CN114717839A - Article with super-hydrophobic surface and preparation method thereof - Google Patents
Article with super-hydrophobic surface and preparation method thereof Download PDFInfo
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- CN114717839A CN114717839A CN202011538147.8A CN202011538147A CN114717839A CN 114717839 A CN114717839 A CN 114717839A CN 202011538147 A CN202011538147 A CN 202011538147A CN 114717839 A CN114717839 A CN 114717839A
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- 230000003075 superhydrophobic effect Effects 0.000 title claims abstract description 50
- 238000002360 preparation method Methods 0.000 title claims abstract description 37
- 238000011065 in-situ storage Methods 0.000 claims abstract description 44
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 41
- 150000004679 hydroxides Chemical class 0.000 claims abstract description 13
- -1 hexadecyltrimethoxysilane modified magnesium aluminum Chemical class 0.000 claims abstract description 5
- 239000004744 fabric Substances 0.000 claims description 61
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 claims description 59
- SNAAJJQQZSMGQD-UHFFFAOYSA-N aluminum magnesium Chemical compound [Mg].[Al] SNAAJJQQZSMGQD-UHFFFAOYSA-N 0.000 claims description 56
- MFUVDXOKPBAHMC-UHFFFAOYSA-N magnesium;dinitrate;hexahydrate Chemical compound O.O.O.O.O.O.[Mg+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MFUVDXOKPBAHMC-UHFFFAOYSA-N 0.000 claims description 38
- RSKGMYDENCAJEN-UHFFFAOYSA-N hexadecyl(trimethoxy)silane Chemical compound CCCCCCCCCCCCCCCC[Si](OC)(OC)OC RSKGMYDENCAJEN-UHFFFAOYSA-N 0.000 claims description 29
- 230000000051 modifying effect Effects 0.000 claims description 29
- 238000000034 method Methods 0.000 claims description 26
- 238000010438 heat treatment Methods 0.000 claims description 22
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 20
- 239000002904 solvent Substances 0.000 claims description 19
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 17
- 239000004202 carbamide Substances 0.000 claims description 17
- 229910052782 aluminium Inorganic materials 0.000 claims description 16
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 16
- 239000011888 foil Substances 0.000 claims description 16
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 12
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 11
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 11
- 238000001035 drying Methods 0.000 claims description 10
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 9
- 229910052751 metal Inorganic materials 0.000 claims description 8
- 239000002184 metal Substances 0.000 claims description 8
- 238000002791 soaking Methods 0.000 claims description 8
- 239000002245 particle Substances 0.000 claims description 6
- 229920006254 polymer film Polymers 0.000 claims description 6
- 229910021529 ammonia Inorganic materials 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 4
- 239000000243 solution Substances 0.000 description 82
- 229920000728 polyester Polymers 0.000 description 29
- 238000006243 chemical reaction Methods 0.000 description 10
- 238000004140 cleaning Methods 0.000 description 10
- 238000012360 testing method Methods 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 8
- 239000008367 deionised water Substances 0.000 description 8
- 229910021641 deionized water Inorganic materials 0.000 description 8
- 229910003023 Mg-Al Inorganic materials 0.000 description 7
- 229910001051 Magnalium Inorganic materials 0.000 description 6
- 238000005406 washing Methods 0.000 description 6
- 239000000463 material Substances 0.000 description 4
- 238000002407 reforming Methods 0.000 description 4
- 238000009736 wetting Methods 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 230000002349 favourable effect Effects 0.000 description 2
- 230000002209 hydrophobic effect Effects 0.000 description 2
- 238000010952 in-situ formation Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 230000002035 prolonged effect Effects 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- NMGRWVWJZHGKLW-UHFFFAOYSA-N C(CCCCCCCCCCCCCCC)[Si](OC)(OC)OC.C(CCCCCCCCCCCCCCC)[Si](OC)(OC)OC Chemical compound C(CCCCCCCCCCCCCCC)[Si](OC)(OC)OC.C(CCCCCCCCCCCCCCC)[Si](OC)(OC)OC NMGRWVWJZHGKLW-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229920003043 Cellulose fiber Polymers 0.000 description 1
- 229910017163 MnFe2O4 Inorganic materials 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- 241000233805 Phoenix Species 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 238000005349 anion exchange Methods 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 230000000845 anti-microbial effect Effects 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- UHYPYGJEEGLRJD-UHFFFAOYSA-N cadmium(2+);selenium(2-) Chemical compound [Se-2].[Cd+2] UHYPYGJEEGLRJD-UHFFFAOYSA-N 0.000 description 1
- AIXMJTYHQHQJLU-UHFFFAOYSA-N chembl210858 Chemical compound O1C(CC(=O)OC)CC(C=2C=CC(O)=CC=2)=N1 AIXMJTYHQHQJLU-UHFFFAOYSA-N 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- FGBJXOREULPLGL-UHFFFAOYSA-N ethyl cyanoacrylate Chemical compound CCOC(=O)C(=C)C#N FGBJXOREULPLGL-UHFFFAOYSA-N 0.000 description 1
- 229940053009 ethyl cyanoacrylate Drugs 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 230000005661 hydrophobic surface Effects 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002114 nanocomposite Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 238000009832 plasma treatment Methods 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 239000004810 polytetrafluoroethylene Substances 0.000 description 1
- 239000002096 quantum dot Substances 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 230000002940 repellent Effects 0.000 description 1
- 239000005871 repellent Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- BTURAGWYSMTVOW-UHFFFAOYSA-M sodium dodecanoate Chemical compound [Na+].CCCCCCCCCCCC([O-])=O BTURAGWYSMTVOW-UHFFFAOYSA-M 0.000 description 1
- 229940082004 sodium laurate Drugs 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
- 230000003313 weakening effect Effects 0.000 description 1
Classifications
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/32—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
- D06M11/36—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
- D06M11/45—Oxides or hydroxides of elements of Groups 3 or 13 of the Periodic System; Aluminates
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/32—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
- D06M11/36—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
- D06M11/44—Oxides or hydroxides of elements of Groups 2 or 12 of the Periodic System; Zincates; Cadmates
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/73—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof
- D06M11/76—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof with carbon oxides or carbonates
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/50—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with organometallic compounds; with organic compounds containing boron, silicon, selenium or tellurium atoms
- D06M13/51—Compounds with at least one carbon-metal or carbon-boron, carbon-silicon, carbon-selenium, or carbon-tellurium bond
- D06M13/513—Compounds with at least one carbon-metal or carbon-boron, carbon-silicon, carbon-selenium, or carbon-tellurium bond with at least one carbon-silicon bond
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- 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
- D06M2101/32—Polyesters
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
- D06M2200/10—Repellency against liquids
- D06M2200/12—Hydrophobic properties
Abstract
The invention discloses an article with a super-hydrophobic surface and a preparation method thereof. The superhydrophobic surface of the article is formed by forming a plurality of hexadecyltrimethoxysilane modified magnesium aluminum layered double hydroxides in situ (in situ) on the surface of the article. The object with the super-hydrophobic surface disclosed by the invention has a water contact angle not less than 130 degrees.
Description
Technical Field
The present invention relates to an article having a superhydrophobic surface and a method for preparing the same, and more particularly, to an article having a superhydrophobic surface having high hydrophobicity, desired water repellency and good washing tolerance and a method for preparing the same.
Background
Due to the unique properties of superhydrophobic articles, such as wettability, self-cleaning, and tack resistance, there has been an increasing interest in superhydrophobic articles in recent years for many research and commercial products. It is known that the wetting behavior of solid surfaces can be controlled by the geometry of the surface and the chemical composition of the material. Recently, the scope of wettability studies has been extended to the fabrication of superhydrophobic surfaces with other functions for application in advanced materials. In this regard, some superhydrophobic surface articles having multiple functions have been prepared by new methods. For example, cellulose fibers were functionalized with different ethylcyanoacrylate nanocomposites shell containing ultraway wax or polytetrafluoroethylene particles to increase hydrophobicity, with MnFe2O4 nanoparticles to increase magnetic properties, with quantum dots CdSe/ZnS to emit light or with nano-silver particles (AgNPs) to obtain antibacterial effect; good self-cleaning and antimicrobial articles are obtained by coating Pt, Au or AgNPs on the surface of the article. However, the above method has disadvantages of expensive coating materials, complicated processes such as plasma treatment or Radio Frequency (RF) sputtering.
In the prior art, it is known to utilize Layered Double Hydroxides (LDHs) on the surface of an article, such as a fabric or cloth, to increase hydrophobicity. The layered double hydroxide may be formed by, for example, hydrolysis, co-precipitation, reconstitution, anion exchange reaction, urea process, sol-gel technique, microwave, ultrasonic or hydrothermal procedures. However, the aforementioned method has disadvantages of requiring high reaction temperature or pressure, not only lowering or weakening the fabric structure, but also being not environmentally friendly. In addition, the conventional layered double hydroxide on the surface has poor cleaning resistance, and the hydrophobicity of the article decreases after cleaning. Thus, prior art articles having a layered double hydroxide on the surface are not suggested for use in durable cloth applications.
Therefore, an object of the present invention is to provide an article having a superhydrophobic surface and a method for preparing the article having the superhydrophobic surface.
Disclosure of Invention
The invention discloses an article with a super-hydrophobic surface and a preparation method for preparing the article with the super-hydrophobic surface. The object with the super-hydrophobic surface has high hydrophobicity, required water repellent performance and good washing tolerance. The object with the super-hydrophobic surface is formed by forming a plurality of magnesium-aluminum layered double hydroxides modified by hexadecyl trimethoxy silane in situ (in situ) on the surface of the object. Hydrophobicity of the surface of the article is enhanced by forming a plurality of hexadecyltrimethoxysilane modified magnesium aluminum layered double hydroxides in situ on the surface of the article. In addition, the article of the present invention can maintain good water repellency after washing.
One object of the present invention is to disclose an article having a superhydrophobic surface. The invention discloses an article with a super-hydrophobic surface, which is formed by forming a plurality of hexadecyl trimethoxy silane modified magnesium-aluminum layered double hydroxides in situ (in situ) on the surface of the article, wherein the water contact angle of the surface of the article is not less than 130 degrees.
In an embodiment of the present disclosure, the particle size of the magnesium-aluminum layered double hydroxide may be between 100 nanometers (nm) and 200 nm.
In an embodiment of the present disclosure, the article may be, for example, a cloth, a metal or a polymer film.
The invention also aims to disclose a preparation method of the object with the super-hydrophobic surface. The preparation method of the article with the superhydrophobic surface can include, but is not limited to, the following steps: (a) mixing magnesium nitrate hexahydrate (Mg (NO3) 2.6H 2O), urea and a first solvent to prepare a solution; (b) soaking an aluminum foil and an article in the solution; (c) heating the solution for a period of time to allow a plurality of magnesium aluminum layered double hydroxides to form in situ (in situ) on the surface of the article; (d) mixing ammonia (NH4OH), hexadecyltrimethoxysilane (hexadecyl trimethoxysilane) and a second solvent to form a modified solution; (e) soaking the article with the magnesium-aluminum layered double hydroxide formed in situ on the surface into the modifying solution; (f) heating the modifying solution for a period of time; and (g) drying the article having the magnesium-aluminum layered double hydroxide formed in situ on the surface.
In one embodiment of the preparation method disclosed herein, in the step (a), the concentration of magnesium nitrate hexahydrate in the solution may be between 3mM and 16mM, and preferably may be between 3.79mM and 15.18 mM.
In one embodiment of the preparation method disclosed in the present invention, in the step (a), the concentration of urea in the solution may be between 0.5mM and 2.2mM, and preferably may be between 0.53mM and 2.14 mM.
In one embodiment of the preparation method disclosed in the present invention, in the step (a), the first solvent may be, for example, an alcohol-free solvent.
In one embodiment of the preparation method disclosed in the present invention, in the step (b), the amount of the aluminum foil added may be between 6 parts by weight and 27 parts by weight, and preferably between 6.5 parts by weight and 26.34 parts by weight, per hundred parts by weight of the magnesium nitrate hexahydrate.
In one embodiment of the preparation method disclosed in the present invention, in the step (c), the heating temperature of the solution may be between 50 ℃ and 100 ℃, and the heating time may be between 6 hours and 48 hours.
In one embodiment of the preparation method disclosed in the present invention, in the step (d), the concentration of the ammonia water in the modified solution may be between 23mM and 95mM, and preferably between 23.5mM and 94 mM.
In one embodiment of the preparation method disclosed in the present invention, in the step (d), the weight ratio of the amount of the hexadecyl trimethoxy silane in the modifying solution to the amount of the material is between 0.005 and 1, and preferably between 0.1 and 0.5.
In one embodiment of the preparation method disclosed in the present invention, in the step (d), the pH of the modifying solution may be between 8 and 14, and preferably between 12 and 13.
In an embodiment of the preparation method disclosed in the present invention, in the step (d), the second solvent may be at least one of water, methanol and ethanol, or a combination thereof.
In one embodiment of the preparation method disclosed in the present invention, in the step (f), the heating temperature of the modifying solution may be between 50 ℃ and 60 ℃, and the heating time is between 1 hour and 3 hours.
In one embodiment of the preparation method disclosed in the present invention, in the step (g), the drying temperature of the article having a plurality of magnesium aluminum layered double hydroxides on the surface thereof may be between 60 ℃ and 80 ℃, and the drying time is between 2 hours and 6 hours.
In an embodiment of the manufacturing method disclosed in the present invention, the article may be, but is not limited to, cloth, metal or polymer film.
It is another object of the present invention to provide an article with a superhydrophobic surface, which is prepared by the preparation method.
The above summary is intended to provide a simplified summary of the disclosure in order to provide a basic understanding to the reader of the disclosure. This summary is not an extensive overview of the disclosure and is intended to neither identify key/critical elements of the embodiments nor delineate the scope of the embodiments. The basic spirit of the present invention and the technical means and embodiments thereof will be readily understood by those skilled in the art after considering the following embodiments.
Detailed Description
In order to make the disclosure more complete and complete, the following description sets forth illustrative aspects and embodiments of the invention; it is not intended to be the only form in which the embodiments of the invention may be practiced or utilized. The embodiments disclosed below may be combined with or substituted for one another where appropriate, and additional embodiments may be added to one embodiment without further recitation or description.
The advantages, features, and technical solutions of the present invention will be described in greater detail with reference to exemplary embodiments for easier understanding, and the present invention may be embodied in different forms, so should not be construed as limited to the embodiments set forth herein, but rather should be provided for enabling one of ordinary skill in the art to more fully and completely convey the scope of the present invention and the present invention is defined only by the appended claims.
Unless otherwise defined, all terms (including technical and scientific terms) and terminology used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs, and terms such as those defined in commonly used dictionaries should be interpreted as having a meaning that is consistent with their meaning in the context of the relevant art and will not be interpreted in an overly idealized or overly formal sense unless expressly so defined herein.
It is an object of the present invention to disclose an article having a superhydrophobic surface that can have a high hydrophobicity, a desired resistance to water spillage, and a good wash tolerance. The water contact angle of the article with the super-hydrophobic surface disclosed by the invention can be not less than 130 degrees, and preferably can be between 130 degrees and 145 degrees. The invention discloses an article with a super-hydrophobic surface, which is formed by forming a plurality of magnesium-aluminum layered double hydroxides modified by hexadecyl trimethoxy silane in situ (in situ) on the surface of the article.
In one embodiment of the present disclosure, the in-situ formation of the magnesium aluminum layered double hydroxide on the surface of the article is performed by immersing the aluminum foil and the article in a solution containing magnesium nitrate hexahydrate, urea and a solvent and heating the solution for a period of time to form the magnesium aluminum layered double hydroxide on the surface of the article in-situ, but is not limited thereto.
In one embodiment of the present disclosure, the particle size of the mg-al layered double hydroxide can be between 100 nanometers (nm) and 200 nanometers (nm), and the present invention uses mg-al layered double hydroxide with smaller particle size, which is less prone to cracking or breaking during cleaning, so that the article can have better cleaning tolerance.
In one embodiment of the present disclosure, the magnesium-aluminum layered double hydroxide modified with hexadecyl trimethoxysilane formed in situ on the surface of the article is modified by immersing the article having magnesium-aluminum layered double hydroxide on the surface in a modifying solution containing ammonia, hexadecyl trimethoxysilane and a solvent.
In one embodiment of the present disclosure, the cleaning resistance of the article can be improved because hexadecyl trimethoxy silane has methyl functional groups and long carbon chains.
In an embodiment of the present disclosure, the article may be, for example, a cloth, a metal or a polymer film, but is not limited thereto.
The article with a superhydrophobic surface disclosed by the invention can be used as a durable hydrophobic cloth, such as a jacket, or used in a wastewater treatment system, such as an oil-water separation technology.
The invention also aims to disclose a preparation method of the object with the super-hydrophobic surface. The disclosed methods may include, but are not limited to, the following steps. The preparation method of the article with the super-hydrophobic surface disclosed by the invention has the advantages of simple process, environmental friendliness and the like.
First, magnesium nitrate hexahydrate, urea and a first solvent are mixed to form a solution. In one embodiment of the disclosed preparation method, the concentration of magnesium nitrate hexahydrate in the solution may be between 3mM and 16mM, and preferably between 3.79mM and 15.18 mM. When the concentration of magnesium nitrate hexahydrate in solution is above the aforementioned range, the magnesium aluminum layered double hydroxide will be highly grown or aggregated and will be non-uniform. When the concentration of magnesium nitrate hexahydrate in the solution is lower than the aforementioned range, the magnesium-aluminum layered double hydroxide will not grow sufficiently or be very minute. The concentration of urea in the solution may be between 0.5mM and 2.2mM, and preferably may be between 0.53mM and 2.14 mM. When the concentration of urea in the solution is higher than the aforementioned range, the magnesium aluminum layered double hydroxide will grow or aggregate highly and will be non-uniform. When the concentration of urea in the solution is lower than the above range, there is a possibility that the reaction may not be sufficiently performed.
The first solvent suitable for the aforementioned solution can be, for example, an alcohol-free solvent, and in an embodiment of the preparation method disclosed in the present invention, the first solvent can be, for example, water, but is not limited thereto.
Then, the aluminum foil and the article are soaked into the solution and the solution is heated until the magnesium-aluminum layered double hydroxide is formed in situ (in situ) on the surface of the article.
In one embodiment of the preparation method disclosed in the present invention, the amount of the aluminum foil may be between 6 parts by weight and 27 parts by weight, and preferably between 6.5 parts by weight and 26.34 parts by weight, per hundred parts by weight of magnesium nitrate hexahydrate.
Suitable articles may be, for example, cloth, metal or polymer films, but are not limited thereto.
In an embodiment of the preparation method disclosed in the present invention, the heating temperature of the solution may be between 50 ℃ and 100 ℃, and the heating time may be between 6 hours and 48 hours. When the aluminum foil and the article are immersed in the solution for a time or heated at a temperature higher than the above range, the magnesium-aluminum layered double hydroxide will grow or aggregate highly and will be non-uniform. When the time for soaking the aluminum foil and the articles in the solution or the heating temperature is lower than the above range, the reaction speed is too slow or sufficient magnesium-aluminum layered double hydroxide cannot be generated.
In one embodiment of the preparation method disclosed in the present invention, after the in-situ formation of the magnesium-aluminum layered double hydroxide on the surface of the article, the article with the in-situ formed magnesium-aluminum layered double hydroxide on the surface can be selectively dried, the drying temperature can be between 60 ℃ and 80 ℃, and the drying time can be between 6 hours and 16 hours.
After forming magnesium aluminum layered double hydroxide in situ on the surface of the article, ammonia, hexadecyl trimethoxy silane and a second solvent are mixed to form a modified solution.
In one embodiment of the disclosed preparation method, the concentration of ammonia in the modified solution may be between 23mM and 95mM, and preferably between 23.5mM and 94 mM. When the concentration of the aqueous ammonia in the modifying solution is higher than the above range, hexadecyltrimethoxysilane is in the form of a gel or a solid, which is not favorable for the modification. When the concentration of the aqueous ammonia in the reforming solution is lower than the above range, the reaction time is prolonged.
In one embodiment of the disclosed preparation method, the ratio of the amount of hexadecyl trimethoxy silane in the modifying solution to the weight of the article can be between 0.005 and 1, and preferably between 0.1 and 0.5. When the concentration of hexadecyltrimethoxysilane in the modifying solution is higher than the aforementioned range, the surface of the article may be hardened. When the concentration of hexadecyltrimethoxysilane in the modifying solution is lower than the aforementioned range, the uniformity of hexadecyltrimethoxysilane is affected.
In one embodiment of the disclosed preparation method, the pH of the modifying solution may be between 8 and 14, and preferably between 12 and 13. When the pH value of the modifying solution is higher than the above range, the hexadecyl trimethoxy silane is in a gel or solid state, which is not favorable for modifying. When the pH of the reforming solution is lower than the above range, the reaction time is prolonged.
The second solvent suitable for the reforming solution may be, for example, at least one of water, methanol, and ethanol, or a combination thereof, but is not limited thereto.
After forming the modifying solution, soaking the article with the magnesium-aluminum layered double hydroxide formed on the surface in situ (in situ) into the modifying solution, and heating the modifying solution for a period of time.
In one embodiment of the preparation method disclosed in the present invention, the heating temperature of the modifying solution may be between 50 ℃ and 60 ℃, and the heating time may be between 1 hour and 3 hours. When the article having the magnesium-aluminum layered double hydroxide formed in situ on the surface thereof is immersed in the reforming solution for a time or heated at a temperature higher than the above range, the solvent may be evaporated. When the time for soaking the article having the magnesium-aluminum layered double hydroxide formed in situ (in situ) on the surface in the modifying solution or the heating temperature is lower than the above range, the modifying effect is affected.
Finally, the article having the surface in situ (in situ) formed with the magnesium aluminum layered double hydroxide is dried. In one embodiment of the preparation method disclosed in the present invention, the drying temperature of the article with the magnesium-aluminum layered double hydroxide formed in situ on the surface thereof may be between 60 ℃ and 80 ℃, and the drying time may be between 2 hours and 6 hours.
It is another object of the present invention to provide an article with a superhydrophobic surface, wherein a plurality of magnesium-aluminum layered double hydroxides modified by hexadecyl trimethoxy silane are formed in situ on the surface of the article, and the article is prepared by the above preparation method of the article with a superhydrophobic surface.
In one embodiment of the present disclosure, the article can be used as a durable hydrophobic cloth or in a sewage treatment system.
Compared with the conventional preparation method of the object with the super-hydrophobic surface, the method disclosed by the invention comprises the steps of forming the magnesium-aluminum layered double hydroxide in situ (in situ) on the surface of the object, soaking the object with the magnesium-aluminum layered double hydroxide formed in situ (in situ) on the surface into the modifying solution containing hexadecyl trimethoxy silane, and then heating the modifying solution. The preparation method of the object with the super-hydrophobic surface disclosed by the invention has the advantages of environmental friendliness due to less chemicals and lower heating temperature. Meanwhile, the preparation method of the article with the super-hydrophobic surface disclosed by the invention also has the advantages of simple process, mass production, easiness in operation and the like. The object with the super-hydrophobic surface prepared by the preparation method disclosed by the invention also has the advantages of high hydrophobicity, required water resistance, good washing tolerance and the like.
The following examples are intended to further illustrate the invention, but the disclosure is not limited thereto.
Examples
Example 1
First, 4.1 grams of magnesium nitrate hexahydrate and 0.58 grams of urea were dissolved in 280ml of water to form a solution. 0.54 grams of aluminum foil and 2.5 grams of polyester cloth were then added to the solution and the solution was heated at 70 ℃ for 46 hours to form magnesium aluminum layered double hydroxide (Mg-Al LDH) in situ on the surface of the cloth. After the reaction was completed, the polyester cloth having magnesium aluminum layered double hydroxide on the surface was washed with deionized water and placed in an oven to dry at 60 ℃ for 16 hours.
Subsequently, 25ml of ethanol, 0.75ml of ammonia water, and 0.25 g of hexadecyltrimethoxysilane (Dynasylan 9116, available from winning industry, germany) were mixed and heated to 50 ℃ and stirred for 1 hour to form a modified solution. 2.5 g of polyester cloth with magnesium-aluminum layered double hydroxide on the surface was immersed in the modifying solution and heated at 50 ℃ for 3 hours. Then the polyester cloth with the magnalium layered double hydroxide is taken out and dried for 2.5 hours at 60 ℃ to prepare the cloth with the super-hydrophobic surface.
Example 2
First, 2.05 grams of magnesium nitrate hexahydrate and 0.58 grams of urea were dissolved in 280ml of water to form a solution. 0.54 grams of aluminum foil and 2.5 grams of polyester cloth were then added to the solution and the solution was heated at 70 ℃ for 46 hours to form magnesium aluminum layered double hydroxide (Mg-Al LDH) in situ on the surface of the cloth. After the reaction was completed, the polyester cloth having magnesium aluminum layered double hydroxide on the surface was washed with deionized water and placed in an oven to dry at 60 ℃ for 16 hours.
Subsequently, 25ml of ethanol, 1.65ml of ammonia water, and 0.25 g of hexadecyltrimethoxysilane (Dynasylan 9116, available from the winning industry, germany) were mixed and heated to 50 ℃ and stirred for 1 hour to form a modified solution. 2.5 g of polyester cloth with magnesium-aluminum layered double hydroxide on the surface was immersed in the modifying solution and heated at 50 ℃ for 3 hours. Then the polyester cloth with the magnesium-aluminum layered double hydroxide is taken out and dried for 2.5 hours at the temperature of 60 ℃ to prepare the cloth with the super-hydrophobic surface.
Example 3
First, 8.2 grams of magnesium nitrate hexahydrate and 0.58 grams of urea were dissolved in 280ml of water to form a solution. 0.54 grams of aluminum foil and 2.5 grams of polyester cloth were then added to the solution and the solution was heated at 70 ℃ for 46 hours to form magnesium aluminum layered double hydroxide (Mg-Al LDH) in situ on the surface of the cloth. After the reaction was completed, the polyester cloth having magnesium-aluminum layered double hydroxide on the surface was washed with deionized water and placed in an oven to dry at 60 ℃ for 16 hours.
Subsequently, 25ml of ethanol, 1.62ml of ammonia water, and 0.25 g of hexadecyltrimethoxysilane (Dynasylan 9116, available from winning industry, germany) were mixed and heated to 50 ℃ and stirred for 1 hour to form a modified solution. 2.5 g of polyester cloth with magnesium-aluminum layered double hydroxide on the surface was immersed in the modifying solution and heated at 50 ℃ for 3 hours. Then the polyester cloth with the magnalium layered double hydroxide is taken out and dried for 2.5 hours at 60 ℃ to prepare the cloth with the super-hydrophobic surface.
Example 4
First, 4.1 grams of magnesium nitrate hexahydrate and 0.29 grams of urea were dissolved in 280ml of water to form a solution. 0.54 grams of aluminum foil and 2.5 grams of polyester cloth were then added to the solution and the solution was heated at 70 ℃ for 46 hours to form magnesium aluminum layered double hydroxide (Mg-Al LDH) in situ on the surface of the cloth. After the reaction was completed, the polyester cloth having magnesium-aluminum layered double hydroxide on the surface was washed with deionized water and placed in an oven to dry at 60 ℃ for 16 hours.
Subsequently, 25ml of ethanol, 1.65ml of ammonia water, and 0.25 g of hexadecyltrimethoxysilane (Dynasylan 9116, available from winning industry, germany) were mixed and heated to 50 ℃ and stirred for 1 hour to form a modified solution. 2.5 g of polyester cloth with magnesium-aluminum layered double hydroxide on the surface was immersed in the modifying solution and heated at 50 ℃ for 3 hours. Then the polyester cloth with the magnalium layered double hydroxide is taken out and dried for 2.5 hours at 60 ℃ to prepare the cloth with the super-hydrophobic surface.
Example 5
First, 4.1 grams of magnesium nitrate hexahydrate and 0.58 grams of urea were dissolved in 280ml of water to form a solution. 0.54 grams of aluminum foil and 2.5 grams of polyester cloth were then added to the solution and the solution was heated at 70 ℃ for 46 hours to form magnesium aluminum layered double hydroxide (Mg-Al LDH) in situ on the surface of the cloth. After the reaction was completed, the polyester cloth having magnesium-aluminum layered double hydroxide on the surface was washed with deionized water and placed in an oven to dry at 60 ℃ for 16 hours.
Subsequently, 25ml of ethanol, 1.65ml of ammonia water, and 0.25 g of hexadecyltrimethoxysilane (Dynasylan 9116, available from winning industry, germany) were mixed and heated to 50 ℃ and stirred for 1 hour to form a modified solution. 2.5 g of polyester cloth with magnesium-aluminum layered double hydroxide on the surface was immersed in the modifying solution and heated at 50 ℃ for 3 hours. Then the polyester cloth with the magnalium layered double hydroxide is taken out and dried for 2.5 hours at 60 ℃ to prepare the cloth with the super-hydrophobic surface.
Comparative example 1
First, 4.1 grams of magnesium nitrate hexahydrate and 1.16 grams of urea were dissolved in 280ml of water to form a solution. 0.54 grams of aluminum foil and 2.5 grams of polyester cloth were then added to the solution and the solution was heated at 70 ℃ for 46 hours to form magnesium aluminum layered double hydroxide (Mg-Al LDH) in situ on the surface of the cloth. After the reaction was completed, the polyester cloth having magnesium-aluminum layered double hydroxide on the surface was washed with deionized water and placed in an oven to dry at 60 ℃ for 16 hours.
Subsequently, 2.5 g of polyester cloth having magnesium-aluminum layered double hydroxide on the surface was immersed in a 2M sodium laurate aqueous solution at 25 ℃ for 2 hours, and then the polyester cloth having magnesium-aluminum layered double hydroxide was taken out and washed with water and ethanol. Finally, the polyester fabric with the magnalium layered double hydroxide is dried for 2.5 hours at 60 ℃ to prepare the fabric with the super-hydrophobic surface.
Comparative example 2
First, 4.1 grams of magnesium nitrate hexahydrate and 0.58 grams of urea were dissolved in 280ml of water to form a solution. 0.54 grams of aluminum foil and 2.5 grams of polyester cloth were then added to the solution and the solution was heated at 70 ℃ for 46 hours to form magnesium aluminum layered double hydroxide (Mg-Al LDH) in situ on the surface of the cloth. After the reaction was completed, the polyester cloth having magnesium aluminum layered double hydroxide on the surface was washed with deionized water and placed in an oven to dry at 60 ℃ for 16 hours.
Subsequently, 25ml of ethanol, 1.67ml of ammonia water, and 0.025 g of hexadecyltrimethoxysilane (Dynasylan 9116, available from the winning industry, germany) were mixed and heated to 50 ℃ and stirred for 1 hour to form a modified solution. 2.5 g of polyester cloth with magnesium-aluminum layered double hydroxide on the surface was immersed in the modifying solution and heated at 50 ℃ for 3 hours. Then the polyester cloth with the magnalium layered double hydroxide is taken out and dried for 2.5 hours at 60 ℃ to prepare the cloth with the super-hydrophobic surface.
Water contact angle measurement
The water contact angles of the surfaces of the cloth having a superhydrophobic Surface of the examples and comparative examples were measured by a contact angle analyzer (Phoenix 150, available from Surface Electro Optics Co, korea).
Water repellency test
The water repellency was evaluated according to AATCC 22-2005. Three pieces of a test piece having a size of 180.0X 180.0mm were cut out from each of the cloths of examples and comparative examples, and the test piece was fitted with a metal ring having a diameter of 150. + -.5 mm so that the test piece was directed in the direction of water spraying, and the distance between the test piece and the metal nozzle was 150. + -.2 mm. Next, 250mL of deionized water was sprayed onto the sample with a nozzle for 20 to 30 seconds. Finally, after the sample is knocked, the pattern formed by wetting the sample is compared with the standard picture.
ISO 5 indicates no wet mark on the surface, rated according to the water splash test standard; ISO 4 indicates a slight surface wetting mark; ISO 3 indicates that the spray point of the surface nozzle has a wetting mark; most of the ISO 2 surface is wet; ISO 1 indicates that the surface is entirely wet; ISO 0 indicates that the specimen is completely wetted.
Cleaning resistance test
After the cloth having the hydrophobic surface of the examples and comparative examples was washed ten times in accordance with AATCC TM 135 standard, the water repellency after washing was measured according to the aforementioned water repellency test method.
Table 1: test results of examples and comparative examples
As can be seen from the test results listed in table 1, the water contact angles of examples 1 to 5 were all 135 °. Therefore, the fabrics of examples 1 to 5 of the present invention all had more excellent hydrophobicity than comparative example 1. In addition, the water repellency of the fabrics of examples 1 to 5 was maintained at ISO 5 after the cleaning, and it was found that good hydrophobicity and water repellency were maintained after the cleaning. On the other hand, the fabrics of comparative examples 1 and 2 were too low in the washing resistance to be used as durable fabrics. The above description is only for the preferred embodiment of the present invention and should not be construed as limiting the scope of the present invention, and any person skilled in the art can make further modifications and variations without departing from the spirit and scope of the present invention.
Claims (17)
1. An article having a superhydrophobic surface, comprising:
an article; and
a plurality of hexadecyl trimethoxy silane modified magnesium-aluminum layered double hydroxides are formed on one surface of the article in situ (in situ), and the water contact angle of the surface is not less than 130 degrees.
2. The article with a superhydrophobic surface of claim 1, wherein the particle size of the magnesium aluminum layered double hydroxide is between 100 nanometers (nm) and 200 nm.
3. The article with a superhydrophobic surface of claim 1, wherein the article is a cloth, a metal or a polymer film.
4. A preparation method of an article with a super-hydrophobic surface is characterized by comprising the following steps:
(a) mixing magnesium nitrate hexahydrate, urea and a first solvent to prepare a solution;
(b) soaking an aluminum foil and an article in the solution;
(c) heating the solution for a period of time to allow a plurality of magnesium-aluminum layered double hydroxides to form in situ on a surface of the article;
(d) mixing ammonia water, hexadecyl trimethoxy silane and a second solvent to form a modified solution;
(e) soaking the article with the magnesium-aluminum layered double hydroxide formed in situ on the surface into the modified solution;
(f) heating the modifying solution for a period of time; and
(g) drying the article with the magnesium-aluminum layered double hydroxide formed in situ on the surface.
5. The method of claim 4, wherein the concentration of magnesium nitrate hexahydrate in the solution is between 3mM and 16 mM.
6. The method for preparing an article with a superhydrophobic surface of claim 4, wherein the urea concentration in the step (a) is between 0.5mM and 2.2 mM.
7. The method for preparing an article having a superhydrophobic surface of claim 4, wherein the first solvent in the previous step (a) is an alcohol-free solvent.
8. The method of claim 4, wherein the aluminum foil is added in an amount of 6 to 27 parts by weight per hundred parts by weight of magnesium nitrate hexahydrate.
9. The method according to claim 4, wherein the heating temperature in the step (c) is between 50 ℃ and 100 ℃ and the heating time is between 6 hours and 48 hours.
10. The method according to claim 4, wherein the concentration of ammonia in the modifying solution is between 23mM and 95 mM.
11. The method of claim 4, wherein the ratio of the amount of hexadecyl trimethoxy silane used in the step (d) to the weight of the article is 0.005 to 1.
12. The method of claim 4, wherein the pH of step (d) is between 8 and 14.
13. The method of claim 4, wherein the second solvent in step (d) is at least one selected from the group consisting of water, methanol and ethanol, or a combination thereof.
14. The method according to claim 4, wherein the heating temperature in the step (f) is between 50 ℃ and 60 ℃ and the heating time is between 1 hour and 3 hours.
15. The method of claim 4, wherein the drying temperature of the article with multiple magnesium aluminum layered double hydroxides on the surface in the step (g) is between 60 ℃ and 80 ℃, and the drying time is between 2 hours and 6 hours.
16. The method of claim 4, wherein the article is a cloth, a metal or a polymer film.
17. An article having a superhydrophobic surface, wherein the article having a superhydrophobic surface is prepared by the preparation method of any one of claims 4-16.
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