CN110615619A - Preparation method and performance test method of silicon dioxide super-hydrophobic coating - Google Patents
Preparation method and performance test method of silicon dioxide super-hydrophobic coating Download PDFInfo
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- CN110615619A CN110615619A CN201810637233.0A CN201810637233A CN110615619A CN 110615619 A CN110615619 A CN 110615619A CN 201810637233 A CN201810637233 A CN 201810637233A CN 110615619 A CN110615619 A CN 110615619A
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- silicon dioxide
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/006—Surface treatment of glass, not in the form of fibres or filaments, by coating with materials of composite character
- C03C17/008—Surface treatment of glass, not in the form of fibres or filaments, by coating with materials of composite character comprising a mixture of materials covered by two or more of the groups C03C17/02, C03C17/06, C03C17/22 and C03C17/28
- C03C17/009—Mixtures of organic and inorganic materials, e.g. ormosils and ormocers
-
- 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
- C09D1/00—Coating compositions, e.g. paints, varnishes or lacquers, based on inorganic substances
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N13/00—Investigating surface or boundary effects, e.g. wetting power; Investigating diffusion effects; Analysing materials by determining surface, boundary, or diffusion effects
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2217/00—Coatings on glass
- C03C2217/70—Properties of coatings
Abstract
The invention provides a method for preparing a silicon dioxide super-hydrophobic coating and testing the performance of the silicon dioxide super-hydrophobic coating in the chemical field, which comprises the following steps of (1) preparing nano silicon dioxide particles; (2) obtaining low surface energy nano silicon dioxide particles; (3) carrying out surface modification on the low-surface-energy nano silicon dioxide by using APTES; (4) carrying out surface modification on the base material; (5) forming a modified nano-silica super-hydrophobic coating on a substrate; (6) testing the hydrophobic property of the modified nano-silica super-hydrophobic coating; (7) testing the stability of the modified nano silicon dioxide super-hydrophobic coating; the invention is simple and has high efficiency.
Description
Technical Field
The invention belongs to the field of chemistry, and particularly relates to a preparation method and a performance test method of a silicon dioxide super-hydrophobic coating.
Background
At present, the method for preparing superhydrophobic coatings is mainly based on two schemes: firstly, constructing a binary micro-nano composite rough structured surface on a hydrophobic material substrate; and secondly, modifying or depositing hydrophobic substances on the binary micro-nano composite rough structured surface by a chemical or physical method. The two schemes are complex in implementation process, inconvenient to operate and low in efficiency.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to overcome the defects in the prior art and provides a method for preparing a silicon dioxide super-hydrophobic coating and testing the performance of the silicon dioxide super-hydrophobic coating.
The purpose of the invention is realized as follows: a method for preparing a silicon dioxide super-hydrophobic coating and testing the performance of the silicon dioxide super-hydrophobic coating comprises the following steps:
(1) preparing nano silicon dioxide particles;
(2) obtaining low surface energy nano silicon dioxide particles;
(3) carrying out surface modification on the low-surface-energy nano silicon dioxide by using APTES;
(4) carrying out surface modification on the base material;
(5) forming a modified nano-silica super-hydrophobic coating on a substrate;
(6) testing the hydrophobic performance of the modified nano-silica super-hydrophobic coating: measuring by using a Drop Meter A-20 contact angle measuring system, wherein the measuring system is used for measuring the contact angle of the surface of an object based on an interface shape analysis method, calculating the contact angle according to the shape of liquid drops, respectively measuring 5 different points on each measured coating when measuring the static contact angle of the coating, and averaging the measured values of the static contact angles of the five points;
(7) testing the stability of the modified nano-silica superhydrophobic coating: and (3) storing the modified nano silicon dioxide super-hydrophobic coating for different time, and measuring the static contact angle and the rolling angle of the water drop on the surface of the coating.
As a further improvement of the present invention, step (1) specifically comprises the following steps:
dissolving 30 mL of TEOS in ethanol to obtain 350 mL of mixed solution of anhydrous ethanol and TEOS, pouring the mixed solution of TEOS and sewage ethanol into a three-neck flask with the capacity of 500mL, which is provided with an electric stirrer, a dropping funnel and a condenser, wherein the dropping funnel contains 2% of distilled water and ammonia water according to the volume ratio of the distilled water to the ammonia water: 7, and preparing a distilled aqueous solution of ammonia water. And starting an electric stirrer on the three-neck flask, simultaneously opening and adjusting a switch of the dropping funnel, uniformly dropping 18 mL of the distilled aqueous solution of the ammonia water into the three-neck flask at the speed of 15 mL/min, and continuously stirring for 1h after the dropping of the distilled aqueous solution of the ammonia water is finished to obtain the nano-silica sol. And (3) drying the nano-silica sol in a drying oven at 120 ℃ for 24h, removing the solvent and byproducts to obtain dried nano-silica gel, grinding the gel, and filtering by using a 300-mesh sample separation sieve to obtain nano-silica particles.
As a further improvement of the present invention, the step (2) specifically comprises the following steps:
(201) 0.5g of PDMS and 0.05g of DBTD were added to a three-necked flask equipped with an electric stirrer, and 50ml of n-heptane was added and mechanically stirred for 10 minutes. Adding 5g of nano silicon dioxide into the mixed solution, mechanically stirring for 15 minutes and ultrasonically shaking for 1min to uniformly disperse nano silicon dioxide particles in the mixed solution;
(202) and standing the system at room temperature for 36h to graft PDMS molecules onto the surface of the nano-silica through a condensation reaction between-OH groups, and volatilizing n-heptane to obtain the low-surface-energy nano-silica particles.
As a further improvement of the present invention, the step (3) specifically comprises the following steps:
(301) 5.5g of low surface energy nano silica particles were dispersed in 150ml of absolute ethanol at room temperature and ultrasonically dispersed for 3 minutes. The absolute ethyl alcohol dispersion liquid of the low surface energy nano silicon dioxide particles is injected into a 500ml three-neck flask, and the system is placed in a water area with the temperature of 60 ℃ for mechanical stirring;
(302) in the mechanical stirring process, 0.5g of APTES and 5ml of acidic ultrapure water are added into the system, wherein the acidic ultrapure water is obtained by adding acetic acid into ultrapure water to adjust the pH value to 5;
(303) and (3) keeping the reaction system at 60 ℃ for 2h, and mechanically stirring to graft APTES molecules to the surface of the low-surface-energy nano-silica particle through a condensation reaction between-OH groups, so as to obtain the low-surface-energy nano-silica particle dispersion liquid of the surface-modified APTES.
As a further improvement of the present invention, the step (4) specifically comprises the following steps:
(401) placing the glass sheet in absolute ethyl alcohol at room temperature, and cleaning the glass sheet for 10 minutes by adopting ultrasonic waves;
(402) placing the glass sheet in deionized water and cleaning the glass sheet for 20 minutes by ultrasonic waves;
(403) placing the cleaned glass sheet in an oven to be dried to obtain a glass sheet with a clean surface;
(404) the clean glass sheet was placed in a mixed solution of 0.5g of EPTMS, 100ml of ethanol, and 5ml of ultrapure water having a pH =5, and the reaction temperature of the system was maintained at 60 ℃, and after 1 hour of reaction, the EPTMS surface-modified glass sheet was obtained.
As a further improvement of the present invention, the step (5) specifically comprises the following steps:
(501) soaking the EPTMS-modified glass sheet in the low surface energy nano silicon dioxide particle dispersion liquid of the surface modified APTES, taking out the glass sheet, placing the glass sheet in an oven at 120 ℃ for 20 minutes to enable the nano silicon dioxide particles to be self-assembled on the surface of the glass sheet, and grafting the nano self-assembly on the surface of the glass sheet through polymerization of epoxy groups on the EPTMS and amino groups on the APTES;
(502) and continuously drying the glass sheet to obtain the modified nano silicon dioxide super-hydrophobic coating.
Drawings
Fig. 1 is a contact angle hysteresis graph of a water drop on a modified nano-silica superhydrophobic coating.
FIG. 2 is a graph of the change of the static contact angle of the modified nano-silica superhydrophobic coating with storage time.
Detailed Description
The invention is further described below with reference to the accompanying drawings.
A method for preparing silicon dioxide super-hydrophobic coating and testing performance thereof comprises the following steps,
(1) preparing nano silicon dioxide particles, specifically: dissolving 30 mL of TEOS in ethanol to obtain 350 mL of mixed solution of anhydrous ethanol and TEOS, pouring the mixed solution of TEOS and sewage ethanol into a three-neck flask with the capacity of 500mL, which is provided with an electric stirrer, a dropping funnel and a condenser, wherein the dropping funnel contains 2% of distilled water and ammonia water according to the volume ratio of the distilled water to the ammonia water: 7, and preparing a distilled aqueous solution of ammonia water. And starting an electric stirrer on the three-neck flask, simultaneously opening and adjusting a switch of the dropping funnel, uniformly dropping 18 mL of the distilled aqueous solution of the ammonia water into the three-neck flask at the speed of 15 mL/min, and continuously stirring for 1h after the dropping of the distilled aqueous solution of the ammonia water is finished to obtain the nano-silica sol. Drying the nano-silica sol in a drying oven at 120 ℃ for 24h, removing the solvent and byproducts to obtain dried nano-silica gel, grinding the gel, and filtering by using a 300-mesh sample separation sieve to obtain nano-silica particles;
(2) the low surface energy nano silicon dioxide particles are obtained, and specifically comprise the following steps:
(201) 0.5g of PDMS and 0.05g of DBTD were added to a three-necked flask equipped with an electric stirrer, and 50ml of n-heptane was added and mechanically stirred for 10 minutes. Adding 5g of nano silicon dioxide into the mixed solution, mechanically stirring for 15 minutes and ultrasonically shaking for 1min to uniformly disperse nano silicon dioxide particles in the mixed solution;
(202) standing the system at room temperature for 36h to graft PDMS molecules onto the surface of the nano-silica through a condensation reaction between-OH groups, and volatilizing n-heptane to obtain low-surface-energy nano-silica particles;
(3) the method for carrying out surface modification on the low-surface-energy nano silicon dioxide by using the APTES specifically comprises the following steps: (301) 5.5g of low surface energy nano silica particles were dispersed in 150ml of absolute ethanol at room temperature and ultrasonically dispersed for 3 minutes. The absolute ethyl alcohol dispersion liquid of the low surface energy nano silicon dioxide particles is injected into a 500ml three-neck flask, and the system is placed in a water area with the temperature of 60 ℃ for mechanical stirring;
(302) in the mechanical stirring process, 0.5g of APTES and 5ml of acidic ultrapure water are added into the system, wherein the acidic ultrapure water is obtained by adding acetic acid into ultrapure water to adjust the pH value to 5;
(303) keeping the reaction system at 60 ℃ for 2h, and mechanically stirring to graft APTES molecules to the surface of the low-surface-energy nano-silica particles through a condensation reaction between-OH groups to obtain a low-surface-energy nano-silica particle dispersion liquid of surface-modified APTES;
(4) the surface modification is carried out on the base material, and specifically comprises the following steps: (401) placing the glass sheet in absolute ethyl alcohol at room temperature, and cleaning the glass sheet for 10 minutes by adopting ultrasonic waves;
(402) placing the glass sheet in deionized water and cleaning the glass sheet for 20 minutes by ultrasonic waves;
(403) placing the cleaned glass sheet in an oven to be dried to obtain a glass sheet with a clean surface;
(404) placing the clean glass sheet in a mixed solution of 0.5g of EPTMS, 100ml of ethanol and 5ml of ultrapure water with the pH =5, keeping the reaction temperature of the system at 60 ℃, and reacting for 1h to obtain the EPTMS surface modified glass sheet;
(5) forming a modified nano-silica super-hydrophobic coating on a substrate, which specifically comprises the following steps:
(501) soaking the EPTMS-modified glass sheet in the low surface energy nano silicon dioxide particle dispersion liquid of the surface modified APTES, taking out the glass sheet, placing the glass sheet in an oven at 120 ℃ for 20 minutes to enable the nano silicon dioxide particles to be self-assembled on the surface of the glass sheet, and grafting the nano self-assembly on the surface of the glass sheet through polymerization of epoxy groups on the EPTMS and amino groups on the APTES;
(502) continuously drying the glass sheet to obtain a modified nano silicon dioxide super-hydrophobic coating;
(6) testing the hydrophobic performance of the modified nano-silica super-hydrophobic coating: measuring by using a Drop Meter A-20 contact angle measuring system, wherein the measuring system is used for measuring the contact angle of the surface of an object based on an interface shape analysis method, calculating the contact angle according to the shape of liquid drops, respectively measuring 5 different points on each measured coating when measuring the static contact angle of the coating, and averaging the measured values of the static contact angles of the five points;
(7) testing the stability of the modified nano-silica superhydrophobic coating: and (3) storing the modified nano silicon dioxide super-hydrophobic coating for different time, and measuring the static contact angle and the rolling angle of the water drop on the surface of the coating.
As can be seen from FIG. 1, the contact angle variation amplitude of the water drop on the surface of the super-hydrophobic coating is very small; as the drop volume increases, the advancing contact angle increases slightly, with a value between 154 ° and 157 °, with an average value of 156.5 °; at the transition moment of the water drop volume from increasing to decreasing, a contact angle turning region occurs, and the contact angle is slightly decreased from 157 degrees to 153 degrees; the receding contact angle is unchanged along with the continuous reduction of the volume of the water drop until the water drop is about to separate from the surface of the coating, the receding contact angle is reduced from 153 degrees to 149 degrees, the average value of the receding contact angle is 152.4 degrees in the whole process of reducing the water drop, and the contact angle hysteresis value is the difference between the advancing contact angle and the receding contact angle, and the average value is 4.1 degrees; the above results show that the superhydrophobic coating prepared by using the steps (1) to (5) has a very small contact angle.
As can be seen from FIG. 2, the change of the static contact angle of the water drop on the super-hydrophobic coating is very small with the extension of the storage time, the static contact angle of the water drop of the super-hydrophobic coating is always kept above 150 degrees within 5 months of storage, and the test results show that the super-hydrophobic coatings prepared by the steps (1) - (5) have good stability.
The present invention is not limited to the above embodiments, and based on the technical solutions disclosed in the present invention, those skilled in the art can make some substitutions and modifications to some technical features without creative efforts based on the disclosed technical solutions, and these substitutions and modifications are all within the protection scope of the present invention.
Claims (10)
1. A method for preparing a silicon dioxide super-hydrophobic coating and testing the performance of the silicon dioxide super-hydrophobic coating is characterized by comprising the following steps:
(1) preparing nano silicon dioxide particles;
(2) obtaining low surface energy nano silicon dioxide particles;
(3) carrying out surface modification on the low-surface-energy nano silicon dioxide by using APTES;
(4) carrying out surface modification on the base material;
(5) forming a modified nano-silica super-hydrophobic coating on a substrate;
(6) testing the hydrophobic performance of the modified nano-silica super-hydrophobic coating: measuring by using a Drop Meter A-20 contact angle measuring system, wherein the measuring system is used for measuring the contact angle of the surface of an object based on an interface shape analysis method, calculating the contact angle according to the shape of liquid drops, respectively measuring 5 different points on each measured coating when measuring the static contact angle of the coating, and averaging the measured values of the static contact angles of the five points;
(7) testing the stability of the modified nano-silica superhydrophobic coating: and (3) storing the modified nano silicon dioxide super-hydrophobic coating for different time, and measuring the static contact angle and the rolling angle of the water drop on the surface of the coating.
2. The preparation method of the silica superhydrophobic coating and the performance test method thereof according to claim 1, wherein the step (1) comprises the following steps:
dissolving 30 mL of TEOS in ethanol to obtain 350 mL of mixed solution of anhydrous ethanol and TEOS, pouring the mixed solution of TEOS and sewage ethanol into a three-neck flask with the capacity of 500mL, which is provided with an electric stirrer, a dropping funnel and a condenser, wherein the dropping funnel contains 2% of distilled water and ammonia water according to the volume ratio of the distilled water to the ammonia water: 7, and preparing a distilled aqueous solution of ammonia water.
3. And starting an electric stirrer on the three-neck flask, simultaneously opening and adjusting a switch of the dropping funnel, uniformly dropping 18 mL of the distilled aqueous solution of the ammonia water into the three-neck flask at the speed of 15 mL/min, and continuously stirring for 1h after the dropping of the distilled aqueous solution of the ammonia water is finished to obtain the nano-silica sol.
4. And (3) drying the nano-silica sol in a drying oven at 120 ℃ for 24h, removing the solvent and byproducts to obtain dried nano-silica gel, grinding the gel, and filtering by using a 300-mesh sample separation sieve to obtain nano-silica particles.
5. The preparation method of the silica superhydrophobic coating and the performance test method thereof according to claim 1 or 2, wherein the step (2) specifically comprises the following steps:
(201) 0.5g of PDMS and 0.05g of DBTD were added to a three-necked flask equipped with an electric stirrer, and 50ml of n-heptane was added and mechanically stirred for 10 minutes.
6. Adding 5g of nano silicon dioxide into the mixed solution, mechanically stirring for 15 minutes and ultrasonically shaking for 1min to uniformly disperse nano silicon dioxide particles in the mixed solution;
(202) and standing the system at room temperature for 36h to graft PDMS molecules onto the surface of the nano-silica through a condensation reaction between-OH groups, and volatilizing n-heptane to obtain the low-surface-energy nano-silica particles.
7. The preparation method of the silica superhydrophobic coating and the performance test method thereof according to claim 2 or 3, wherein the step (3) comprises the following steps:
(301) 5.5g of low surface energy nano silica particles were dispersed in 150ml of absolute ethanol at room temperature and ultrasonically dispersed for 3 minutes.
8. The absolute ethyl alcohol dispersion liquid of the low surface energy nano silicon dioxide particles is injected into a 500ml three-neck flask, and the system is placed in a water area with the temperature of 60 ℃ for mechanical stirring;
(302) in the mechanical stirring process, 0.5g of APTES and 5ml of acidic ultrapure water are added into the system, wherein the acidic ultrapure water is obtained by adding acetic acid into ultrapure water to adjust the pH value to 5;
(303) and (3) keeping the reaction system at 60 ℃ for 2h, and mechanically stirring to graft APTES molecules to the surface of the low-surface-energy nano-silica particle through a condensation reaction between-OH groups, so as to obtain the low-surface-energy nano-silica particle dispersion liquid of the surface-modified APTES.
9. The method for preparing the silica superhydrophobic coating and the performance test thereof according to claim 3 or 4, wherein the step (4) comprises the following steps:
(401) placing the glass sheet in absolute ethyl alcohol at room temperature, and cleaning the glass sheet for 10 minutes by adopting ultrasonic waves;
(402) placing the glass sheet in deionized water and cleaning the glass sheet for 20 minutes by ultrasonic waves;
(403) placing the cleaned glass sheet in an oven to be dried to obtain a glass sheet with a clean surface;
(404) the clean glass sheet was placed in a mixed solution of 0.5g of EPTMS, 100ml of ethanol, and 5ml of ultrapure water having a pH =5, and the reaction temperature of the system was maintained at 60 ℃, and after 1 hour of reaction, the EPTMS surface-modified glass sheet was obtained.
10. The preparation method of the silica superhydrophobic coating and the performance test method thereof according to any one of claims 1-5, wherein the step (5) specifically comprises the following steps:
(501) soaking the EPTMS-modified glass sheet in the low surface energy nano silicon dioxide particle dispersion liquid of the surface modified APTES, taking out the glass sheet, placing the glass sheet in an oven at 120 ℃ for 20 minutes to enable the nano silicon dioxide particles to be self-assembled on the surface of the glass sheet, and grafting the nano self-assembly on the surface of the glass sheet through polymerization of epoxy groups on the EPTMS and amino groups on the APTES;
(502) and continuously drying the glass sheet to obtain the modified nano silicon dioxide super-hydrophobic coating.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109575651A (en) * | 2018-11-20 | 2019-04-05 | 安徽伊法拉电气有限公司 | A kind of super self-cleaning anti-pollution flashover coating of super-hydrophobic and its preparation process |
| CN109593387A (en) * | 2018-11-20 | 2019-04-09 | 安徽伊法拉电气有限公司 | A kind of preparation process of the super self-cleaning anti-pollution flash insulator of super-hydrophobic applied to electric system |
| CN111532373A (en) * | 2020-05-08 | 2020-08-14 | 山东交通学院 | Preparation method of super-icephobic coating for ship deck deicing |
-
2018
- 2018-06-20 CN CN201810637233.0A patent/CN110615619A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109575651A (en) * | 2018-11-20 | 2019-04-05 | 安徽伊法拉电气有限公司 | A kind of super self-cleaning anti-pollution flashover coating of super-hydrophobic and its preparation process |
| CN109593387A (en) * | 2018-11-20 | 2019-04-09 | 安徽伊法拉电气有限公司 | A kind of preparation process of the super self-cleaning anti-pollution flash insulator of super-hydrophobic applied to electric system |
| CN111532373A (en) * | 2020-05-08 | 2020-08-14 | 山东交通学院 | Preparation method of super-icephobic coating for ship deck deicing |
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Application publication date: 20191227 |