CN113337174B - Preparation method of super-hydrophobic coating with high light transmittance and high haze - Google Patents
Preparation method of super-hydrophobic coating with high light transmittance and high haze Download PDFInfo
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Abstract
The invention relates to the field of super-hydrophobic materials, in particular to a preparation method of a high-light-transmittance and high-haze super-hydrophobic coating. The invention takes octachloropropyl polyhedral oligomeric silsesquioxane, styrene, 2-2 bipyridyl and cuprous chloride as raw materials to synthesize a star-shaped copolymer POSS-PS by an atom transfer radical polymerization method. The star-shaped copolymer POSS-PS and the prepared room temperature curing silicone rubber are dissolved in a solvent by a non-solvent phase separation method (NIPS), and then mixed and poured into a non-solvent coagulating bath containing a matrix to obtain the super-hydrophobic coating. The preparation method is simple and easy to operate, and the prepared coating has the characteristics of super-hydrophobicity, adhesion resistance, self-cleaning property, high temperature resistance, high light transmittance, high haze and the like.
Description
Technical Field
The invention relates to the field of super-hydrophobic materials, in particular to a preparation method of a high-light-transmittance and high-haze super-hydrophobic coating.
Background
The cluster structure on the surface of the loaded leaf is beneficial to locking air, prevents the inspiration of water from wetting the surface, and can prepare the super-hydrophobic material with a contact angle of over 150 degrees and good wettability. The preparation method of the super-hydrophobic material with the unique microstructure is various and comprises an etching method, a template method, a femtosecond laser etching method, a photoetching method, a casting method, an in-situ polymerization method, an electrochemical method, a self-assembly method, an electrostatic spinning method, a spin-coating method and the like. The method has wide application and very wide prospect in the fields of self-cleaning, corrosion prevention, ice thinning prevention, battery interference shielding, self-repairing, liquid drop control, pipeline transportation, oil-water separation, biomedicine and the like. In the earlier research, the preparation method of the CN202010040398.7 hydrophobic star polymer porous membrane firstly synthesizes POSS-b-PS-b-PHEMA star copolymer and prepares the porous membrane by a breathing pattern method. And then the porous membrane is infused with the modified silicone oil to prepare the hydrophobic star polymer porous membrane, the light transmittance of which is close to that of glass, but the hydrophobicity of which is less than 150 degrees and does not reach a super-hydrophobic state. And wherein no investigation of haze problems was involved. In general, a material with high light transmittance has low haze, and it is difficult to satisfy the effects of high haze and high light transmittance at the same time. Therefore, how to prepare the super-hydrophobic coating and solve the problems of high light transmittance and low haze are the research direction of the invention.
Disclosure of Invention
The invention provides a preparation method of a super-hydrophobic coating with high light transmittance and high haze, and the preparation method is simple and convenient in process and simple in reaction conditions. The prepared super-hydrophobic coating has good hydrophobic property, high light transmittance and high haze.
In order to achieve the purpose, the invention adopts the following scheme:
(1) synthesis of Star-shaped copolymer POSS-PS
Styrene, octachloropropyl polyhedral oligomeric silsesquioxane, cuprous chloride, 2' -bipyridyl and solvent N, N-dimethylformamide are added into a Schlenk bottle, and the mixture is reacted for 24 hours at 110 ℃ by an Atom Transfer Radical Polymerization (ATRP) method to obtain a product. And then, after cuprous chloride is removed from the product by passing through an alkaline alumina column, the product is precipitated in methanol, and the star-shaped copolymer POSS-PS is obtained after vacuum drying.
Further, the mol ratio of the octachloropropyl polyhedral oligomeric silsesquioxane to the cuprous chloride to the 2, 2' -bipyridyl to the styrene is 1: 1: 3: 100-200. The volume ratio of the styrene to the solvent N, N-dimethylformamide is 2-4: 1.
(2) synthesizing room temperature curing silicone rubber;
uniformly mixing hydroxyl-terminated polydimethylsiloxane and methyltributanoxime silane (D-30) at the mass ratio of 10:1 at room temperature for about 10min to obtain room-temperature curing silicone rubber;
(3) preparation of super-hydrophobic coatings
And (3) weighing the star-shaped copolymer POSS-PS in the step (1) and the room-temperature curing silicone rubber prepared in the step (2), respectively dissolving in a solvent, and performing ultrasonic dissolution to obtain a mixed solution. And (3) placing the glass substrate in a non-solvent coagulation bath, settling, pouring the mixed solution into the non-solvent coagulation bath, and volatilizing the solvent and the non-solvent to obtain the super-hydrophobic coating.
Further, the solvent is one or a mixture of two of dichloromethane and trichloromethane; the non-solvent is one or two of n-hexane and acetone. The invention selects normal hexane and acetone as non-solvent, can obtain coating with good forming effect, if other solvents are used, the coating is not beneficial to forming, and the light transmittance, haze and contact angle of the coating can be influenced.
Further, the concentration of the star-shaped copolymer POSS-PS in the solvent is 10-25 mg/ml; the concentration of the room temperature curing silicone rubber in the solvent is 0.4-2 times of that of the star-shaped copolymer POSS-PS.
Compared with the prior art, the invention has the following excellent effects: the star-shaped copolymer POSS-PS is synthesized by an atom transfer radical polymerization method, the star-shaped copolymer POSS-PS and prepared room-temperature curing silicone rubber are dissolved in a solvent by a non-solvent phase separation method (NIPS), and then the mixture is poured into a non-solvent coagulating bath containing a matrix to obtain the super-hydrophobic coating. The preparation method is simple and easy to operate, and the prepared coating has the characteristics of super-hydrophobicity, adhesion resistance, self-cleaning property, high temperature resistance, high light transmittance, high haze and the like.
Drawings
FIG. 1 is a Fourier infrared spectrum of a star-shaped copolymer POSS-PS of example 1;
FIG. 2 is a diagram of the star copolymer POSS-PS of example 11H nuclear magnetic map;
in fig. 3 a is a graph of the static contact angle of example 1, which is 151 °. The right panel b is a static contact angle diagram for comparative example 1, with a contact angle of 100 °.
FIG. 4 is a scanning electron micrograph of the superhydrophobic coating of example 1; the coating surface is composed of a plurality of microspheres.
Detailed Description
Example 1
(1) Synthesis of Star-shaped copolymer POSS-PS
0.42g octachloropropyl polyhedral oligomeric silsesquioxane, 0.04g cuprous chloride and 0.2g 2, 2' -bipyridine, 9.2ml styrene, 3ml N, N-dimethylamide were added to a Schlenk bottle, and reacted at 110 ℃ for 24 hours by an Atom Transfer Radical Polymerization (ATRP) method to synthesize a star-shaped copolymer POSS-PS.
(2) Synthesis of Room temperature curing Silicone rubber
10g of the hydroxyl-terminated polysiloxane and 1g were mixed uniformly to give a room-temperature-curing silicone rubber.
(3) Preparing a super-hydrophobic coating;
weighing 20mg of star-shaped copolymer POSS-PS star-shaped copolymer, dissolving in 1ml of dichloromethane (the solubility is 20mg/ml), dissolving 10mg of room-temperature curing silicone rubber in 1ml of dichloromethane, respectively carrying out ultrasonic treatment until the solution is dissolved, and uniformly mixing the two solutions according to the volume of 1:1 to obtain a mixed solution. And (3) placing the glass substrate in a normal hexane coagulation bath, then pouring the mixed solution into the normal hexane coagulation bath containing the substrate, and obtaining the super-hydrophobic coating after the solvent and the non-solvent are volatilized and dried.
FIG. 1 is a Fourier infrared spectrum of a star-shaped copolymer POSS-PS of example 1; 3100-3000cm-1 is a telescopic vibration peak of a C-H bond of a benzene ring, 1601-1493cm-1 is an infrared characteristic absorption peak of a benzene ring framework vibration peak. 1028cm-1 is the absorption peak of the-Si-O-bond, and 906cm-1 is the infrared characteristic peak of Si-C. And the infrared characteristic peak of C-Cl bond of POSS and C ═ C bond of monomer styrene does not appear in the figure, which shows that Si-Cl disappears, C ═ C bond is opened, and POSS and styrene react to successfully synthesize the POSS-PS star copolymer.
FIG. 2 is a diagram of the star copolymer POSS-PS of example 11H nuclear magnetic map. The characteristic peak at δ of 0.89 ppm is caused by hydrogen on-CH 2-Si on chloropropyl group in POSS, chemical shifts on vinyl group of styrene are at δ of 1.44ppm, 1.84ppm, chemical shifts of hydrogen on benzene ring of styrene are at δ of 6.60ppm and 7.08ppm, and the characteristic peak at 7.28 ppm is chemical shift of solvent deuterated chloroform.
FIG. 4 is a scanning electron micrograph of the superhydrophobic coating of example 1; the coating surface is composed of a plurality of microspheres.
Comparative example 1(1)
Comparative example 1(1) compared to example 1, the difference is that: the glass substrate was not placed in a n-hexane coagulation bath.
(1) Firstly, respectively synthesizing star-shaped copolymer POSS-PS and room-temperature curing silicone rubber; same as example 1;
(2) weighing 20mg of star-shaped copolymer POSS-PS star-shaped copolymer to be dissolved in 1ml of dichloromethane (the solubility is 20mg/ml), dissolving 10mg of room temperature curing silicone rubber in 1ml of dichloromethane, and respectively carrying out ultrasonic treatment until the mixture is dissolved to obtain a mixed solution. And directly putting the base material into the mixed solution, and volatilizing and airing the solvent to obtain the coating.
The non-solvent coagulation bath of example 1 precipitated the polymer as microspheres to give a coating, whereas comparative example 1 was a film-like coating, the coagulation bath affected the surface morphology of the coating and ultimately the light transmittance, haze and hydrophobicity of the coating.
In comparison with example 1, if ethanol or/and water is used as the non-solvent coagulation bath, the experimental results show that: the flocculent precipitate in the coating can not be uniformly formed, the coating appearance of the embodiment 1 is difficult to obtain, and the effects of light transmittance, haze and hydrophobicity are greatly reduced.
Comparative examples 1(2)
Comparative example 1(2) compared to example 1, the difference is that: no room temperature curing silicone rubber was added.
(1) Synthesizing a star-shaped copolymer POSS-PS; same as example 1;
(2) 20mg of star-shaped copolymer POSS-PS star-shaped copolymer is weighed and dissolved in 1ml of dichloromethane (the solubility is 20mg/ml) and ultrasonic treatment is carried out until the star-shaped copolymer POSS-PS star-shaped copolymer is dissolved. And placing the glass substrate in a normal hexane coagulation bath, then pouring the solution into the normal hexane coagulation bath for placing the substrate, and obtaining the coating after the solvent and the non-solvent are volatilized and dried.
Comparative examples 1(3)
Comparative example 1(3) compared to example 1, the difference is that: the star copolymer POSS-PS was not added.
(1) Synthesizing room temperature curing silicone rubber; same as example 1;
(2) 10mg of room temperature curing silicone rubber was dissolved in 1ml of methylene chloride and sonicated until dissolved. And (3) placing the substrate in a normal hexane coagulation bath, then pouring the solution into the normal hexane coagulation bath for placing the glass substrate, and drying to obtain the coating after the solvent and the non-solvent are volatilized.
Example 2
(1) Synthesis of Star-shaped copolymer POSS-PS
0.42g of octachloropropyl polyhedral oligomeric silsesquioxane, 0.04g of cuprous chloride and 0.2g of 2, 2' -bipyridyl, 6.9ml of styrene and 2ml of N, N-dimethylamide are added into a Schlenk bottle and reacted for 24 hours at 110 ℃ by an Atom Transfer Radical Polymerization (ATRP) method to synthesize the star-shaped copolymer POSS-PS.
(2) Room temperature curing silicone rubber was synthesized as in example 1;
(3) a superhydrophobic coating was prepared as in example 1.
Comparative example 2
(1) Synthesizing star-shaped copolymer POSS-PS, and performing the same operation as the step (1) in the example 2;
(2) synthesizing room temperature curing silicone rubber; the same as example 2;
(3) weighing 20mg of star-shaped copolymer POSS-PS star-shaped copolymer, dissolving in 1ml of dichloromethane (the solubility is 20mg/ml), dissolving 10mg of room-temperature curing silicone rubber in 1ml of dichloromethane, respectively carrying out ultrasonic treatment until the two solutions are dissolved, uniformly mixing the two solutions to obtain a mixed solution, putting a glass substrate into the mixed solution, and drying the glass substrate after the solvent is volatilized to obtain the coating.
Example 3
(1) Synthesis of Star-shaped copolymer POSS-PS
0.42g octachloropropyl polyhedral oligomeric silsesquioxane, 0.04g cuprous chloride and 0.2g 2, 2' -bipyridine, 4.6ml styrene, 1.6ml N, N-dimethyl amide were added into a Schlenk bottle, and reacted at 110 ℃ for 24 hours by an Atom Transfer Radical Polymerization (ATRP) method to synthesize a star-shaped copolymer POSS-PS.
(2) Room temperature curing silicone rubber was synthesized as in example 1;
(3) a superhydrophobic coating was prepared as in example 1.
Comparative example 3
(1) Synthesizing star-shaped copolymer POSS-PS, and performing the same operation as the step (1) in the example 3;
(2) synthesizing room temperature curing silicone rubber; the same as in example 3;
(3) weighing 20mg of star-shaped copolymer POSS-PS star-shaped copolymer, dissolving in 1ml of dichloromethane (the solubility is 20mg/ml), dissolving 10mg of room-temperature curing silicone rubber in 1ml of dichloromethane, respectively carrying out ultrasonic treatment until the solution is dissolved, and uniformly mixing the two solutions to obtain a mixed solution. And putting the base material into the mixed solution, and volatilizing and airing the solvent to obtain the coating.
Example 4
(1) Synthesizing star-shaped copolymer POSS-PS as in example 1;
(2) room temperature curing silicone rubber was synthesized as in example 1;
(3) weighing 25mg of star-shaped copolymer POSS-PS star-shaped copolymer, dissolving in 1ml of dichloromethane (the solubility is 25mg/ml), dissolving 10mg of room-temperature curing silicone rubber in 1ml of dichloromethane, respectively carrying out ultrasonic treatment until the solution is dissolved, and mixing the two solutions uniformly according to the volume ratio of 1:1 to obtain a mixed solution. And placing the glass substrate in a normal hexane coagulation bath, pouring the mixed solution into the normal hexane coagulation bath containing the glass substrate, and volatilizing and airing the solvent and the non-solvent to obtain the super-hydrophobic coating.
Comparative example 4
(1) Synthesizing star-shaped copolymer POSS-PS as in example 4;
(2) room temperature curing silicone rubber was synthesized as in example 4;
(3) weighing 25mg of star-shaped copolymer POSS-PS star-shaped copolymer, dissolving in 1ml of dichloromethane (the solubility is 25mg/ml), dissolving 10mg of room-temperature curing silicone rubber in 1ml of dichloromethane, respectively carrying out ultrasonic treatment until the solution is dissolved, and uniformly mixing the two solutions to obtain a mixed solution. And putting the glass substrate into the mixed solution, and volatilizing and airing the solvent to obtain the coating.
Example 5
(1) Synthesizing star-shaped copolymer POSS-PS as in example 1;
(2) room temperature curing silicone rubber was synthesized as in example 1;
(3) weighing 20mg of star-shaped copolymer POSS-PS star-shaped copolymer, dissolving in 1ml of dichloromethane (the solubility is 20mg/ml), dissolving 20mg of room-temperature curing silicone rubber in 1ml of dichloromethane, respectively carrying out ultrasonic treatment until the solution is dissolved, and uniformly mixing the two solutions to obtain a mixed solution. And placing the glass substrate in a normal hexane coagulating bath, pouring the mixed solution into the normal hexane coagulating bath for placing the substrate, and volatilizing and airing the solvent and the non-solvent to obtain the super-hydrophobic coating.
Comparative example 5
(1) Synthesizing star-shaped copolymer POSS-PS as in example 5;
(2) room temperature curing silicone rubber was synthesized as in example 5;
(3) 20mg of star-shaped copolymer POSS-PS star-shaped copolymer is weighed and dissolved in 1ml of dichloromethane (the solubility is 20mg/ml), 20mg of room temperature curing silicone rubber is dissolved in 1ml of dichloromethane, and the mixture is respectively subjected to ultrasonic treatment until the mixture is dissolved. The two solutions are mixed evenly to obtain a mixed solution. And putting the glass substrate into the mixed solution, and volatilizing and airing the solvent to obtain the coating.
Example 6
(1) Synthesis of Star-shaped copolymer POSS-PS, as in example 1
(2) Synthesis of Room temperature curing Silicone rubber, same as example 1
(3) Weighing 20mg of star-shaped copolymer POSS-PS star-shaped copolymer, dissolving in 1ml of dichloromethane (the solubility is 20mg/ml), dissolving 30mg of room-temperature curing silicone rubber in 1ml of dichloromethane, respectively carrying out ultrasonic treatment until the solution is dissolved, and uniformly mixing the two solutions to obtain a mixed solution. And placing the glass substrate in a normal hexane coagulating bath, pouring the mixed solution into the normal hexane coagulating bath for placing the substrate, and volatilizing and airing the solvent and the non-solvent to obtain the super-hydrophobic coating.
Comparative example 6
(1) Synthesizing star-shaped copolymer POSS-PS as in example 6;
(2) room temperature curing silicone rubber was synthesized as in example 6;
(3) 20mg of star-shaped copolymer POSS-PS star-shaped copolymer is weighed and dissolved in 1ml of dichloromethane (the solubility is 20mg/ml), 30mg of room temperature curing silicone rubber is dissolved in 1ml of dichloromethane, and the mixture is respectively subjected to ultrasonic treatment until the mixture is dissolved. The two solutions are mixed evenly to obtain a mixed solution. And putting the glass substrate into the mixed solution, and volatilizing and airing the solvent to obtain the coating.
Example 7
(1) Synthesizing star-shaped copolymer POSS-PS as in example 1;
(2) room temperature curing silicone rubber was synthesized as in example 1;
(3) weighing 20mg of star-shaped copolymer POSS-PS star-shaped copolymer, dissolving in 1ml of dichloromethane (the solubility is 20mg/ml), dissolving 40mg of room-temperature curing silicone rubber in 1ml of dichloromethane, respectively carrying out ultrasonic treatment until the solution is dissolved, and uniformly mixing the two solutions to obtain a mixed solution. And (3) placing the substrate in a normal hexane coagulation bath, then pouring the mixed solution into the normal hexane coagulation bath for placing the substrate, and obtaining the super-hydrophobic coating after the solvent and the non-solvent are volatilized and dried.
Comparative example 7
(1) Synthesis of Star-shaped copolymer POSS-PS, as in example 7;
(2) room temperature curing silicone rubber was synthesized as in example 7;
(3) 20mg of star-shaped copolymer POSS-PS star-shaped copolymer is weighed and dissolved in 1ml of dichloromethane (the solubility is 20mg/ml), 40mg of room temperature curing silicone rubber is dissolved in 1ml of dichloromethane, and the mixture is respectively subjected to ultrasonic treatment until the mixture is dissolved. The two solutions are mixed evenly to obtain a mixed solution. And putting the glass substrate into the mixed solution, and volatilizing and airing the solvent to obtain the coating.
The coatings prepared in the above examples and comparative examples were measured for contact angle, haze and transmittance, and the coatings were measured for transmittance and haze using a WGT-S transmittance haze measuring apparatus (Shanghai precision scientific instruments Co., Ltd.).
The results are shown in Table 1.
TABLE 1 contact angle, light transmittance and haze of the coatings
Claims (5)
1. A preparation method of a super-hydrophobic coating with high light transmittance and high haze is characterized by comprising the following steps: the preparation method comprises the following steps:
(1) synthesizing a star-shaped copolymer POSS-PS; synthesizing a star copolymer POSS-PS by using octachloropropyl polyhedral oligomeric silsesquioxane as an initiator, styrene as a reaction monomer, cuprous chloride and a 2, 2' -bipyridyl complex as a catalyst and N, N-dimethylformamide as a solvent through an Atom Transfer Radical Polymerization (ATRP) method under the conditions of removing oxygen and water;
(2) synthesizing room temperature curing silicone rubber: uniformly mixing hydroxyl-terminated polydimethylsiloxane and methyl tributyrinoxime silane to obtain room-temperature curing silicone rubber; uniformly mixing hydroxyl-terminated polydimethylsiloxane and methyl tributyrinoxime silane according to the mass ratio of 10: 1;
(3) preparing a super-hydrophobic coating: dissolving the star-shaped copolymer POSS-PS and the prepared room-temperature curing silicone rubber in a solvent, pouring the mixture into a normal hexane or/and acetone non-solvent coagulation bath containing a substrate, and obtaining the super-hydrophobic coating after the solvent and the non-solvent are volatilized and dried.
2. The method of preparing a high light transmittance and high haze superhydrophobic coating of claim 1, wherein: octachloropropyl polyhedral oligomeric silsesquioxane, cuprous chloride, 2-2 bipyridyl and styrene in a molar ratio of 1: 1: 3: 100-200.
3. The method of preparing a high light transmittance and high haze superhydrophobic coating of claim 1, wherein: the volume ratio of the styrene to the solvent N, N-dimethylformamide is 2-4: 1.
4. the method of preparing a high light transmittance and high haze superhydrophobic coating of claim 1, wherein: the solvent in the step (3) is dichloromethane or/and trichloromethane.
5. The method of preparing a high light transmittance and high haze superhydrophobic coating of claim 1, wherein: the concentration of the star-shaped copolymer POSS-PS is 10-25mg/ml, and the concentration of the room temperature curing silicone rubber is 0.4-2 times that of the star-shaped copolymer POSS-PS.
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