CN110028899A - A kind of patterning polysiloxanes ice-covering-proof coating and preparation method thereof - Google Patents
A kind of patterning polysiloxanes ice-covering-proof coating and preparation method thereof Download PDFInfo
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- CN110028899A CN110028899A CN201910359279.5A CN201910359279A CN110028899A CN 110028899 A CN110028899 A CN 110028899A CN 201910359279 A CN201910359279 A CN 201910359279A CN 110028899 A CN110028899 A CN 110028899A
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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- 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
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- 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
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Abstract
The invention discloses a kind of patterning polysiloxanes ice-covering-proof coatings and preparation method thereof.This method is that the branching shape dimethyl silicone polymer that will be prepared uniformly is mixed with fluorinated poss, both-end hydrogen dimethyl silicone polymer, change the temperature and humidity when coating surface drying, 15~45 DEG C, under 45~85% high humidity environment, patterned surface is obtained by breathing pattern method, heat cross-linking film-forming obtains the ice-covering-proof coating with patterned surface.Wherein: branching shape dimethyl silicone polymer 3~10%；Fluorinated poss 0~5%；Both-end hydrogen-based dimethyl siloxane 10~20%；Catalyst 0.01~0.12%；Surplus is solvent.Patterning fluorination POSS crosslinked, branched shape polysiloxanes ice-covering-proof coating carries out ice shear strength and wearability test, obtains the ice shear strength and up to 2500 times abrasion cycles numbers down to 15kPa.Preparation method of the present invention is easy, and condition is controllable, has great application prospect in ice-covering-proof field.
Description
Technical field
The invention belongs to ice-covering-proof coating field of material technology, and in particular to a kind of patterning polysiloxanes ice-covering-proof coating
And preparation method thereof.
Background technique
Icing is the common natural phenomena of cold district, but accumulation of the ice sheet on various infrastructure surfaces can be to people
Production and living cause many potential hazards, that there are deicing efficiencies is low for the active de-icing method of current practice, energy consumption is big, dirty
The disadvantages of contaminating environment.The ice-covering-proof coating that can be realized passive deicing effect is not only time saving and energy saving and small to environmental hazard, is mesh
Preceding research hotspot.Low-surface-energy elastomeric material is one of ice-covering-proof strategy general at present, and organosilicon material is then extensive
Low-surface-energy elastomeric material applied to ice-covering-proof field.The low-surface-energy of fluorinated poss (POSS)
Be conducive to it to migrate to coating surface, the addition for being fluorinated POSS can improve the hydrophobicity of coating, can also play ice-covering-proof coating
To certain humidification.The micro-structure of patterning coating surface can promote to generate micro-crack between coating and ice interface, cause
Stress is concentrated, and is promoted ice to remove from coating surface, is improved the anti-icing performance of coating.
Pore-foaming agent is introduced in dimethyl silicone polymer (PDMS) system, PDMS base sandwich-like coating is obtained after removing,
The PDMS layer at top hinders to generate mechanical riveted effect between ice and coating, while sandwich-like porous structure reduces coating itself
Elasticity modulus, realize ultralow ice adhesive strength (He Z, Zhuo Y, He J, the Zhang Z.Design and of 0.9kPa
preparation of sandwich-like polydimethylsiloxane(PDMS)sponges with super-low
ice adhesion.Soft Matter,2018,14(23):4846-4851).This seminar is prepared for the branch containing POSS early period
Change shape PDMS slipping property ice-covering-proof coating makes lubricity silicone oil play interface sliding in coating surface by means of branching shape PDMS
Effect reduces ice shear strength, while the addition of POSS improves coating abrasion performance, and ice-covering-proof coating is made to have good durability
(Gao S,Liu B,Peng J,Zhu K,Zhao Y,Li X,Yuan X.Icephobic durability of branched
PDMS slippage coatings co-crosslinked by functionalized POSS.ACS
Appl.Mater.Interfaces,2019,11(4):4654–4666)。
Breathing pattern method is a kind of excellent process for preparing patterned surface easy to operate, mild condition is controllable.It will gather
Polymer solution is coated in substrate surface, and quickly volatilizing with the immiscible low boiling point solvent of water declines Coated Surface Temperature sharply,
The vapor in high humidity environment is caused to condense, after coating surface is nucleated and to form droplet, the regular arrangement of droplet is formed orderly
Array.When in coating solvent and droplet volatilize completely after, formed patterned surface.Han et al. is connect using polystyrene
The toluene mixed solution of branch ethylene glycol copolymer and iron chloride has layering micro/nano level by breathing pattern method preparation
The coating of topological structure, it can be achieved that the quick landing of liquid, shows excellent Adhesion Resistance (Han under lesser inclination angle
K,Heng L,Jiang L.Multiphase media antiadhesive coatings:Hierarchical self-
assembled porous materials generated using breath figure patterns.ACS Nano,
2016,10(12):11087-11095)。
The soft elasticity of present invention combination branching shape PDMS and the hydrophobic enhancing function of fluorination POSS, it is logical using breathing pattern method
The temperature and humidity during regulation surface drying are crossed, the patterning ice-covering-proof coating prepared is with excellent anti-icing performance and absolutely
The ice shear strength of good mechanical stability, obtained ice-covering-proof coating can may be up to 2500 down to 15kPa, wear-resistant number
It is secondary, and had not been reported before this work.
Summary of the invention
It is an object of the invention to overcome the deficiencies in the prior art, are prepared by breathing pattern method regulating and controlling temperature with humidity
A kind of patterning polysiloxanes ice-covering-proof coating, preparation method of the present invention is easy, and reaction is mild controllable.
The present invention is by the branching shape dimethyl silicone polymer being prepared and fluorinated poss, both-end
Hydrogen dimethyl silicone polymer after evenly mixing, heat cross-linking film-forming is carried out under different temperatures, different humidity, is obtained after surface drying
Patterning ice-covering-proof coating have excellent anti-icing performance and excellent mechanical stability, can be applied to ice-covering-proof coating neck
Domain.
The preparation method of branching shape dimethyl silicone polymer is referred to from Chinese patent CN 108610959 A (Yuan Xiaoyan, Peng
Outstanding person, Gao Shuhui, Li Xiaohui, a kind of preparation side for being fluorinated POSS cross-linked silicone scopiform molecule ice-covering-proof coating Zhu Kongying, Liu Bo
Method .CN 108610959 A, 2018).The structural formula of the branching shape dimethyl silicone polymer of synthesis are as follows:
In formula, (n-x)/x=0.1~10, m/n=1~24；Wherein R' is methyl or normal-butyl.
The preparation method of fluorinated poss is referred to from 104263238 B (Yuan Xiao of Chinese patent CN
Swallow, Tao Chao, Zhu Kongying, Luo Cheng Hao, Zhao Yunhui, Li Xiaohui, a kind of fluorination POSS composite organic coating of the strong of Zhang Kai and preparation side
Method and ice-covering-proof 104263238 B of application .CN, 2017).The structural formula of the fluorinated poss of synthesis are as follows:
In formula, R is-OSiH (CH3)2Group is-OSi (CH3)2CH2CH(CH3)COOCH2CH2C5F13Group, every kind
The number of group is 1~7, and the sum of number of two kinds of groups is 8.
The structural formula of both-end hydrogen dimethyl silicone polymer are as follows:
In formula, the molecular weight of both-end hydrogen dimethyl silicone polymer is 500~20000.
First technical solution of the invention is a kind of preparation method for patterning polysiloxanes ice-covering-proof coating, by branching
Shape dimethyl silicone polymer is uniformly mixed with fluorinated poss, both-end hydrogen dimethyl silicone polymer, is changed
The temperature and humidity of surface drying, heat cross-linking film-forming obtain the ice-covering-proof coating with patterned surface by breathing pattern method.
The method specifically includes following steps:
1) by branching shape dimethyl silicone polymer and fluorinated poss, both-end hydrogen polydimethylsiloxanes
Alkane and catalyst, which are dissolved in solvent, is made into mixed solution, and 1~3h of concussion makes solution uniformly be mixed to get mixed solution；
Wherein, the mass percent of each component are as follows:
Branching shape dimethyl silicone polymer: 3~10%；
Fluorinated poss: 0~5%；
Both-end hydrogen dimethyl silicone polymer: 10~20%；
Catalyst: 0.01~0.12%；
Surplus is solvent；
2) it takes the mixed solution of 200~500 μ L to be coated in substrate surface, changes the temperature and humidity of surface drying, surface drying time
For 2~4h；
3) it is put into 80~120 DEG C of convection ovens and is crosslinked 2~4h film forming, obtain patterning polysiloxanes ice-covering-proof coating.
Catalyst is one of Karstedt ' s catalyst or chloroplatinic acid catalyst in step 1) of the present invention.
Solvent is toluene, dimethylbenzene, benzotrifluoride, methylene chloride, chloroform, curing in step 1) of the present invention
One of carbon or tetrahydrofuran.
At 15~45 DEG C, relative humidity controls the high humidity 45~85% for base material temperature control in step 2) of the present invention
In environment.
Second technical solution of the invention is gathered using patterning polysiloxanes ice-covering-proof coating obtained by the above method
Siloxanes ice-covering-proof coating with a thickness of 150~250 μm, coating surface forms patterning regular texture, the poly- silicon of test patternization
Down to 15kPa, wear-resistant number is up to 2500 times the ice shear strength of oxygen alkane ice-covering-proof coating.
Beneficial effect
Patterning polysiloxanes ice-covering-proof coating of the present invention and preparation method thereof is easy to operate, mild controllable.Figure
The ice shear strength of case ice-covering-proof coating patterns ice-covering-proof coating with good mechanical stability down to 15kPa,
Wear-resistant number is up to 2500 times, has achieved the purpose that ice-covering-proof, illustrates that this coating can be widely used in ice-covering-proof field.
Detailed description of the invention
Fig. 1 is patterning polysiloxanes ice-covering-proof coating structural schematic diagram.
Fig. 2 is patterning polysiloxanes ice-covering-proof coating ice testing device for shear strength schematic diagram.
Fig. 3 is patterning polysiloxanes ice-covering-proof coating wear testing schematic diagram.
Fig. 4 is to pattern the photo after polysiloxanes ice-covering-proof coating is worn 2200 times.
Specific embodiment
Below by case study on implementation technical scheme of the present invention will be further described explanation.Implementation case in detail below
Example is but to be not intended to limit the scope of application of the invention to further explanation of the invention.
Fig. 1 shows patterning polysiloxanes ice-covering-proof coating structural schematic diagram.Fig. 2 is the patterning ice-covering-proof painting of polysiloxanes
Layer ice testing device for shear strength schematic diagram.Fig. 3 is patterning polysiloxanes ice-covering-proof coating wear testing schematic diagram.Fig. 4 is
Pattern the photo after polysiloxanes ice-covering-proof coating is worn 2200 times.
Embodiment 1
Pattern the preparation of polysiloxanes ice-covering-proof coating.Take branching shape dimethyl silicone polymer, the fluorination of 0g of 2g more
Face body oligomeric silsesquioxane (number of si-h bond be 1), the both-end hydrogen dimethyl silicone polymer (molecular weight 20000) of 4g with
And 7 Karstedt ' the s catalyst of μ L uniformly mixed, 14g methylene chloride is made into the concentration of reactant solution as solvent
400 μ L of mixed reaction solution is taken after shaking 1.5h for 30wt%, uniform drop coating is on processed 2cm × 2cm aluminium flake, drop
After painting, it is 15 DEG C that coating, which is placed on temperature, and surface drying 4h in the environment that relative humidity is 45% is then placed in 80 DEG C of baking ovens
In full cross-linked solidification 5h.
The ice shear strength for measuring coating is 29kPa, and wear-resistant number is 1000 times.
Embodiment 2
Pattern the preparation of polysiloxanes ice-covering-proof coating.Take the fluorination of branching the shape dimethyl silicone polymer, 1g of 2.5g
Polyhedral oligomeric silsesquioxane (si-h bond number be 3), the both-end hydrogen dimethyl silicone polymer (molecular weight 500) of 7g and
The chloroplatinic acid catalyst of 17 μ L is uniformly mixed, and as solvent, the concentration for being made into reactant solution is 29.5g carbon disulfide
21wt% takes 500 μ L of mixed reaction solution, for uniform drop coating on processed 2cm × 2cm aluminium flake, drop coating is complete after shaking 3h
Bi Hou, it is 25 DEG C that coating, which is placed on temperature, and surface drying 2h in the environment that relative humidity is 60% is then placed in 120 DEG C of baking ovens
Full cross-linked solidification 2h.
The ice shear strength for measuring coating is 30kPa, and wear-resistant number is 1800 times.
Embodiment 3
Pattern the preparation of polysiloxanes ice-covering-proof coating.Take the fluorination of branching the shape dimethyl silicone polymer, 1.5g of 4g
Polyhedral oligomeric silsesquioxane (number of si-h bond be 7), (molecular weight is the both-end hydrogen dimethyl silicone polymer of 10g
10000) and Karstedt ' the s catalyst of 13 μ L is uniformly mixed, and 34.5g methylene chloride is made into reactant as solvent
The concentration of solution is that 31wt% takes 330 μ L of mixed reaction solution, uniform drop coating is in processed 2cm × 2cm after shaking 2h
On aluminium flake, after drop coating, it is 45 DEG C that coating, which is placed on temperature, then surface drying 3h in the environment that relative humidity is 85% is put
Enter full cross-linked solidification 3.5h in 100 DEG C of baking ovens.
The ice shear strength for measuring coating is 26kPa, and wear-resistant number is 2200 times.
Embodiment 4
Pattern the preparation of polysiloxanes ice-covering-proof coating.Take the fluorination of branching the shape dimethyl silicone polymer, 2.5g of 5g
Polyhedral oligomeric silsesquioxane (number of si-h bond be 5), (molecular weight is the both-end hydrogen dimethyl silicone polymer of 10g
12000) and the chloroplatinic acid catalyst of 70 μ L is uniformly mixed, and 32.5g toluene is made into the dense of reactant solution as solvent
Degree is that 35wt% takes 200 μ L of mixed reaction solution after shaking 2h, and uniform drop coating is on processed 2cm × 2cm aluminium flake, drop
After painting, it is 20 DEG C that coating, which is placed on temperature, and surface drying 2h in the environment that relative humidity is 75% is then placed in 100 DEG C of bakings
Full cross-linked solidification 3h in case.
The ice shear strength for measuring coating is 15kPa, and wear-resistant number is 2500 times.
Embodiment 5
Pattern the preparation of polysiloxanes ice-covering-proof coating.Take branching shape dimethyl silicone polymer, the fluorination of 1g of 2g more
Face body oligomeric silsesquioxane (number of si-h bond be 4), the both-end hydrogen dimethyl silicone polymer (molecular weight 7000) of 5g with
And 8 Karstedt ' the s catalyst of μ L uniformly mixed, 42g benzotrifluoride is made into the concentration of reactant solution as solvent
450 μ L of mixed reaction solution is taken, uniform drop coating is on processed 2cm × 2cm aluminium flake, drop coating after shaking 1h for 16wt%
After, it is 15 DEG C that coating, which is placed on temperature, and surface drying 4h in the environment that relative humidity is 45% is then placed in 90 DEG C of baking ovens
Full cross-linked solidification 4h.
The ice shear strength for measuring coating is 32kPa, and wear-resistant number is 1600 times.
Embodiment 6
Pattern the preparation of polysiloxanes ice-covering-proof coating.Take the fluorination of branching the shape dimethyl silicone polymer, 2g of 4.5g
Polyhedral oligomeric silsesquioxane (number of si-h bond is 6), the both-end hydrogen dimethyl silicone polymer (molecular weight 17000) of 7g
And 25 Karstedt ' the s catalyst of μ L uniformly mixed, 36.5g chloroform is made into reactant solution as solvent
Concentration is 27wt%, shake 1h after, take 400 μ L of mixed reaction solution, uniform drop coating on processed 2cm × 2cm aluminium flake,
After drop coating, it is 35 DEG C that coating, which is placed on temperature, and surface drying 4h in the environment that relative humidity is 70% is then placed in 90 DEG C of bakings
Full cross-linked solidification 4h in case.
The ice shear strength for measuring coating is 20kPa, and wear-resistant number is 1500 times.
Embodiment 7
Pattern the preparation of polysiloxanes ice-covering-proof coating.Take the fluorination of branching the shape dimethyl silicone polymer, 2.5g of 3g
Polyhedral oligomeric silsesquioxane (number of si-h bond is 5), the both-end hydrogen dimethyl silicone polymer (molecular weight 13000) of 6g
And 35 Karstedt ' the s catalyst of μ L uniformly mixed, 38.5g tetrahydrofuran is made into reactant solution as solvent
Concentration is 23wt%, after shaking 1.5h, takes 250 μ L of mixed reaction solution, uniform drop coating is in processed 2cm × 2cm aluminium flake
On, after drop coating, it is 25 DEG C that coating, which is placed on temperature, and surface drying 3h in the environment that relative humidity is 65% is then placed in 110
Full cross-linked solidification 2.5h in DEG C baking oven.
The ice shear strength for measuring coating is 25kPa, and wear-resistant number is 1700 times.
A kind of patterning polysiloxanes ice-covering-proof coating and preparation method thereof that the present invention is disclosed and proposed, art technology
Personnel can be by using for reference present disclosure, and the appropriate links such as condition route that change are realized, although method of the invention has passed through preferably
Examples of implementation are described, and related technical personnel can obviously not depart from spirit of that invention, range and content to this paper institute
The methods and techniques route stated is modified or reconfigures, to realize final technology of preparing.In particular, it should be pointed out that institute
There are similar replacement and change apparent to those skilled in the art, they are considered as being included in the present invention
In spirit, range and content.
Claims (7)
1. a kind of preparation method for patterning polysiloxanes ice-covering-proof coating, characterized in that by branching shape dimethyl silicone polymer
It is uniformly mixed with fluorinated poss, both-end hydrogen dimethyl silicone polymer, changes the temperature and humidity of surface drying,
Heat cross-linking film-forming obtains the ice-covering-proof coating with patterned surface by breathing pattern method.
2. a kind of preparation method for patterning polysiloxanes ice-covering-proof coating according to claim 1, characterized in that specific
Include the following steps:
1) by branching shape dimethyl silicone polymer and fluorinated poss, both-end hydrogen dimethyl silicone polymer with
And catalyst is dissolved in solvent and is made into mixed solution, 1~3h of concussion makes solution uniformly be mixed to get mixed solution；
2) it taking the mixed solution of 200~500 μ L to be coated in substrate surface, changes the temperature and humidity of surface drying, surface drying time is 2~
4h；
3) it is put into 80~120 DEG C of convection ovens and is crosslinked 2~4h film forming, obtain patterning polysiloxanes ice-covering-proof coating.
3. a kind of preparation method for patterning polysiloxanes ice-covering-proof coating according to claim 2, characterized in that described
The mass percent of each component in step 1) are as follows:
Branching shape dimethyl silicone polymer: 3~10%；
Fluorinated poss: 0~5%；
Both-end hydrogen dimethyl silicone polymer: 10~20%；
Catalyst: 0.01~0.12%；
Surplus is solvent.
4. a kind of preparation method for patterning polysiloxanes ice-covering-proof coating according to claim 2, characterized in that described
Catalyst is one of Karstedt ' s catalyst or chloroplatinic acid catalyst in step 1).
5. a kind of preparation method for patterning polysiloxanes ice-covering-proof coating according to claim 2, characterized in that described
Solvent is one in toluene, dimethylbenzene, benzotrifluoride, methylene chloride, chloroform, carbon disulfide or tetrahydrofuran in step 1)
Kind.
6. a kind of preparation method for patterning polysiloxanes ice-covering-proof coating according to claim 2, characterized in that described
At 15~45 DEG C, relative humidity is controlled in 45~85% high humidity environment for base material temperature control in step 2).
7. the patterning polysiloxanes ice-covering-proof coating that preparation method according to any one of claim 1 to 6 obtains,
Be characterized in, polysiloxanes ice-covering-proof coating with a thickness of 150~250 μm, coating surface forms patterning regular texture, test chart
Down to 15kPa, wear-resistant number is up to 2500 times the ice shear strength of case polysiloxanes ice-covering-proof coating.
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| CN113201170B (en) * | 2021-05-12 | 2022-11-29 | 慕思健康睡眠股份有限公司 | Graphene polyurethane composite sponge material with good anti-fouling performance and application thereof |
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