此过程中，需要严格控制各个组分的用量和比例。端乙烯基硅油的粘度为10000~50000里斯（cst）、端氢硅油的粘度为10~200里斯、甲基硅油的粘度为1000~5000里斯，优选地，端乙烯基硅油的粘度为20000里斯、端氢硅油的粘度为50里斯、甲基硅油的粘度为1000里斯。
S2：将混合物制成涂层。在该步骤中，通过刮涂、辊涂、喷射、溅射的方法制备出厚度为1~5毫米的涂层，且可以将混合物刮涂、辊涂、喷射、溅射在基底1上以制备涂层2（如图2所示），基底可以选用本领域常用的基底。
S3：固化涂层，制得防冰涂层。在该步骤中，将涂层放在温度为60~80℃的烘箱中固化20~28小时，然后冷却至室温，制得防冰涂层，优选地，将涂层在70℃温度下，固化24小时，然后冷却至室温，制得防冰涂层。
对所制得的防冰涂层进行水接触角、滚动角、冰粘附强度和耐久性测试，测试结果为：防冰涂层的水接触角为110°~150°，滚动角为5°~10°，冰粘附强度为30~80 kPa，因此，本发明的防冰涂层防冰性能好。经过100次结冰/除冰循环，防冰涂层的冰粘附强度仅下降15%~20%，可见，防冰涂层具有好的耐久性。
本发明提供的防冰涂层的制备方法，通过将端乙烯基硅油、端氢硅油、甲基硅油、卡斯特催化剂、二氧化硅纳米微粒按比例进行混合并且去气泡，制成涂层，然后固化以制备防冰涂层。该防冰涂层的制备方法成本低、生产工艺简单，并且制备的防冰涂层具有低冰粘附强度，防冰性能好且耐久性好，可作为主动防冰系统，广泛地应用于航空航天、高速机车、输电线、风力发电等领域。
实施例1
按质量份数，分别称取100份粘度为10000里斯的端乙烯基硅油、10份粘度为100里斯的端氢硅油、200份粘度为3500里斯的甲基硅油、0.01份卡斯特催化剂和50份二氧化硅纳米微粒，加入到玻璃器皿中，在5000rpm的搅拌速率下，剧烈搅拌30分钟以混合均匀，抽真空除去气泡。然后采用刮涂的方法，制备出厚度2毫米的涂层。放在60℃烘箱中固化26小时，冷却至室温，得到具有低冰粘附强度的防冰涂层。制得的防冰涂层的水接触角为110°，滚动角为8°，冰粘附强度为50 kPa，经过100次结冰/除冰循环，防冰涂层的冰粘附强度仅下降20%。
实施例2
按质量份数，分别称取10份粘度为50000里斯的端乙烯基硅油、1份粘度为10里斯的端氢硅油、100份粘度为1500里斯的甲基硅油、0.1份卡斯特催化剂和5份二氧化硅纳米微粒，加入到玻璃器皿中，在4000rpm的搅拌速率下，剧烈搅拌35分钟以混合均匀，抽真空除去气泡。然后采用辊涂的方法，制备出厚度1毫米的涂层。放在70℃烘箱中固化24小时，冷却至室温，得到具有低冰粘附强度的防冰涂层。制得的防冰涂层的水接触角为120°，滚动角为10°，冰粘附强度为30 kPa，经过100次结冰/除冰循环，防冰涂层的冰粘附强度仅下降20%。
实施例3
按质量份数，分别称取50份粘度为20000里斯的端乙烯基硅油、4份粘度为50里斯的端氢硅油、500份粘度为1000里斯的甲基硅油、0.5份卡斯特催化剂和1份二氧化硅纳米微粒，加入到玻璃器皿中，在6000rpm的搅拌速率下，剧烈搅拌25分钟以混合均匀，抽真空除去气泡。然后采用溅射的方法，制备出厚度4毫米的涂层。放在80℃烘箱中固化20小时，冷却至室温，得到具有低冰粘附强度的防冰涂层。制得的防冰涂层的水接触角大于140°，滚动角为5°，冰粘附强度为80 kPa，经过100次结冰/除冰循环，防冰涂层的冰粘附强度仅下降20%。
实施例4
按质量份数，分别称取35份粘度为12000里斯的端乙烯基硅油、8份粘度为200里斯的端氢硅油、300份粘度为2500里斯的甲基硅油、0.7份卡斯特催化剂和20份二氧化硅纳米微粒，加入到玻璃器皿中，在4500rpm的搅拌速率下，剧烈搅拌33分钟以混合均匀，抽真空除去气泡。然后采用喷射的方法，制备出厚度3毫米的涂层。放在65℃烘箱中固化28小时，冷却至室温，得到具有低冰粘附强度的防冰涂层。制得的防冰涂层的水接触角大于120°，滚动角为9°，冰粘附强度为30 kPa，经过100次结冰/除冰循环，防冰涂层的冰粘附强度仅下降15%。
实施例5
按质量份数，分别称取75份粘度为35000里斯的端乙烯基硅油、3份粘度为150里斯的端氢硅油、10份粘度为5000里斯的甲基硅油、1份卡斯特催化剂和15份二氧化硅纳米微粒，加入到玻璃器皿中，在5500rpm的搅拌速率下，剧烈搅拌28分钟以混合均匀，抽真空除去气泡。然后采用刮涂的方法，制备出厚度5毫米的涂层。放在75℃烘箱中固化23小时，冷却至室温，得到具有低冰粘附强度的防冰涂层。制得的防冰涂层的水接触角大于130°，滚动角为6°，冰粘附强度为30 kPa，经过100次结冰/除冰循环，防冰涂层的冰粘附强度仅下降18%。
以上仅为本发明的较佳实施例而已，并不用以限制本发明，凡在本发明的精神和原则之内，所作的任何修改、等同替换、改进等，均应包含在本发明的保护范围之内。

Claims (12)

  1. 一种防冰涂层的制备方法，其特征在于，包括：
    将端乙烯基硅油、端氢硅油、甲基硅油、卡斯特催化剂、二氧化硅纳米微粒混合均匀并去除气泡，制得混合物；
    将所述混合物制成涂层；
    固化所述涂层，制得防冰涂层。
  2. 根据权利要求1所述的制备方法，其特征在于，按质量份数，将10-100份端乙烯基硅油、1-10份端氢硅油、10-500份甲基硅油、0.01-1份卡斯特催化剂、1-50份二氧化硅纳米微粒混合均匀并去除气泡。
  3. 根据权利要求1所述的制备方法，其特征在于，将端乙烯基硅油、端氢硅油、甲基硅油、卡斯特催化剂、二氧化硅纳米微粒在4000~6000rpm的搅拌速率下，搅拌25~35min以混合均匀。
  4. 根据权利要求1所述的制备方法，其特征在于，将端乙烯基硅油、端氢硅油、甲基硅油、卡斯特催化剂、二氧化硅纳米微粒在5000rpm的搅拌速率下，搅拌30min以混合均匀。
  5. 根据权利要求1所述的制备方法，其特征在于，采用抽真空的方法去除所述气泡。
  6. 根据权利要求1所述的制备方法，其特征在于，所述端乙烯基硅油的粘度为10000~50000里斯，所述端氢硅油的粘度为10~200里斯以及所述甲基硅油的粘度为1000~5000里斯。
  7. 根据权利要求1所述的制备方法，其特征在于，采用刮涂、辊涂、喷射、溅射的方法将所述混合物制成所述涂层。
  8. 根据权利要求1所述的制备方法，其特征在于，在将所述混合物制成所述涂层的步骤中，所述涂层的厚度为1~5毫米。
  9. 根据权利要求1所述的制备方法，其特征在于，将所述涂层在60~80℃温度下，固化20~28小时，然后冷却至室温，制得所述防冰涂层。
  10. 根据权利要求1所述的制备方法，其特征在于，将所述涂层在70℃温度下，固化24小时，然后冷却至室温，制得所述防冰涂层。
  11. 根据权利要求1所述的制备方法，其特征在于，所述防冰涂层的水接触角为110°~150°，滚动角为5°~10°，冰粘附强度为30~80 kPa。
  12. 根据权利要求1~12任一项所述的制备方法制得的防冰涂层。
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