CN114457592B - Method for preparing super-amphiphobic fabric by using semitransparent fluorosilane polymer emulsion - Google Patents
Method for preparing super-amphiphobic fabric by using semitransparent fluorosilane polymer emulsion Download PDFInfo
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- C08G77/04—Polysiloxanes
- C08G77/22—Polysiloxanes containing silicon bound to organic groups containing atoms other than carbon, hydrogen and oxygen
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- D06M2101/16—Synthetic fibres, other than mineral fibres
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- D06M2101/16—Synthetic fibres, other than mineral fibres
- D06M2101/30—Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
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- D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
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- D06M2200/10—Repellency against liquids
- D06M2200/12—Hydrophobic properties
Abstract
The invention relates to a method for preparing super-amphiphobic fabrics by using semitransparent fluorosilane polymer emulsion, which comprises the following steps: 1. the semitransparent fluorosilane polymer emulsion is prepared by using water as a solvent, acid as a catalyst and a cationic surfactant as a dispersing agent, forming a fluorosilane polymer through hydrolysis and condensation of fluorosilane, and performing ultrasonic treatment. The resulting emulsion had the following characteristics: (1) The solution has semitransparent state, and the light transmittance at 600nm reaches 91.7 percent (taking distilled water as a reference); (2) Excellent stability, and good uniformity is maintained after the composition is placed in a 60 ℃ oven for 96 hours, frozen and thawed 3 times or placed at room temperature for 10 months. 2. Soaking the fabric in the fluorosilane polymer emulsion and curing at a certain temperature to obtain the super-amphiphobic fabric. The technology of the invention also has the advantages of easy scale, low cost, safe production and the like, and has wide application prospect.
Description
Technical Field
The invention relates to a preparation method of super-amphiphobic fabric, in particular to a method for preparing super-amphiphobic fabric by using semitransparent fluorosilane polymer emulsion.
Background
The surface with super amphiphobic function has important application value in the aspects of water resistance, oil resistance, pollution resistance, self cleaning and the like. The fluorosilane polymer provides low surface energy, and the micro-nano particles are utilized to provide a coarse structure, so that the method is an effective method for realizing the super-amphiphobic function.
At present, organic solvents such as ethanol, acetone, dimethylformamide, tetrahydrofuran, alkane, fluoroalkane and the like are mainly used for dispersing fluorosilane. However, the use of organic solvents creates a great safety hazard and environmental pollution problem, and also increases manufacturing costs. Meanwhile, the production process has a certain degree of harm to operators. Water is a green solvent compared to organic solvents, but is rarely used to make super-amphiphobic fabrics because low surface energy materials often do not dissolve or disperse well in water, resulting in delamination of the solution, precipitation or substantial adhesion of the fluorosilane polymer to the bottle wall, thereby severely affecting the super-amphiphobic function.
Chinese patent CN111501352a uses silane and silane coupling agent to prepare aqueous suspension and is used to prepare superhydrophobic fabric; chinese patent CN104789124B uses alcohol-water mixture, organosilane and nanoparticles to prepare suspension for preparing super-amphiphobic coating; chinese patent No. 106800885A is a suspension prepared by dehydration condensation of dispersed nanoparticles and organosilane for preparing transparent super-hydrophobic super-amphiphobic coating. Although the surfaces with good superhydrophobic and superhydrophobic properties are prepared by the methods, the prepared solutions are suspension, so that the solutions are likely to be settled and layered after being placed for a long time, and the convenience and even the use effect of the solutions are further affected. Therefore, storage and long-term use of the suspension are difficult.
In current aqueous solutions of dispersed fluorosilane polymers, fluorosurfactants are typically employed to effect dispersion. Chinese patent No. 112457438A adopts a gemini fluorine-containing surfactant (fine chemicals) to achieve the purpose of dispersing perfluoropolyether, but the method has complex process (long-time maintenance at 90-100 ℃ and nitrogen protection, etc.), does not relate to long-term storage stability of the solution, and is not beneficial to the application thereof. Chinese patent No. CN109233482A uses fluorocarbon surfactant vinyl 321 to disperse heptadecafluorodecyl triethoxysilane and heptadecatrimethoxysilane. The surfactant used in the method is only zolyl 321, the selection range is narrow, and the uniformity and long-term placement stability of the obtained solution are not related, so that the application of the surfactant is restricted. At the same time, non-fluorosurfactants are generally less expensive than fluorosurfactants. For example, the fluorocarbon surfactant Capstone FS-3100 (newer product of vinyl 321) has a price of 1600 yuan/kg, while cetyltrimethylammonium bromide has a price of 38 yuan/kg. In addition, the present research and technical invention focuses mainly on the properties of the obtained fabrics, neglecting the transportation and storage stability of the solutions, which are critical constraints faced by the application.
Disclosure of Invention
The invention aims to provide a semitransparent fluorosilane polymer emulsion and a method for preparing a super-amphiphobic fabric by using the same, so as to solve the problems of poor dispersibility and stability of the existing super-amphiphobic emulsion and unfavorable long-term storage.
1. Preparation of semitransparent fluorosilane polymer emulsion and super-amphiphobic fabric
(1) Preparation of semitransparent fluorosilane polymer emulsion: and (3) taking water as a solvent, acid as a catalyst, and a cationic surfactant as a dispersing agent, performing hydrolytic condensation reaction on fluorosilane and a silane coupling agent for 1-24 hours at the temperature of 25-40 ℃, and performing ultrasonic treatment to obtain the semitransparent fluorosilane polymerization emulsion. The acid is one of sulfuric acid, hydrochloric acid, acetic acid and oxalic acid, and the mass fraction of the acid in the reaction system is 0.1-1%. The cationic surfactant is at least two of dodecyl trimethyl ammonium bromide, didodecyl dimethyl ammonium bromide, ditetyl dimethyl ammonium bromide, cetyl trimethyl ammonium bromide and octadecyl trimethyl ammonium chloride, and the mass fraction of the cationic surfactant in the reaction system is 0.1-0.24%. The fluorosilane is one of perfluorodecyl trimethoxy silane, perfluorodecyl triethoxy silane and perfluoropolyether silane, and the mass fraction of the fluorosilane in the reaction system is 0.2-4%. The silane coupling agent is at least one of gamma-aminopropyl trimethoxy silane and gamma- (2, 3-glycidoxy) propyl trimethoxy silane, and the mass fraction of the silane coupling agent in a reaction system is 0.20% or 0.29%.
(2) Preparation of super-amphiphobic fabric: soaking the washed fabric in the semitransparent fluorosilane polymer emulsion for 1-20 min, taking out, press-filtering to remove redundant liquid, and then curing at 140-190 ℃ for 2-10 min to obtain the super-amphiphobic fabric. The fabric comprises a polyester fabric, a nylon fabric, a cotton fabric, a cashmere fabric or a hemp fabric.
2. Semitransparent fluorosilane polymer emulsion and performance evaluation of semitransparent fluorosilane polymer emulsion on preparation of super-amphiphobic fabric
1. Semitransparent fluorosilane polymer emulsion properties
(1) The emulsion is semitransparent. The light transmittance of the emulsion reaches 91.7% at the wavelength of 600nm by taking distilled water as a reference, which shows that the emulsion has good uniformity and provides conditions for storage and long-term use.
(2) Good dispersibility and stability. After 96 hours of standing in an oven at 60 ℃,3 times of freezing and thawing or 10 months of standing at room temperature, good uniformity is still maintained.
2. Evaluation of the Properties of the super-amphiphobic fabrics
Tests prove that the contact angle of 20 mu L of water drops on the surface of the super-amphiphobic fabric prepared by the invention is more than 153.5 degrees, and the rolling angle is less than 6 degrees; the contact angle of 20 mu L soybean oil drop is more than 151.6 DEG, and the rolling angle is less than 10 deg.
In conclusion, the fluorosilane polymer emulsion prepared by the invention is semitransparent, has excellent dispersibility and stability, and the super-surface double of the fabric treated by the fluorosilane polymer emulsion has good super-amphiphobic performance and stability, and has obvious advantages in transportation, storage and application.
Drawings
FIG. 1 is a photograph of a translucent fluorosilane emulsion produced in example 1.
FIG. 2 is a graph showing the change in transmittance with wavelength of the semitransparent fluorosilane emulsion prepared in example 2 (distilled water as a reference).
FIG. 3 is a photograph of 20. Mu.L of water droplets (right side, methylene blue dyeing) and 20. Mu.L of soybean oil droplets (left side) on the super-amphiphobic fabric prepared in example 3.
Detailed Description
The invention is further illustrated by the following examples.
Example 1
(1) Preparation of semitransparent fluorosilane polymer emulsion: 0.5g of perfluorodecyl trimethoxysilane, 0.1g of gamma- (2, 3-epoxypropoxy) propyl trimethoxysilane, 0.25. 0.25 g hydrochloric acid (12 mol/L), 0.03g of dodecyl trimethyl ammonium bromide and 0.09g of hexadecyl trimethyl ammonium bromide are sequentially added into a 100 mL beaker containing 50 mL distilled water, magnetically stirred at 25 ℃ for reaction for 4 hours, and ultrasonic treated for 10 minutes to obtain a uniform semitransparent fluorosilane polymer emulsion.
(2) Preparation of super-amphiphobic fabric: soaking the cleaned polyester fiber fabric in the fluorosilane polymer emulsion for 5 minutes, taking out, removing residual liquid, and curing for 10 minutes at 160 ℃ to obtain the super-amphiphobic fabric.
The resulting translucent fluorosilane polymer emulsion (fig. 1) was left in an oven at 60 ℃ for 96 hours, with good uniformity of the solution; on the surface of the obtained super-amphiphobic fabric, the contact angle of 20 μl of water drop is 155.4 °, the rolling angle is 5 °, the contact angle of 20 μl of soybean oil drop is 152 °, and the rolling angle is 8 °.
Example 2
(1) Preparation of semitransparent fluorosilane polymer emulsion: 0.5g of perfluoro-silicon-based triethoxysilane, 0.1g of gamma- (2, 3-epoxypropoxy) propyl trimethoxysilane, 0.25 g hydrochloric acid (12 mol/L) and 0.03g of didodecyl dimethyl ammonium bromide, and 0.09g of octadecyl trimethyl ammonium chloride are sequentially added into a 100 mL beaker containing 50 mL distilled water, magnetically stirred and reacted for 4 hours at 25 ℃, and then ultrasonic treated for 5 minutes, thus obtaining uniform semitransparent fluorosilane polymer emulsion.
(2) Preparation of super-amphiphobic fabric: soaking the cleaned linen fabric in the fluorosilane polymer emulsion for 8 minutes, taking out, removing redundant residual liquid, and curing for 4 minutes at 180 ℃ to obtain the super-amphiphobic fabric.
The obtained semitransparent fluorosilane polymer emulsion has good light transmittance, and the light transmittance reaches 91.7 percent (taking distilled water as a reference) at the wavelength of 600nm (figure 2); it is placed at the temperature of minus 18 ℃ for 2 hours to freeze, then is placed at the room temperature of 25 ℃ to ablate, and is circulated for 3 times, and the solution still keeps good uniformity; on the surface of the obtained super-amphiphobic fabric, the contact angle of 20 μl of water drop is 156.5 °, the rolling angle is 4 °, the contact angle of 20 μl of soybean oil drop is 152.6 °, and the rolling angle is 8.5 °.
Example 3
(1) Preparation of semitransparent fluorosilane polymer emulsion: 0.75g of perfluoropolyether silane, 0.15g of gamma-aminopropyl trimethoxysilane, 0.25 g of g hydrochloric acid (12 mol/L), 0.03g of dicetyl dimethyl ammonium bromide and 0.09g of cetyltrimethylammonium bromide are sequentially added into a 100 mL beaker containing 50 mL distilled water, and the mixture is magnetically stirred at 25 ℃ for reaction for 8 hours and then subjected to ultrasonic treatment for 5 minutes to obtain a uniform semitransparent fluorosilane polymer emulsion.
(2) Preparation of super-amphiphobic fabric: soaking the cleaned cashmere fabric in the fluorosilane polymer emulsion for 2 minutes, taking out, removing residual liquid, and curing at 170 ℃ for 6 minutes to obtain the super-amphiphobic fabric.
The semitransparent fluorosilane polymer emulsion is placed for 10 months at room temperature, and the solution keeps good uniformity; on the surface of the resulting super-amphiphobic fabric, 20 μl of water droplets had a contact angle of 154 °, a roll angle of 3 °,20 μl of soybean oil droplets had a contact angle of 154.5 °, and a roll angle of 9 ° (fig. 3).
Example 4
(1) Preparation of semitransparent fluorosilane polymer emulsion: 5g of perfluorodecyl triethoxysilane, 1.5g of gamma-aminopropyl trimethoxysilane, 2.5 g g hydrochloric acid (12 mol/L), 0.3g of dicetyl dimethyl ammonium bromide and 0.9g of hexadecyl trimethyl ammonium bromide are sequentially added into a 1000mL beaker containing 500 mL distilled water, and the mixture is magnetically stirred at 30 ℃ for reaction for 12 hours and then is subjected to ultrasonic treatment for 10 minutes, so that uniform semitransparent fluorosilane polymer emulsion is obtained.
(2) Preparation of super-amphiphobic fabric: soaking the cleaned nylon fabric in the fluorosilane polymer emulsion for 3 minutes, taking out, removing residual liquid, and curing for 4 minutes at 180 ℃ to obtain the super-amphiphobic fabric.
On the surface of the obtained super-amphiphobic fabric, the contact angle of 20 μl of water drop is 156.1 °, the rolling angle is 3 °, the contact angle of 20 μl of soybean oil drop is 151.6 °, and the rolling angle is 10 °.
Example 5
(1) Preparation of semitransparent fluorosilane polymer emulsion: 7g of perfluoropolyether silane, 1.0g of gamma-aminopropyl trimethoxy silane, 2.5 g hydrochloric acid (12 mol/L), 0.3g of didodecyl dimethyl ammonium bromide and 0.9g of hexadecyl trimethyl ammonium bromide are sequentially added into a 1000mL beaker containing 500 mL distilled water, and the mixture is magnetically stirred at 40 ℃ for reaction for 16 hours and then subjected to ultrasonic treatment for 10 minutes to obtain a uniform semitransparent fluorosilane polymer emulsion.
(2) Preparation of super-amphiphobic fabric: soaking the cleaned polyester fiber fabric in the fluorosilane polymer emulsion for 3 minutes, taking out, removing residual liquid, and curing at 190 ℃ for 3 minutes to obtain the super-amphiphobic fabric.
On the surface of the obtained super-amphiphobic fabric, the contact angle of 20 mu L of water drops is 154.5 degrees, the rolling angle is 5.5 degrees, the contact angle of 20 mu L of soybean oil drops is 152 degrees, and the rolling angle is 9 degrees.
Claims (1)
1. A method for preparing a super-amphiphobic fabric using a translucent fluorosilane polymer emulsion, comprising the steps of:
(1) Preparation of semitransparent fluorosilane polymer emulsion: taking water as a solvent, acid as a catalyst, and a cationic surfactant as a dispersing agent, performing hydrolytic condensation reaction on fluorosilane and a silane coupling agent for 1-24 hours at the temperature of 25-40 ℃, and performing ultrasonic treatment to obtain semitransparent fluorosilane polymerization emulsion; the acid is one of sulfuric acid, hydrochloric acid, acetic acid and oxalic acid, the mass fraction of the acid in the reaction system is 0.1-1%, the cationic surfactant is at least two of dodecyl trimethyl ammonium bromide, didodecyl dimethyl ammonium bromide, dicetyl dimethyl ammonium bromide, hexadecyl trimethyl ammonium bromide and octadecyl trimethyl ammonium chloride, and the mass fraction of the acid in the reaction system is 0.1-0.24%; the fluorosilane is one of perfluorodecyl trimethoxy silane, perfluorodecyl triethoxy silane and perfluoropolyether silane, and the mass fraction of the fluorosilane in the reaction system is 0.2-4%; the silane coupling agent is at least one of gamma-aminopropyl trimethoxy silane and gamma- (2, 3-epoxypropoxy) propyl trimethoxy silane, and the mass fraction of the silane coupling agent in a reaction system is 0.20% or 0.29%;
(2) Preparation of super-amphiphobic fabric: soaking the washed fabric in semitransparent fluorosilane polymer emulsion for 1-20 min, taking out, press-filtering to remove redundant liquid, and then curing at 140-190 ℃ for 2-10 min to obtain the super-amphiphobic fabric; the fabric comprises a polyester fabric, a nylon fabric, a cotton fabric, a cashmere fabric or a hemp fabric.
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| CN104003406A (en) * | 2014-05-30 | 2014-08-27 | 武汉理工大学 | Preparation method and applications of super-hydrophobic SiO2 aerogel powder |
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