CN114657789A - Organic silicon super-hydrophobic coating, super-hydrophobic coating based on organic silicon super-hydrophobic coating and application of organic silicon super-hydrophobic coating - Google Patents
Organic silicon super-hydrophobic coating, super-hydrophobic coating based on organic silicon super-hydrophobic coating and application of organic silicon super-hydrophobic coating Download PDFInfo
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Abstract
The invention belongs to the technical field of functional materials, and discloses an organic silicon super-hydrophobic coating, a super-hydrophobic coating based on the organic silicon super-hydrophobic coating and application of the organic silicon super-hydrophobic coating. The coating comprises the following raw materials in parts by mass: 2.0-5.0 parts of tetraethyl orthosilicate, 2.0-6.0 parts of hydroxyl-terminated sealing agent, 0.05-0.5 part of silicon dioxide particles and a proper amount of catalyst. The tetraethyl orthosilicate, the hydroxyl-terminated sealing agent and the hydroxyl on the surface of the silicon dioxide in the coating are subjected to hydrolysis condensation reaction, and a nano composite rough structure with low surface energy and a rigid structure is constructed on the surface of the substrate in situ, so that the surface tension of the interface of the substrate is effectively reduced, the roughness of the interface is increased, the obtained coating has excellent light transmittance, wear resistance and corrosion resistance, a lasting super-hydrophobic effect can be realized, the water contact angle can reach 164 degrees, the good super-hydrophobic performance can be still maintained after 100 times of washing, and the hydrophobicity and the durability of the substrate are greatly improved.
Description
Technical Field
The invention belongs to the technical field of functional materials, and particularly relates to an organic silicon super-hydrophobic coating, a super-hydrophobic coating based on the organic silicon super-hydrophobic coating and application of the organic silicon super-hydrophobic coating.
Background
The super-hydrophobic surface refers to a surface with a contact angle with water of more than 150 degrees and a rolling angle of less than 10 degrees. The super-hydrophobic surface has special surface wettability, so that the super-hydrophobic surface can be widely applied to various fields of electronic information, biomedicine, aerospace, new materials and the like, has wide prospects, and is still limited in industrial production and practical life application. One of the main reasons is that the durability of the coating is generally poor, and the micro-nano structure of the super-hydrophobic surface is easily abraded and damaged in use; secondly, the preparation process is complex, the preparation period is long, and many methods adopt a complex process when constructing a surface microstructure, so that the time and the labor are consumed, and the cost investment is increased; thirdly, organic fluorides such as perfluorosilane are mostly adopted during low surface energy treatment, the used solvent is often a toxic and harmful organic reagent, the application range of the finished product is greatly limited due to the problems of safety, environmental protection and the like, and the waste liquid treatment wastes time and energy and is expensive, so that the large-scale industrial production is not suitable.
The organic silicon has low surface energy and high thermal stability, is used for fire prevention and heat insulation of polymers as a flame retardant, is widely used for preparing super-hydrophobic coating, is more environment-friendly and more economical than fluorine-containing materials, and is popular with the public. Therefore, it is very important to develop a simple, convenient, safe and environment-friendly method for preparing the super-hydrophobic coating with excellent performance.
Disclosure of Invention
In order to overcome the defects and shortcomings of poor durability and unsafe and environment-friendly preparation method of the super-hydrophobic coating in the prior art, the invention aims to provide the organic silicon super-hydrophobic coating.
The invention also aims to provide a super-hydrophobic coating based on the organic silicon super-hydrophobic coating.
The invention also aims to provide a preparation method of the super-hydrophobic coating.
The invention further aims to provide application of the organic silicon super-hydrophobic coating. When the organic silicon super-hydrophobic coating is applied to surface hydrophobic modification, particularly fabric surface modification, the obtained super-hydrophobic coating has good hydrophobic property and is durable.
The purpose of the invention is realized by the following scheme:
an organic silicon super-hydrophobic coating comprises the following raw materials in parts by weight: 2.0-5.0 parts of tetraethyl orthosilicate, 2.0-6.0 parts of hydroxyl-terminated sealing agent, 0.05-0.5 part of silicon dioxide particles and a proper amount of catalyst.
The hydroxyl-terminated blocking agent comprises at least one of hydroxyl-terminated polydimethylsiloxane, hydroxyl-terminated polybutadiene polyurethane, hydroxyl-terminated polyether and the like.
The silica particles include but are not limited to SiO2Nanoparticle and mesoporous SiO2Nanoparticles and hydrophobically modified SiO2At least one of the nanoparticles.
Further, the silica particles preferably have a particle diameter of 50 to 100nm and good dispersibility.
The catalyst is a common catalyst for dehydration condensation reaction, such as alkali, including but not limited to at least one of ammonia water, sodium hydroxide, sodium bicarbonate, sodium carbonate and the like.
The organic silicon super-hydrophobic coating component also contains a solvent; the solvent includes at least one of organic solvents such as methanol, ethanol, acetone, etc. The dosage of the solvent is adjusted according to actual use.
The organic silicon super-hydrophobic coating can be applied to surface hydrophobic modification, particularly to fabric surface modification; through coating modes such as soaking or spraying, the organic silicon super-hydrophobic coating can form a super-hydrophobic coating on the surface of a base material, and has excellent corrosion resistance, durability and super-hydrophobicity.
The invention also provides a super-hydrophobic coating based on the organic silicon super-hydrophobic coating.
The invention also provides a preparation method of the super-hydrophobic coating, which comprises the following steps:
(1) dispersing silica particles in a solvent to obtain a silica dispersion liquid A; adding tetraethyl orthosilicate, a hydroxyl-terminated sealing agent and a catalyst into a solvent, and uniformly stirring to obtain a solution B;
(2) soaking a base material in the silicon dioxide dispersion liquid A in the step (1) and taking out; and coating the solution B on the surface of a base material for reaction to obtain the super-hydrophobic coating after the reaction is finished.
In the step (1), the concentration of silica particles in the silica dispersion A is preferably 0.05 to 0.5% (m/V), Kg/L.
The substrate can be glass material, metal material, ceramic material, wood, high polymer material, artificial high polymer fabric, natural high polymer fabric and the like.
The concentration of tetraethyl orthosilicate in the solution B is preferably 2.0-5.0% (m/V), Kg/L.
The dosage of the catalyst is based on the adjustment of the pH value of the solution B to 8.5-9.5.
In the step (2), the soaking time in the silicon dioxide dispersion liquid A can be 30min-4 h.
After being taken out, the base material can be washed by a solvent, and then used for subsequent reaction after being dried. The drying treatment can be carried out at 60-80 deg.C; the drying time can be 3-5 h.
The reaction time can be 30min-4 h.
The reaction can be carried out at room temperature, preferably at 20 to 30 ℃.
After the reaction is finished, the reaction product can be washed by a solvent and dried. Preferably drying in an oven at 60-80 deg.C for 3-5 h.
The coating method can comprise various liquid coating processing modes such as dipping, spraying, curtain coating, wiping and the like.
In the above preparation method, the solvents may be the same or different and may be at least one of organic solvents such as methanol, ethanol, acetone, etc. Such as absolute ethanol.
Component of the coating of the invention, SiO2The particles are firstly deposited on the surface of the fabric through hydrogen bonds and electrostatic interaction to increase the surface roughness of the fabric, then tetraethyl orthosilicate, a hydroxyl-terminated sealing agent and hydroxyl on the surface of silicon dioxide are added to perform hydrolytic condensation reaction, and a nano composite rough structure with low surface energy and a rigid structure is constructed on the surface of the substrate in situ, so that the surface tension of the interface of the substrate is effectively reduced, the interface roughness is increased, the obtained coating has excellent light transmittance, wear resistance and corrosion resistance, a durable super-hydrophobic effect can be realized, the water contact angle can reach 164 degrees, the good super-hydrophobic property can be still maintained after 100 times of washing, and the hydrophobicity and the durability of the substrate are greatly improved.
Compared with the prior art, the invention has the following advantages and beneficial effects:
(1) according to the invention, through condensation reaction of hydroxyl, nano particles with different sizes are effectively attached to the base material, and a nano composite structure with certain structural rigidity is constructed, so that the surface energy is reduced, the roughness is improved, and the durable super-hydrophobic function is realized.
(2) The solvent and the reagent in the paint are both environment-friendly, the waste liquid treatment in the using process is simple and low in consumption, the defects that a large amount of organic toxic reagents are used in the traditional hydrophobic coating preparation process, the manufacturing process is complex, the cost is high, the hydrophobic performance is poor and the like are overcome, and compared with the existing preparation methods of most hydrophobic coatings, the paint has obvious advantages and good industrialization prospects.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained according to the drawings without inventive efforts.
FIG. 1 is SiO prepared in example 12TEM images of the nanoparticles.
FIG. 2 is SiO prepared in example 12SEM images of nanoparticles.
Fig. 3 is a test chart of static water contact angle of the superhydrophobic polyester fabric prepared in example 1.
FIG. 4 shows mesoporous SiO prepared in example 22TEM images of the nanoparticles.
FIG. 5 shows mesoporous SiO prepared in example 22SEM images of nanoparticles.
Fig. 6 is a test chart of static water contact angle of the superhydrophobic nylon fabric prepared in example 2.
Fig. 7 is a static water contact angle test chart of the superhydrophobic cotton fabric prepared in example 3.
Detailed Description
The present invention will be described in further detail with reference to examples, but the embodiments of the present invention are not limited thereto. The materials referred to in the following examples are commercially available without specific reference. The method is a conventional method unless otherwise specified. The dosage of each component is g and mL in parts by mass and parts by volume.
Example 1
An organic silicon super-hydrophobic coating comprises the following raw materials in parts by mass: 2 parts of tetraethyl orthosilicate, 6 parts of a hydroxyl-terminated sealing agent, 0.05 part of silicon dioxide particles, a proper amount of ammonia water and a proper amount of absolute ethyl alcohol.
A super-hydrophobic coating based on the organic silicon super-hydrophobic coating is prepared by the following steps:
(1) the silicon dioxide particles are prepared by a Stober method according to a conventional method, ammonia water is used as a catalyst, tetraethoxysilane is used as a raw material, and SiO is prepared2Nanoparticles. From TEM (FIG. 1) and SEM (FIG. 2), SiO can be derived2The average size of the nanoparticles was 80 nm.
(2) SiO prepared in the step (1)2Adding 0.05 part by mass of particles into 100 parts by volume of absolute ethyl alcohol, uniformly dispersing, putting the polyester fabric into the absolute ethyl alcohol, soaking for 2 hours, taking out, cleaning the fabric for 3 times by using the absolute ethyl alcohol, and placing the fabric in a baking ovenDrying at 60 deg.C for 3 h;
(3) mixing 2 parts by mass of ethyl orthosilicate, 6 parts by mass of hydroxyl-terminated polydimethylsiloxane and 100 parts by volume of absolute ethyl alcohol, adding ammonia water to adjust the pH value to 9, uniformly stirring, soaking the dried fabric in the step (2), taking out the fabric after reaction for 2 hours, washing the fabric for 3 times by using the absolute ethyl alcohol, and drying the fabric in an oven at 60 ℃ for 3 hours to obtain the fabric with the surface being provided with the super-hydrophobic coating.
(4) The contact angle test result for the obtained polyester fabric was 162 ° as shown in fig. 3. The prepared super-hydrophobic fabric is soaked in an ammonia water solution with the pH value of 9 for 12 hours, the fabric is washed by absolute ethyl alcohol for 3 times, the contact angle test result after drying is 161 degrees, and the hydrophobic performance of the fabric before and after alkaline corrosion does not change obviously. The prepared super-hydrophobic fabric is placed in a pulsator washing machine for standard washing (15min is one cycle), and after 100 times of washing, the contact angle test result is 143 degrees. It is demonstrated that the superhydrophobic fabric prepared in this example has excellent alkali corrosion resistance and durability.
Example 2
An organic silicon super-hydrophobic coating comprises the following raw materials in parts by weight: 3 parts of tetraethyl orthosilicate, 3 parts of a hydroxyl-terminated sealing agent, 0.1 part of silicon dioxide particles, a proper amount of sodium hydroxide solution and a proper amount of anhydrous methanol.
A super-hydrophobic coating based on the organic silicon super-hydrophobic coating is prepared by the following steps:
(1) the used silicon dioxide particles are prepared by a template method according to a conventional method, hexadecyl trimethyl p-methyl benzene sulfonic acid ammonium salt serving as a template agent and triethanolamine are dissolved in deionized water, the mixture is stirred for 1 hour at the temperature of 80 ℃, tetraethyl orthosilicate is added after the mixture is fully dissolved, the reaction is continued for 2 hours, the obtained nano particles are centrifuged, washed, freeze-dried, calcined and ground for later use, and the prepared mesoporous SiO is known from TEM (figure 4) and SEM (figure 5)2The average size of the nanoparticles was 80 nm.
(2) Preparing the mesoporous SiO prepared in the step (1)2Adding 0.1 part by mass of particles into 100 parts by volume of absolute methanol, uniformly dispersing, putting the nylon fabric into the absolute methanol, soaking for 2 hours, taking out, and cleaning the fabric for 3 times by using the absolute ethanolDrying in an oven at 60 deg.C for 3 hr;
(3) mixing 3 parts by mass of ethyl orthosilicate, 3 parts by mass of hydroxyl-terminated polybutadiene polyurethane and 100 parts by volume of anhydrous methanol, adding a sodium hydroxide solution to adjust the pH value to 9, uniformly stirring, soaking the dried fabric in the step (2), taking out the fabric after reaction for 2 hours, washing the fabric for 3 times by using the anhydrous ethanol, and drying the fabric in an oven at 60 ℃ for 3 hours to obtain the fabric with the surface being the super-hydrophobic coating.
(4) The contact angle test result for the obtained nylon fabric was 164 ° as shown in fig. 6. The prepared super-hydrophobic fabric is soaked in a hydrochloric acid solution with the pH value of 5 for 12 hours, is washed by absolute ethyl alcohol for 3 times, and has a contact angle test result of 162 degrees after being dried, and the hydrophobic performance of the fabric is not obviously changed before and after acidic corrosion. The prepared super-hydrophobic fabric is placed in a pulsator washing machine for standard washing (15min is one cycle), and after 100 times of washing, the contact angle test result is 146 degrees. It is demonstrated that the superhydrophobic fabrics prepared in this example have excellent acid corrosion resistance and durability.
Example 3
An organic silicon super-hydrophobic coating comprises the following raw materials in parts by weight: 5 parts of tetraethyl orthosilicate, 2 parts of a hydroxyl-terminated sealing agent, 0.5 part of silicon dioxide particles, a proper amount of sodium carbonate solution and a proper amount of absolute ethyl alcohol.
A super-hydrophobic coating based on the organic silicon super-hydrophobic coating is prepared by the following steps:
(1)SiO2the particles were prepared as in example 1.
(2) SiO prepared in the step (1)2Adding 0.5 part by mass of particles into 100 parts by volume of absolute ethyl alcohol, uniformly dispersing, putting the cotton fabric into the particles, soaking for 2 hours, taking out, cleaning the fabric for 3 times by using the absolute ethyl alcohol, and drying for 3 hours at the temperature of 60 ℃ in an oven;
(3) mixing 5 parts by mass of ethyl orthosilicate, 2 parts by mass of double-end hydroxyl polyether and 100 parts by volume of absolute ethyl alcohol, adding a sodium carbonate solution to adjust the pH value to 9, uniformly stirring, soaking the dried fabric in the step (2), taking out the fabric after reaction for 2 hours, washing the fabric for 3 times by using the absolute ethyl alcohol, and drying the fabric in an oven at 60 ℃ for 3 hours to obtain the fabric with the surface provided with the super-hydrophobic coating, wherein the contact angle test result is 160 degrees, as shown in fig. 7; the corrosion resistance and durability are similar to those of the above embodiments, and detailed description thereof is omitted.
Comparative example 1
(1)SiO2The particles were prepared as in example 1.
(2) SiO prepared in the step (1)2Adding 0.05 part by mass of particles into 100 parts by volume of absolute ethyl alcohol, uniformly dispersing, putting the polyester fabric into the absolute ethyl alcohol, soaking for 2 hours, taking out, cleaning the fabric for 3 times by using the absolute ethyl alcohol, and drying for 3 hours at the temperature of 60 ℃ in an oven; the contact angle test result of the obtained polyester fabric was 134 °. The prepared hydrophobic polyester fabric is placed in a pulsator washing machine for washing for 20 times, and the contact angle test result is 105 degrees.
It can be seen that SiO is used2The nano particles can obtain the effect of hydrophobic modification, but cannot achieve the effect of super-hydrophobicity, and the obtained coating has an unstable structure and is easy to damage, the hydrophobic property is obviously reduced, and the service life of the product is greatly shortened.
Comparative example 2
Mixing 2 parts by mass of tetraethoxysilane, 6 parts by mass of a terminal hydroxyl blocking agent and 100 parts by volume of absolute ethyl alcohol, adding ammonia water to adjust the pH to 9, uniformly stirring, soaking the polyester fabric in the mixture, taking out the polyester fabric after reacting for 2 hours, washing the polyester fabric for 3 times by using the absolute ethyl alcohol, and drying the polyester fabric in an oven at 60 ℃ for 3 hours to obtain a contact angle test result of the polyester fabric of 141 degrees. The prepared hydrophobic polyester fabric is placed in a pulsator washing machine to be washed for 20 times, and the contact angle test result is 120 degrees.
Therefore, the fabric surface is modified by utilizing tetraethyl orthosilicate and a hydroxyl-terminated sealing agent to obtain a hydrophobic modification effect, but the super-hydrophobic effect cannot be achieved, the obtained coating is unstable in structure and easy to damage, the hydrophobic property is obviously reduced, and the service life of the product is greatly shortened.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (10)
1. The organic silicon super-hydrophobic coating is characterized by comprising the following raw materials in parts by mass: 2.0-5.0 parts of tetraethyl orthosilicate, 2.0-6.0 parts of hydroxyl-terminated sealing agent, 0.05-0.5 part of silicon dioxide particles and a proper amount of catalyst.
2. The silicone superhydrophobic coating of claim 1, wherein: the hydroxyl-terminated blocking agent comprises at least one of hydroxyl-terminated polydimethylsiloxane, hydroxyl-terminated polybutadiene polyurethane and hydroxyl-terminated polyether end-group blocking agent.
3. The silicone superhydrophobic coating of claim 1, wherein: the silica particles comprise SiO2Nanoparticle and mesoporous SiO2Nanoparticles and hydrophobically modified SiO2At least one of the nanoparticles.
4. Use of the silicone superhydrophobic coating of any of claims 1-3 in surface modification.
5. A superhydrophobic coating based on the silicone superhydrophobic coating of claim 1.
6. A method for preparing the superhydrophobic coating of claim 5, comprising the steps of:
(1) dispersing silica particles in a solvent to obtain a silica dispersion liquid A; adding tetraethyl orthosilicate, a hydroxyl-terminated sealing agent and a catalyst into a solvent, and uniformly stirring to obtain a solution B;
(2) soaking a base material in the silicon dioxide dispersion liquid A in the step (1) and taking out; and then soaking the substrate in the solution B, or spraying the solution B on the surface of the substrate to react, and obtaining the super-hydrophobic coating after the reaction is finished.
7. The method of claim 6, wherein: in the step (1), the concentration of the silica particles in the silica dispersion liquid A is 0.05-0.5% m/V; in the solution B, the concentration of tetraethyl orthosilicate is 2.0-5.0% m/V.
8. The method of manufacturing according to claim 6, characterized in that: the dosage of the catalyst is based on the adjustment of the pH value of the solution B to 8.5-9.5.
9. The method of claim 6, wherein: in the step (2), the soaking time in the silicon dioxide dispersion liquid A is 30min-4 h; the reaction time is 30min-4 h.
10. The method of claim 6, wherein: the solvents are the same or different and are at least one of methanol, ethanol and acetone respectively.
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| CN115637104A (en) * | 2022-11-04 | 2023-01-24 | 山东大学 | Preparation method and application of tetraethoxysilane-siloxane-surfactant hybrid material |
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|---|---|---|---|---|
| CN103276590A (en) * | 2013-06-04 | 2013-09-04 | 东北林业大学 | Method for preparing super-hydrophobic super-oleophylic cotton |
| EP2990527A1 (en) * | 2014-08-18 | 2016-03-02 | Kemijski Institut | A process for preparing of cotton textiles having self-cleaning and washing resistant properties |
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| CN103276590A (en) * | 2013-06-04 | 2013-09-04 | 东北林业大学 | Method for preparing super-hydrophobic super-oleophylic cotton |
| EP2990527A1 (en) * | 2014-08-18 | 2016-03-02 | Kemijski Institut | A process for preparing of cotton textiles having self-cleaning and washing resistant properties |
| WO2018133469A1 (en) * | 2017-01-18 | 2018-07-26 | 华南理工大学 | Durable hydrophilic-super-hydrophobic bipolar self-cleaning composite film, and preparation method therefor |
| CN107164947A (en) * | 2017-05-27 | 2017-09-15 | 华南理工大学 | A kind of durable superhydrophobic fabric and preparation method thereof |
| CN108951165A (en) * | 2018-07-20 | 2018-12-07 | 华南理工大学 | A kind of preparation method of super-hydrophobic/anti-ultraviolet functional fabric |
| CN113047050A (en) * | 2021-03-19 | 2021-06-29 | 安徽工业大学 | TiO 22-SiO2Preparation method of @ PDMS composite super-hydrophobic filter material |
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| CN115637104A (en) * | 2022-11-04 | 2023-01-24 | 山东大学 | Preparation method and application of tetraethoxysilane-siloxane-surfactant hybrid material |
| CN115637104B (en) * | 2022-11-04 | 2023-12-22 | 山东大学 | Preparation method and application of ethyl orthosilicate-siloxane-surfactant hybrid material |
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