CN115722433A - Controllable method for underwater super-oleophobic coating from super-hydrophilic to super-hydrophobic under oil - Google Patents
Controllable method for underwater super-oleophobic coating from super-hydrophilic to super-hydrophobic under oil Download PDFInfo
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Abstract
The invention relates to a controllable method for an underwater super-oleophobic coating from super-hydrophilic to super-hydrophobic under oil, which comprises the following steps: the method includes the steps that a stainless steel mesh substrate is subjected to ultrasonic cleaning through different types of solvents and dried to obtain a dry stainless steel mesh; respectively preparing spraying solutions A (n = 0), B (n = 2), C (n = 4), D (n = 6) and E (n = 4) with different alkyl acid carbon chain lengths8) F (n = 10), G (n = 12), H (n = 14), I (n = 16); thirdly, respectively spraying different spraying solutions on the surface of the dry stainless steel mesh at room temperature; fourthly, respectively heating and curing different coatings obtained by spraying to respectively form 0Aa-AP-TiO 2 Surface, 2Aa-AP-TiO 2 Surface, 4Aa-AP-TiO 2 Surface, 6Aa-AP-TiO 2 Surface, 8Aa-AP-TiO 2 Surface, 10Aa-AP-TiO 2 Surface, 12Aa-AP-TiO 2 Surface, 14Aa-AP-TiO 2 Surface, 16Aa-AP-TiO 2 A surface. The preparation method is simple, mild in condition and environment-friendly and causes little pollution when in use.
Description
Technical Field
The invention relates to the technical field of material surface modification controllable preparation, in particular to a controllable method for an underwater super-oleophobic coating from super-hydrophilic to super-hydrophobic under oil.
Background
The controlled liquid repellency or adsorptivity of a super-wetting surface has attracted a great deal of attention, and the improvement of other interface properties of super-wetting materials also typically relies on specific wettabilities, such as catalysis, friction, bioengineering, oil-water separation, and the like. Inspired by fish scales, people developed various underwater surfaces with super oleophobic properties. In recent years, there have been many studies focusing on the investigation of the submerged limiting wettability. In water-solid-oil systems, oil is either replaced by water or vice versa, depending on the competing affinity interaction between oil/water and the surface. According to thermodynamic theory, it is unlikely that both underwater superhydrophobicity and oil superhydrophobicity will occur on the same surface at the same time, and only one super-wettability may be thermodynamically stable. And the surface of the material with reasonable surface chemistry and roughness can simultaneously obtain underwater super-hydrophobicity and oily super-hydrophobicity submerged double super-lyophobic. Furthermore, because the surface tension of oil is lower than that of water, it is difficult to achieve the oil-below superhydrophilicity of underwater superoleophobic surfaces.
Because the oily super-hydrophilicity and the oily super-hydrophobicity of the underwater super-hydrophobic surface have respective advantages: the oily super-hydrophobic coating can meet the corrosion resistance requirement of the water on the oil lubrication surface; the sub-oil superhydrophilic surface also plays an important role in the purification of oily water. Therefore, the research on the change rule of the subsurface wettability of the surface is of great significance for understanding the essential mechanism of the subsurface super-wettability of the surface. However, no report is available on the controllable preparation technology of the underwater super-hydrophobic surface from super-hydrophobic to super-hydrophilic in oil at present.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a controllable method for preparing an underwater super-oleophobic coating from super-hydrophilic to super-hydrophobic under oil, which has the advantages of simple method, high operability and mild conditions.
In order to solve the problems, the invention discloses a controllable method for an underwater super-oleophobic coating from super-hydrophilic to super-hydrophobic under oil, which comprises the following steps:
the method comprises the steps of ultrasonically cleaning a stainless steel mesh substrate by using acetone, ethanol and deionized water in sequence, cleaning for half an hour each time, and drying to obtain a dry stainless steel mesh;
preparing a spraying solution a of a surface with an alkyl acid carbon chain length n =0 (n = 0), a spraying solution B of a surface with an alkyl acid carbon chain length n =2 (n = 2), a spraying solution C of a surface with an alkyl acid carbon chain length n =4 (n = 4), a spraying solution D of a surface with an alkyl acid carbon chain length n =6 (n = 6), a spraying solution E of a surface with an alkyl acid carbon chain length n =8 (n = 8), a spraying solution F of a surface with an alkyl acid carbon chain length n =10 (n = 10), a spraying solution G of a surface with an alkyl acid carbon chain length n =12 (n = 12), a spraying solution H of a surface with an alkyl acid carbon chain length n =14 (n = 14), and a spraying solution I of a surface with an alkyl acid carbon chain length n =16 (n = 16), respectively;
thirdly, uniformly spraying nine spraying solutions a (n = 0), B (n = 2), C (n = 4), D (n = 6), E (n = 8), F (n = 10), G (n = 12), H (n = 14), I (n = 16) on the surface of the dry stainless steel mesh under the nitrogen gas pressure of 0.2 MPa at room temperature by using a gas compression spray gun;
fourthly, the different coatings obtained through spraying are respectively placed under the condition of 120 ℃ to be heated for 2 hours, then 200 ℃ is continuously cured for 1 hour, and a surface with the chain length of the alkyl acid carbon n =0, a surface with the chain length of the alkyl acid carbon n =2, a surface with the chain length of the alkyl acid carbon n =4, a surface with the chain length of the alkyl acid carbon n =6, a surface with the chain length of the alkyl acid carbon n =8, a surface with the chain length of the alkyl acid carbon n =10, a surface with the chain length of the alkyl acid carbon n =12, a surface with the chain length of the alkyl acid carbon n =14 and a surface with the chain length of the alkyl acid carbon n =16 are respectively formed, and are respectively abbreviated as 0Aa-AP-TiO 2 Surface, 2Aa-AP-TiO 2 Surface, 4Aa-AP-TiO 2 Surface, 6Aa-AP-TiO 2 Surface, 8Aa-AP-TiO 2 Surface, 10Aa-AP-TiO 2 Surface, 12Aa-AP-TiO 2 Surface, 14Aa-AP-TiO 2 Surface, 16Aa-AP-TiO 2 A surface.
The mesh number of the stainless steel mesh substrate in the step is 2300 meshes.
The steps of spraying the solution A (n = 0), B (n = 2), C (n = 4), D (n = 6), E (n = 8), F (n = 10), G (n = 12), H (n = 14) and I (n = 16) in the second phase are prepared according to the following methods:
(1) preparing an inorganic aluminum phosphate binder: diluting phosphoric acid to 60% by using deionized water, adding aluminum hydroxide to ensure that the molar ratio of the phosphoric acid to the aluminum hydroxide is 3, and stirring for 3 hours at 100 ℃ to obtain the compound;
(2) preparing an aluminum phosphate solution: dissolving 1g of inorganic aluminum phosphate binder in 4 mL of deionized water, and uniformly stirring to obtain the aluminum phosphate adhesive;
(3) preparing a titanium dioxide dispersion liquid: dispersing 0.5 g of titanium dioxide nanoparticles in 5 mL of absolute ethanol, and performing ultrasonic treatment for 10 minutes to uniformly disperse the titanium dioxide nanoparticles to obtain the titanium dioxide nanoparticles;
(4) 9 parts of the titanium dioxide dispersion were added with 0.02 mmol of an alkyl acid (CH) having a carbon chain length of n =0, 2, 4, 6, 8, 10, 12, 14, 16, respectively 3 (CH 2 ) n COOH), the same volume of aluminum phosphate solution was dropped into the solution after stirring uniformly, and the solution was stirred for half an hour to uniformly mix the solution, thereby obtaining nine kinds of spray solutions a (n = 0), B (n = 2), C (n = 4), D (n = 6), E (n = 8), F (n = 10), G (n = 12), H (n = 14), and I (n = 16).
The average particle diameter of the titanium dioxide particles in the step (3) is 25 nm.
Compared with the prior art, the invention has the following advantages:
1. the invention adopts the strategy of 'inorganic adhesive + functional coating', and the fine regulation and control of the surface chemistry of the alkyl acid can be realized by finely regulating and controlling the carbon chain length of the alkyl acid; meanwhile, the controllable preparation of the underwater super-oleophobic surface from the oil super-hydrophilic state to the super-hydrophobic state is realized by utilizing the synergistic effect of the inorganic aluminum phosphate binder and the functional coating embedded in the binder.
2. The super-wettability of the surface of the stainless steel mesh substrate can be accurately regulated and controlled by regulating and controlling the alkyl acid with different carbon chain lengths.
3. The invention uses the inorganic binder to prepare the super-wetting functional coating with excellent performance, and compared with the organic binder, the super-wetting functional coating is environment-friendly and has little pollution.
4. The materials used in the invention are easy to obtain and low in price; meanwhile, the preparation process is simple and the conditions are mild.
Drawings
The following describes embodiments of the present invention in further detail with reference to the accompanying drawings.
FIG. 1 is a schematic illustration of a controllable process for an underwater super oleophobic coating from super hydrophilic to super hydrophobic under oil in accordance with the present invention.
FIG. 2 shows 6Aa-AP-TiO in the present invention 2 (a, c) with 14Aa-AP-TiO 2 (b, d) scanning electron microscopy and elemental surface distribution maps of the surface; (e) 6Aa-AP-TiO 2 Surface (1), 14Aa-AP-TiO 2 X-ray diffraction patterns of the surface (2) and the original stainless steel mesh (3).
FIG. 3 is a) the contact angles of water and oil drops (hexadecane) on the surfaces of different coatings in the air, the contact angle of the oil drop (1, 2-dichlorohexane) in the water and the contact angle of the water drop in the oil (normal hexane) in the invention, and the function change relationship of the parameter n representing the carbon chain length of the alkyl acid on the surface of the coating; 6Aa-AP-TiO 2 Surface (b) and 14Aa-AP-TiO 2 Surface (c) contact angle pictures of different coating surfaces in air, water and oil drops (hexadecane), oil drops (1, 2-dichlorohexane) in water and water drops in oil (n-hexane).
Fig. 4 is a working principle diagram of the present invention.
Detailed Description
As shown in figures 1 and 4, a suspension prepared by mixing aluminum phosphate, titanium dioxide nanoparticles and alkyl acid is sprayed on a stainless steel net and is continuously heated, and the coating has underwater super-oleophobic property. By changing the carbon chain length of the alkyl acid, the surface chemistry of the coating can be controlled, thereby realizing the fine controllable oil super-wettability.
A controllable method of providing an underwater superoleophobic coating from superhydrophilic to superhydrophobic under oil comprising the steps of:
the method comprises the steps of ultrasonically cleaning a 2300-mesh stainless steel mesh substrate by using acetone, ethanol and deionized water in sequence, cleaning for half an hour each time, and drying for 1 hour at 60 ℃ to obtain the dry stainless steel mesh.
Preparing a spraying solution a of a surface with an alkyl acid carbon chain length n =0 (n = 0), a spraying solution B of a surface with an alkyl acid carbon chain length n =2 (n = 2), a spraying solution C of a surface with an alkyl acid carbon chain length n =4 (n = 4), a spraying solution D of a surface with an alkyl acid carbon chain length n =6 (n = 6), a spraying solution E of a surface with an alkyl acid carbon chain length n =8 (n = 8), a spraying solution F of a surface with an alkyl acid carbon chain length n =10 (n = 10), a spraying solution G of a surface with an alkyl acid carbon chain length n =12 (n = 12), a spraying solution H of a surface with an alkyl acid carbon chain length n =14 (n = 14), and a spraying solution I of a surface with an alkyl acid carbon chain length n =16 (n = 16), respectively. The specific method comprises the following steps:
(1) preparing an inorganic aluminum phosphate binder: diluting phosphoric acid to 60% by using deionized water, adding aluminum hydroxide to ensure that the molar ratio of the phosphoric acid to the aluminum hydroxide is 3;
(2) preparing an aluminum phosphate solution: dissolving 1g of inorganic aluminum phosphate binder in 4 mL of deionized water, and uniformly stirring to obtain the aluminum phosphate binder;
(3) preparing a titanium dioxide dispersion liquid: dispersing 0.5 g of titanium dioxide nanoparticles in 5 mL of absolute ethanol, and performing ultrasonic treatment for 10 minutes to uniformly disperse the titanium dioxide nanoparticles to obtain the titanium dioxide nanoparticles;
(4) 9 parts of the titanium dioxide dispersion were added with 0.02 mmol of an alkyl acid (CH) having a carbon chain length of n =0, 2, 4, 6, 8, 10, 12, 14, 16, respectively 3 (CH 2 ) n COOH), the same volume of aluminum phosphate solution was dropped into the solution after stirring uniformly, and the solution was stirred for half an hour to uniformly mix the solution, thereby obtaining nine kinds of spray solutions a (n = 0), B (n = 2), C (n = 4), D (n = 6), E (n = 8), F (n = 10), G (n = 12), H (n = 14), and I (n = 16).
(1) Preparing an inorganic aluminum phosphate binder: diluting phosphoric acid to 60% by using deionized water, adding aluminum hydroxide to ensure that the molar ratio of the phosphoric acid to the aluminum hydroxide is 3;
(2) preparing an aluminum phosphate solution: dissolving 1g of inorganic aluminum phosphate binder in 4 mL of deionized water, and uniformly stirring to obtain the aluminum phosphate adhesive;
(3) preparing a titanium dioxide dispersion liquid: dispersing 0.5 g of titanium dioxide nanoparticles with the average particle size of 25 nm in 5 mL of absolute ethyl alcohol, and performing ultrasonic treatment for 10 minutes to uniformly disperse the titanium dioxide nanoparticles to obtain the titanium dioxide nanoparticles;
(4) taking 9 parts of titanium dioxide dispersion liquid, and adding carbon chain length n =0, 2, 4, 6, 8, 10 and 1 respectively2, 14, 16 of 0.02 mmol of alkyl acid (CH) 3 (CH 2 ) n COOH), stirring uniformly, dropping the same volume of aluminum phosphate solution, stirring for half an hour to mix uniformly, thereby obtaining nine kinds of spray solutions a (n = 0), B (n = 2), C (n = 4), D (n = 6), E (n = 8), F (n = 10), G (n = 12), H (n = 14), and I (n = 16).
The surfaces of the dried stainless steel mesh were uniformly sprayed with nine kinds of spraying solutions a (n = 0), B (n = 2), C (n = 4), D (n = 6), E (n = 8), F (n = 10), G (n = 12), H (n = 14), I (n = 16), respectively, under a nitrogen gas pressure of 0.2 MPa at room temperature, all using a gas compression spray gun.
Fourthly, respectively placing different coatings obtained through spraying under the condition of 120 ℃ for heating for 2 hours, then continuously curing for 1 hour at 200 ℃, and respectively forming a surface with the alkyl acid carbon chain length n =0, a surface with the alkyl acid carbon chain length n =2, a surface with the alkyl acid carbon chain length n =4, a surface with the alkyl acid carbon chain length n =6, a surface with the alkyl acid carbon chain length n =8, a surface with the alkyl acid carbon chain length n =10, a surface with the alkyl acid carbon chain length n =12, a surface with the alkyl acid carbon chain length n =14 and a surface with the alkyl acid carbon chain length n =16, which are respectively abbreviated as 0Aa-AP-TiO 2 Surface, 2Aa-AP-TiO 2 Surface, 4Aa-AP-TiO 2 Surface, 6Aa-AP-TiO 2 Surface, 8Aa-AP-TiO 2 Surface, 10Aa-AP-TiO 2 Surface, 12Aa-AP-TiO 2 Surface, 14Aa-AP-TiO 2 Surface, 16Aa-AP-TiO 2 A surface.
Spraying the obtained coating by adopting the spraying solutions C and D to obtain super-hydrophilic and oil in air, super-hydrophilic in oil medium and super-oleophobic underwater state; the coating obtained by spraying the spraying solutions H and I can realize super-hydrophilic and oil in the air, super-hydrophobic in an oil medium and super-oleophobic underwater states.
The wettability and surface analysis of the underwater super-oleophobic coating from super-hydrophilic to super-hydrophobic under oil in oil are as follows:
observation of 6Aa-AP-TiO, respectively 2 Surface and 14Aa-AP-TiO 2 The scanning electron microscope image of the surface can show that the material has a microstructure with similar nanostructure accumulation, and the microstructure increases the roughness of the surface of the material and is beneficial to realizing corresponding submerged super-wetting characteristicsAs shown in fig. 2 (a, b). Further by analyzing the element surface distribution, it was found that the coating exhibited a uniform distribution of elements of C, O, P, al and Ti in addition to the elements of Fe and Cr corresponding to the stainless steel net, as shown in fig. 2 (C, d). Furthermore, from X-ray diffraction it can be concluded that the aluminum phosphate binder and titanium dioxide nanoparticles were successfully coated on the surface of the stainless steel mesh (fig. 2 e). After solidification, the coating produced retains the characteristic peaks of the original stainless steel and of P25 (anatase and rutile). Therefore, solidification of the AP binder plays an important role in the formation of the network structure and further cross-linking between the particles and the substrate, while the alkyl acid is a key factor in regulating the controllable preparation of the under-oil super-wetting coating.
In the air, water and oil drop (hexadecane) can spread on all the coating surfaces, and the super-hydrophilicity and super-oleophylic super-amphiphilicity are displayed, and the corresponding contact angle is 0 o (FIG. 3 a). FIG. 3a also shows the contact angle (UOCAs) of the underwater oil drop (1, 2-dichloroethane) of the coating as a function of the carbon-carbon chain length of the alkyl acid and the contact angle (UWCAs) of the water drop in oil (n-hexane). When the parameter (n) of the coating, which is indicative of the carbon chain length of the alkyl acid, is within 4 and 6, the UOCA remains at 150 o Above, the rolling angle is less than 10 o (FIG. 3 a). 6Aa-AP-TiO formed 2 The surface has underwater super oleophobic property, and the UOCA is 155.3 +/-1.9 o The rolling angle is 8.2 +/-0.8 o . However, 6Aa-AP-TiO 2 UWCA of the coating is 0 o The water droplets only need to diffuse in the oil for 48 ms (fig. 3 b). When the parameter (n) is between 14 and 16, both the UOCA and the UWCA of the prepared coating are more than 150 o Roll angle less than 10 o . 14Aa-AP-TiO when the prepared surface is immersed in water 2 The water layer on the surface showed super-oleophobic property, and UOCA was 155.6 + -1.1 o The rolling angle is 8.3 +/-0.7 o . UWCA in oil is 157.6 +/-1.7 o The rolling angle is 7.8 +/-0.8 o It is still easy to reach the oil superhydrophobicity, resulting in dual superhydrophobic properties in the oil-water system (fig. 3 c). When the parameter (n) is in the range of 6-14 and 0-4, the formed nano surface still shows underwater super-oleophobic property. But as the carbon chain length parameter (n) increases from 0 to 4, the UWCA of the nanocoating decreases dramatically. And with the parameter (n) from6 to 14, it sharply increases to 150 o As described above.
Experiments prove that the conversion of the underwater super-oleophobic surface from the oil super-hydrophobicity to the super-hydrophilicity can be effectively regulated and controlled by adjusting the length of the alkyl acid carbon chain of the coating.
Claims (4)
1. A controllable method of providing an underwater super oleophobic coating from super hydrophilic to super hydrophobic under oil comprising the steps of:
the method comprises the steps of ultrasonically cleaning a stainless steel mesh substrate by using acetone, ethanol and deionized water in sequence, cleaning for half an hour each time, and drying to obtain a dry stainless steel mesh;
preparing a spraying solution a of a surface with an alkyl acid carbon chain length n =0 (n = 0), a spraying solution B of a surface with an alkyl acid carbon chain length n =2 (n = 2), a spraying solution C of a surface with an alkyl acid carbon chain length n =4 (n = 4), a spraying solution D of a surface with an alkyl acid carbon chain length n =6 (n = 6), a spraying solution E of a surface with an alkyl acid carbon chain length n =8 (n = 8), a spraying solution F of a surface with an alkyl acid carbon chain length n =10 (n = 10), a spraying solution G of a surface with an alkyl acid carbon chain length n =12 (n = 12), a spraying solution H of a surface with an alkyl acid carbon chain length n =14 (n = 14), and a spraying solution I of a surface with an alkyl acid carbon chain length n =16 (n = 16), respectively;
performing uniform spraying on the surface of the dry stainless steel net at room temperature by using nine spraying solutions a (n = 0), B (n = 2), C (n = 4), D (n = 6), E (n = 8), F (n = 10), G (n = 12), H (n = 14), and I (n = 16) using a gas compression spray gun under a nitrogen gas pressure of 0.2 MPa;
fourthly, the different coatings obtained through spraying are respectively placed under the condition of 120 ℃ to be heated for 2 hours, then 200 ℃ is continuously cured for 1 hour, and a surface with the chain length of the alkyl acid carbon n =0, a surface with the chain length of the alkyl acid carbon n =2, a surface with the chain length of the alkyl acid carbon n =4, a surface with the chain length of the alkyl acid carbon n =6, a surface with the chain length of the alkyl acid carbon n =8, a surface with the chain length of the alkyl acid carbon n =10, a surface with the chain length of the alkyl acid carbon n =12, a surface with the chain length of the alkyl acid carbon n =14 and a surface with the chain length of the alkyl acid carbon n =16 are respectively formed, and are respectively abbreviated as 0Aa-AP-TiO 2 Surface, 2Aa-AP-TiO 2 Surface, 4Aa-AP-TiO 2 Surface, 6Aa-AP-TiO 2 Surface, 8Aa-AP-TiO 2 Surface, 10Aa-AP-TiO 2 Surface, 12Aa-AP-TiO 2 Surface, 14Aa-AP-TiO 2 Surface, 16Aa-AP-TiO 2 A surface.
2. A controllable process for providing an underwater superoleophobic coating from superhydrophilic to superhydrophobic beneath oil in accordance with claim 1 wherein: the mesh number of the stainless steel mesh substrate in the step is 2300 meshes.
3. A controllable process for providing a super hydrophilic to super hydrophobic underwater super oleophobic coating in accordance with claim 1, in which: the spraying solution A (n = 0), B (n = 2), C (n = 4), D (n = 6), E (n = 8), F (n = 10), G (n = 12), H (n = 14) and I (n = 16) in the step II is prepared by the following method:
(1) preparing an inorganic aluminum phosphate binder: diluting phosphoric acid to 60% by using deionized water, adding aluminum hydroxide to ensure that the molar ratio of the phosphoric acid to the aluminum hydroxide is 3;
(2) preparing an aluminum phosphate solution: dissolving 1g of inorganic aluminum phosphate binder in 4 mL of deionized water, and uniformly stirring to obtain the aluminum phosphate binder;
(3) preparing a titanium dioxide dispersion liquid: dispersing 0.5 g of titanium dioxide nanoparticles in 5 mL of absolute ethanol, and performing ultrasonic treatment for 10 minutes to uniformly disperse the titanium dioxide nanoparticles to obtain the titanium dioxide nanoparticles;
(4) 9 parts of the titanium dioxide dispersion were added with 0.02 mmol of an alkyl acid having a carbon chain length of n =0, 2, 4, 6, 8, 10, 12, 14, 16, respectively, and after stirring uniformly, the same volume of an aluminum phosphate solution was added dropwise, and after stirring for half an hour to mix uniformly, nine kinds of spray solutions a (n = 0), B (n = 2), C (n = 4), D (n = 6), E (n = 8), F (n = 10), G (n = 12), H (n = 14), and I (n = 16) were obtained.
4. A controllable method of providing underwater superoleophobic coating from superhydrophilic to superhydrophobic beneath oil in accordance with claim 3, wherein: the average particle diameter of the titanium dioxide particles in the step (3) is 25 nm.
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