CN115787306A - Preparation method of high-robustness super-hydrophobic anti-icing fabric - Google Patents
Preparation method of high-robustness super-hydrophobic anti-icing fabric Download PDFInfo
- Publication number
- CN115787306A CN115787306A CN202211517997.9A CN202211517997A CN115787306A CN 115787306 A CN115787306 A CN 115787306A CN 202211517997 A CN202211517997 A CN 202211517997A CN 115787306 A CN115787306 A CN 115787306A
- Authority
- CN
- China
- Prior art keywords
- fabric
- icing
- bisphenol
- super
- pdms
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 239000004744 fabric Substances 0.000 title claims abstract description 136
- 230000003075 superhydrophobic effect Effects 0.000 title claims abstract description 98
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 54
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 39
- 239000004205 dimethyl polysiloxane Substances 0.000 claims abstract description 36
- 235000013870 dimethyl polysiloxane Nutrition 0.000 claims abstract description 36
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims abstract description 36
- 239000000243 solution Substances 0.000 claims abstract description 33
- 239000007921 spray Substances 0.000 claims abstract description 33
- 238000005507 spraying Methods 0.000 claims abstract description 23
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 22
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000005543 nano-size silicon particle Substances 0.000 claims abstract description 19
- 239000011259 mixed solution Substances 0.000 claims abstract description 16
- 239000004841 bisphenol A epoxy resin Substances 0.000 claims abstract description 14
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 11
- 238000001035 drying Methods 0.000 claims abstract description 10
- 239000000203 mixture Substances 0.000 claims abstract description 10
- 238000002156 mixing Methods 0.000 claims abstract description 7
- 239000002105 nanoparticle Substances 0.000 claims abstract description 5
- CXQXSVUQTKDNFP-UHFFFAOYSA-N octamethyltrisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)O[Si](C)(C)C CXQXSVUQTKDNFP-UHFFFAOYSA-N 0.000 claims abstract 8
- 238000004987 plasma desorption mass spectroscopy Methods 0.000 claims abstract 8
- LCFVJGUPQDGYKZ-UHFFFAOYSA-N Bisphenol A diglycidyl ether Chemical compound C=1C=C(OCC2OC2)C=CC=1C(C)(C)C(C=C1)=CC=C1OCC1CO1 LCFVJGUPQDGYKZ-UHFFFAOYSA-N 0.000 claims description 19
- 238000000034 method Methods 0.000 claims description 16
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 7
- 229920006395 saturated elastomer Polymers 0.000 claims description 4
- 238000004140 cleaning Methods 0.000 abstract description 15
- 239000000126 substance Substances 0.000 abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 18
- 239000007788 liquid Substances 0.000 description 13
- 239000000123 paper Substances 0.000 description 13
- 238000000576 coating method Methods 0.000 description 11
- 239000004753 textile Substances 0.000 description 11
- 239000003822 epoxy resin Substances 0.000 description 10
- 235000019441 ethanol Nutrition 0.000 description 10
- 229920000647 polyepoxide Polymers 0.000 description 10
- 239000011248 coating agent Substances 0.000 description 9
- 238000012360 testing method Methods 0.000 description 9
- 239000003795 chemical substances by application Substances 0.000 description 8
- 239000000835 fiber Substances 0.000 description 8
- 230000002209 hydrophobic effect Effects 0.000 description 8
- 238000005406 washing Methods 0.000 description 8
- 229910004298 SiO 2 Inorganic materials 0.000 description 6
- 239000000853 adhesive Substances 0.000 description 6
- 230000001070 adhesive effect Effects 0.000 description 6
- 238000007790 scraping Methods 0.000 description 6
- 229920000742 Cotton Polymers 0.000 description 5
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 5
- 239000008367 deionised water Substances 0.000 description 5
- 229910021641 deionized water Inorganic materials 0.000 description 5
- 229910052731 fluorine Inorganic materials 0.000 description 5
- 239000011737 fluorine Substances 0.000 description 5
- 230000008859 change Effects 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- -1 polydimethylsiloxane Polymers 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 238000001878 scanning electron micrograph Methods 0.000 description 4
- 239000006228 supernatant Substances 0.000 description 4
- 239000000725 suspension Substances 0.000 description 4
- 240000002853 Nelumbo nucifera Species 0.000 description 3
- 235000006508 Nelumbo nucifera Nutrition 0.000 description 3
- 235000006510 Nelumbo pentapetala Nutrition 0.000 description 3
- 241000274582 Pycnanthus angolensis Species 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 241000607479 Yersinia pestis Species 0.000 description 3
- 230000001680 brushing effect Effects 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 239000000428 dust Substances 0.000 description 3
- 230000003628 erosive effect Effects 0.000 description 3
- 239000004530 micro-emulsion Substances 0.000 description 3
- 239000011087 paperboard Substances 0.000 description 3
- 238000007639 printing Methods 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 238000001694 spray drying Methods 0.000 description 3
- 231100000701 toxic element Toxicity 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 238000005299 abrasion Methods 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 description 2
- 239000003431 cross linking reagent Substances 0.000 description 2
- 238000005520 cutting process Methods 0.000 description 2
- 239000011505 plaster Substances 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 238000012113 quantitative test Methods 0.000 description 2
- 238000002791 soaking Methods 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 238000012876 topography Methods 0.000 description 2
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 description 1
- 241000272194 Ciconiiformes Species 0.000 description 1
- 239000006087 Silane Coupling Agent Substances 0.000 description 1
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical class [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 1
- 241000219793 Trifolium Species 0.000 description 1
- 241001147416 Ursus maritimus Species 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000011324 bead Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000003139 buffering effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000013098 chemical test method Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 230000003111 delayed effect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000003618 dip coating Methods 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 230000008014 freezing Effects 0.000 description 1
- 238000007710 freezing Methods 0.000 description 1
- 231100001261 hazardous Toxicity 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000009863 impact test Methods 0.000 description 1
- 238000002329 infrared spectrum Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229960000907 methylthioninium chloride Drugs 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000011664 nicotinic acid Substances 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 230000002572 peristaltic effect Effects 0.000 description 1
- 239000002504 physiological saline solution Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000010079 rubber tapping Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 238000004506 ultrasonic cleaning Methods 0.000 description 1
- 238000009281 ultraviolet germicidal irradiation Methods 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
Images
Landscapes
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Abstract
The invention discloses a preparation method of a high-robustness super-hydrophobic anti-icing fabric, which comprises the following steps: adding PDMS and bisphenol A epoxy resin into absolute ethyl alcohol to obtain PDMS and bisphenol A epoxy resin solution; adding the nano particles and 3-aminopropyltriethoxysilane into absolute ethanol, and uniformly dispersing to obtain a nano silicon dioxide mixed solution; mixing PDMS, bisphenol A epoxy resin solution and nano-silica mixed solution, and dispersing the mixture uniformly by ultrasonic waves to obtain a spray; and spraying the spray on the fabric, and drying to obtain the high-robustness super-hydrophobic anti-icing fabric. The contact angle of the super-hydrophobic fabric is as high as 162 degrees, and the super-hydrophobic fabric has anti-icing and self-cleaning performances, and can still maintain the contact angle of more than 150 degrees even after being worn 1200 times by using abrasive paper. The surface still shows excellent hydrophobicity after being tested by other extreme physical and chemical environments.
Description
Technical Field
The invention relates to the technical field of super-hydrophobic materials, in particular to a preparation method of a high-robustness super-hydrophobic anti-icing fabric.
Background
Inspired by natural organisms such as lotus leaves, polar bear hair, clover, penguin and the like, the super-hydrophobic surface with a Water Contact Angle (WCA) of more than 150 degrees and a Sliding Angle (SA) of less than 10 degrees plays an important role in interface application such as self-cleaning, anti-icing, drag reduction, oil-water separation, metal corrosion protection, wearable equipment and the like due to the characteristics of the super-hydrophobic surface. With the deep development of research on super-hydrophobic and anti-icing materials, the lotus leaf bionic hydrophobic coating surface is found to be an effective anti-icing material surface, and has longer freezing delay time and lower ice adhesion strength. The existing textile is easily wetted by water, and is also easily frozen in a cold environment, so that the clothes lose the function of keeping warm. Therefore, under extreme weather conditions, the development of a strong textile with super-hydrophobic and anti-icing functions for outdoor clothing is of great significance. However, the surface of the prepared fabric contains toxic elements such as fluorine, the process is complex, harmful gas is generated in the preparation process, and the durability hinders the development of the super-hydrophobic anti-icing fabric.
In summary, the current methods for manufacturing superhydrophobic fabrics by dip coating, vapor deposition and the like have the following disadvantages:
(1) The preparation process is complicated.
(2) The durability is insufficient.
(3) Contains toxic elements such as fluorine.
Disclosure of Invention
In order to overcome the problems in the prior art, the invention aims to provide a preparation method of a high-robustness superhydrophobic anti-icing fabric, which is simple in process, good in durability, free of toxic elements such as fluorine and the like, convenient to produce and long in service life.
In order to achieve the purpose, the invention adopts the technical scheme that:
a preparation method of a high-robustness super-hydrophobic anti-icing fabric comprises the following steps:
adding PDMS and bisphenol A epoxy resin into absolute ethyl alcohol to obtain PDMS and bisphenol A epoxy resin solution;
adding the nano particles and 3-aminopropyltriethoxysilane into absolute ethanol, and uniformly dispersing to obtain a nano silicon dioxide mixed solution;
mixing PDMS (polydimethylsiloxane), bisphenol A epoxy resin solution and nano silicon dioxide mixed solution, and uniformly dispersing by ultrasonic waves to obtain a spray; and spraying the spray on the fabric, and drying to obtain the high-robustness super-hydrophobic anti-icing fabric.
Further, the bisphenol a type epoxy resin is bisphenol a diglycidyl ether.
Furthermore, the PDMS and bisphenol a type epoxy resin solution is saturated with PDMS and bisphenol a type epoxy resin.
Further, the nanoparticles are nano-silica.
Furthermore, the mass fraction of the nano silicon dioxide in the nano silicon dioxide mixed solution is 2-4%.
Further, the mass fraction of 3-aminopropyltriethoxysilane was 16%.
Furthermore, the mass concentration of the nano silicon dioxide in the spray is 0.5-3%.
Further, the ultrasonic dispersion time is 30-60 min.
Compared with the prior art, the invention has the following beneficial effects:
the invention uses 3-aminopropyl triethoxysilane as cross-linking agent, cross-links bisphenol A type epoxy resin and polydimethylsiloxane, does not contain any fluorine element, forms low surface energy, and introduces nano silicon dioxide to construct micro emulsion structure on the fiber surface. The micro-emulsion head structure enables the contact angle of the super-hydrophobic fabric to reach 162 degrees and has super-hydrophobic performance. The superhydrophobic fabric surface has significant anti-icing properties because the droplets create less heterogeneous nucleation on the superhydrophobic surface and because the contact area with the cold surface is smaller, reducing the heat transfer rate. Due to the action of the bisphenol A epoxy resin and the 3-aminopropyltriethoxysilane, a firm molecular bridge is formed between the coating formed after the spray liquid is cured and the fabric, so that the adhesive force between the coating and the fiber of the fabric is improved. Due to the strong adhesion of the coating to the substrate, and the impact buffering of PDMS as a soft segment and the friction reducing layer, even after the abrasive paper with 320mesh is worn 1200 times, the contact angle (super-hydrophobic) of more than 150 degrees can be still maintained. The surface still exhibits excellent hydrophobicity as tested by other extreme physical and chemical environments such as (knife-scraping, acid etching). The whole preparation process only uses four reagents, and a two-step method is used in the preparation process, so that the problem that the existing preparation process of the super-hydrophobic fabric is complex is solved. Also, such coatings can be easily grafted onto garments and paper by a two-step spray drying process. More importantly, the super-hydrophobic surface has obvious anti-icing and self-cleaning performances. Therefore, the high-robustness super-hydrophobic anti-icing fabric spray and the preparation method thereof have a good application scene in real life. The preparation method has simple preparation process, only uses a two-step spray drying method, and has low cost. The preparation process is safe, no hazardous gas is generated, the components do not contain fluorine elements, and the preparation method is green and environment-friendly. The coating prepared by the invention is firm and wear-resistant, and has good physical and chemical stability.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings required to be used in the description of the embodiments are briefly introduced below, and it is obvious that the drawings in the description below are only some embodiments of the present invention, and it is obvious for those skilled in the art that other drawings can be obtained according to the drawings without inventive labor.
Wherein the content of the first and second substances,
FIG. 1 is a surface SEM image of an untreated cotton-flax blended fabric in an example of the present invention;
FIG. 2 is a surface SEM image of a superhydrophobic anti-icing fabric prepared in an example of the invention;
FIG. 3 is a contact angle graph of a superhydrophobic anti-icing fabric according to an embodiment of the invention;
FIG. 4 is a Fourier infrared spectrum of a superhydrophobic anti-icing fabric according to an embodiment of the invention;
FIG. 5 is an atomic force microscope three-dimensional topography of a raw fabric of the present invention;
FIG. 6 is an atomic force microscope three-dimensional topography of the superhydrophobic anti-icing fabric of the embodiment;
FIG. 7 is a graph of contact angle change of a superhydrophobic anti-icing fabric after abrasion testing in an embodiment of the invention;
FIG. 8 is a graph of contact angle data for a superhydrophobic anti-icing fabric of an embodiment of the invention after extreme chemical testing;
FIG. 9 is a graph of contact angle change of a superhydrophobic anti-icing fabric of an embodiment of the invention after UV irradiation testing;
FIG. 10 is a graph of ice delay time data for a superhydrophobic anti-icing fabric according to an embodiment of the invention; wherein, the icing time of the liquid drops on the original fabric is 64s, and the icing time of the liquid drops on the super-hydrophobic anti-icing fabric is 1483s
FIG. 11 is a self-cleaning pair diagram of a superhydrophobic anti-icing fabric and a virgin fabric according to an embodiment of the invention; wherein, (a) is before washing, (b) is in washing, (c) is after washing, (d) is before washing, (e) is in washing, and (f) is after washing.
FIG. 12 is a graph of qualitative mechanical test and hydrophobic effect of a superhydrophobic anti-icing fabric according to an embodiment of the invention; wherein, (a) is brushing, (b) is scraping, (c) is peeling of 3M adhesive plaster, (d) is impact of a hammer, (e) is hydrophobic effect of the cloth after brushing, (f) is hydrophobic effect of the cloth after scraping of the knife, (g) is hydrophobic effect of the cloth after peeling of the 3M adhesive plaster, and (h) is hydrophobic effect of the cloth after impact of the hammer.
FIG. 13 is a graph of icing of a virgin fabric according to an embodiment of the present invention; wherein, one side of the fabric is wetted by liquid, and the other side of the fabric is frozen in a large area.
FIG. 14 is an icing chart of the superhydrophobic anti-icing fabric according to the embodiment of the invention; wherein, (a) one side of the fabric is not wetted by liquid, and (b) the other side of the fabric is hardly frozen.
FIG. 15 is a comparison graph of the hydrophobic effect of the original cap after the super-hydrophobic anti-icing spray of the present invention is sprayed on the cap and dried; the method comprises the steps of (a) pouring liquid into an original cap, (b) pouring liquid into the original cap, (c) pouring liquid into the original cap, (d) pouring liquid into the cap after spraying of a spray, (e) pouring liquid into the cap after spraying of the spray, and (f) pouring liquid into the cap after spraying of the spray.
FIG. 16 is a graph of the hydrophobic effect of the drops after the super-hydrophobic anti-icing spray of the invention is sprayed on various papers and fabrics and dried.
The spraying agent is sprayed on medical gauze, (b) the spraying agent is sprayed on old clothes, (c) the spraying agent is sprayed on boxboard paper, (d) the spraying agent is sprayed on cotton, and (e) the spraying agent is sprayed on printing paper. (f) Spraying the spray on cotton and linen textile, and (g) spraying the spray on toilet paper.
Detailed Description
The present invention will be described in detail below by way of examples with reference to the accompanying drawings.
The present invention is not limited to the listed embodiments, which are merely illustrative of the present invention.
The PDMS prepolymer used in the examples described below was selected from commercially available Dow Corning Sylgard 184A, and its associated curing agent was not used.
The invention adopts a plurality of letters, PDMS, sylgard 184A polydimethylsiloxane prepolymer. DGEBA bisphenol A diglycidyl ether (epoxy resin); SEM, scanning electron microscope.
The invention provides a preparation method of a high-robustness super-hydrophobic anti-icing fabric, which comprises the following steps:
step 1: preparing PDMS and bisphenol A diglycidyl ether solution:
adding PDMS and bisphenol A diglycidyl ether (bisphenol A epoxy resin) into absolute ethyl alcohol, stirring, dissolving, taking supernatant, and filtering to obtain PDMS and bisphenol A diglycidyl ether solutions, wherein the PDMS and the bisphenol A diglycidyl ether in the PDMS and bisphenol A diglycidyl ether solutions are both in a saturated state.
Step 2: preparing a dispersed nano silicon dioxide mixed solution:
adding nano silicon dioxide and 3-aminopropyl triethoxysilane into absolute ethyl alcohol, and uniformly dispersing by ultrasonic waves to obtain a nano silicon dioxide mixed solution;
wherein the mass fraction of the nano silicon dioxide in the nano silicon dioxide mixed solution is 2-4%, the mass fraction of the 3-aminopropyl triethoxysilane is 16%, and the ultrasonic dispersion time is 30min.
And step 3: preparing a super-hydrophobic anti-icing spray:
mixing saturated PDMS, bisphenol A diglycidyl ether solution and nano silicon dioxide mixed solution, and dispersing uniformly by ultrasonic waves to obtain the spray. Wherein the mass concentration of the nano silicon dioxide is 0.5-3%.
The mass concentration of the nano silicon dioxide in the spray is less than the mass fraction of the nano silicon dioxide in the nano silicon dioxide mixed solution.
The ultrasonic dispersion time is 30min;
and 4, step 4: cutting the fabric by adopting a spraying method. Firstly cutting a fabric, sequentially carrying out ultrasonic cleaning and drying on the fabric by using deionized water and absolute ethyl alcohol through an ultrasonic water bath method, then spraying the spray on the fabric by using a spray bottle, wherein the spraying distance is about 10cm, spraying is carried out for 3-5 times, and heating is carried out for 4 hours at 70 ℃ to obtain the high-robustness superhydrophobic anti-icing fabric.
The high-robustness super-hydrophobic anti-icing fabric is a fluorine-free durable super-hydrophobic anti-icing fabric with excellent mechanical and chemical stability, ultraviolet irradiation resistance and self-cleaning performance.
The spray is sprayed on paper and dried, and has strong hydrophobicity.
The PDMS prepolymer is selected from Sylgard 184 of Dow Corning, a matched curing agent is not used, and bisphenol A diglycidyl ether is used as a matrix adhesive.
The 3-aminopropyl triethoxysilane is used as the curing agent and adhesive for coating.
Example 1
The fabric is exemplified by a cotton and linen blended textile.
Firstly, preparing a solution A;
4g PDMS and 2g DGEBA in 30mL ethanol, the suspension in a magnetic stirrer at 800r/min for half an hour of stirring, so that it fully dissolved, and standing for half an hour after the solid precipitation supernatant.
Step two, preparing a solution B;
0.4g of Nano-SiO 2 (nanosilica) and 1.6g of APTES (3-aminopropyltriethoxysilane as silane coupling agent) were placed in 8g of ethanol. Then the mixture is dispersed for half an hour by ultrasonic waves to obtain uniformly dispersed nano SiO 2 And (3) mixing the solution.
Thirdly, cleaning the original textile and spraying a super-hydrophobic spray;
and (3) respectively and sequentially cleaning the surface fabric by using deionized water and ethanol ultrasonic waves, removing dust and organic matters on the surface of the fabric, and drying to obtain the clean fabric. And storing the solution A and the solution B into a spray bottle, and preparing a final mixture with the mass fraction of silicon dioxide of 1%. And finally, after the mixed solution is subjected to ultrasonic dispersion for more than half an hour, spraying the fabric for 3-5 times at a position 10cm away from the fabric, putting the fabric into a constant-temperature drying oven for 4 hours, and keeping the temperature for 70 ℃ to obtain the high-robustness super-hydrophobic anti-icing fabric, which is recorded as PEST.
The SEM image of the fiber surface of the textile used in this example is shown in fig. 1, and it can be seen that the surface is smooth.
The SEM image of the fiber surface of the superhydrophobic anti-icing fabric prepared in this example is shown in fig. 2, and it can be seen that the surface is PDMS and is a rough waxy surface with a granular feel. Coverage of the waxy surface turns the fiber into a low surface energy surface.
The contact angle of the surface of the superhydrophobic anti-icing fabric prepared in the embodiment is shown in fig. 3, and the contact angle is up to 160 degrees.
Example 2
The difference from example 1 is that only PDMS and 3-aminopropyltriethoxysilane were contained, i.e. no DGEBA was added in step 1, and the obtained highly robust superhydrophobic anti-icing fabric is noted as PT.
Example 3
Unlike example 1, which contains only epoxy resin (bisphenol a diglycidyl ether) and 3-aminopropyltriethoxysilane, i.e. no PDMS is added in step 1, the highly robust superhydrophobic anti-icing fabric obtained is noted ET.
Example 4
Unlike example 1, which contains only epoxy resin (bisphenol a diglycidyl ether) and 3-aminopropyltriethoxysilane, i.e., no nanosilica is added in step 2, the resulting highly robust superhydrophobic anti-icing fabric is noted as PET.
The fourier ir spectrum of the spray prepared in this example sprayed on PT, ET, PET or PEST surface is shown in fig. 4, and it can be seen that the peak of the spectral intensity of the coated fabric surface (PT, ET, PET or PEST) is reduced compared to BT, indicating that the coating has been coated, and the result is consistent with SEM and afm results.
In this embodiment, the roughness of the fabric fiber surface within the range of 5 μm × 5 μm is tested by using the Tapping mode of an atomic force microscope, and fig. 5 shows the three-dimensional morphology of the original fabric surface, where the visible root mean square roughness is 29.9nm, and fig. 6 shows the three-dimensional morphology of the superhydrophobic anti-icing fabric surface, where the visible root mean square roughness is 80nm. The increase in roughness causes the hydrophobicity of the surface to increase further.
In order to embody the performance of the superhydrophobic anti-icing fabric in the embodiment, quantitative tests such as abrasion, chemical erosion, ultraviolet interference and ice delay time are performed, and qualitative tests such as self-cleaning, washing resistance, tape stripping, knife scraping, impact, ice residue and the like are performed.
Quantitative test
And (3) wear testing: the superhydrophobic anti-icing fabric prepared in the embodiment has excellent wear resistance, and the contact angle change curve graph of the superhydrophobic anti-icing fabric is shown in fig. 7 when the superhydrophobic anti-icing fabric is ground by using 320-mesh sandpaper under the pressure of 2kPa, and the contact angle of the superhydrophobic anti-icing fabric is still more than 150 degrees after 1200 cycles. The super-hydrophobic anti-icing fabric has good wear resistance.
Chemical erosion: the superhydrophobic anti-icing fabric prepared in this example has excellent chemical stability, and when the superhydrophobic anti-icing fabric is respectively soaked in hot water at 80 ℃, a saturated sodium chloride solution, an ethanol solution, a hydrochloric acid solution with PH =1, and a sodium hydroxide solution with PH =13 for 48 hours, the contact angle after soaking is as shown in fig. 8, it can be seen that the contact angle after hot water soaking is still more than 140 °, and the contact angle after other solutions are soaked is still more than 150 °. The super-hydrophobic anti-icing fabric has strong chemical erosion resistance.
Ultraviolet interference: the superhydrophobic anti-icing fabric prepared in the embodiment has strong ultraviolet interference resistance, and the pattern of the change of the contact angle of the superhydrophobic anti-icing fabric along with time under the ultraviolet irradiation with the wavelength of 295nm is shown in fig. 9, so that the contact angle of the superhydrophobic anti-icing fabric is still more than 160 degrees after the superhydrophobic anti-icing fabric is irradiated for 20 hours. The super-hydrophobic anti-icing fabric is proved to have excellent anti-interference capability.
Ice delay time: the superhydrophobic anti-icing fabric prepared in the embodiment has a delayed droplet icing time, and 20 μ L of droplets are dripped on the superhydrophobic anti-icing fabric on the surface at-8 ℃ under the conditions that the indoor temperature is 24 ℃ and the humidity is 52%, as shown in (a) - (h) of fig. 10, the droplet icing time is obviously increased. The super-hydrophobic anti-icing fabric has obvious icing delaying performance.
Qualitative testing
Self-cleaning test: the superhydrophobic anti-icing fabric prepared in the embodiment has self-cleaning capability. As shown in fig. 11, 1mL of coffee is dropped on the original fabric and the superhydrophobic anti-icing fabric respectively, and washed by deionized water, it is obvious that the coffee on the superhydrophobic anti-icing fabric is easily washed off, and most of the coffee on the original fabric remains on the surface of the fabric.
Anti washing, tape stripping, knife scraping and impact testing: the superhydrophobic anti-icing fabric prepared in this example was impacted by using a toothbrush for brushing, 3M tape stripping, knife scraping, and a hammer for more than 30 times, as shown in fig. 12, it was seen that the droplets remained spherical after being dropped on the surface of the superhydrophobic anti-icing fabric. Therefore, the superhydrophobic anti-icing fabric has good mechanical stability.
Ice residue test: dropping physiological saline at a speed of 0.125mL/s on the surfaces of the original fabric and the superhydrophobic anti-icing fabric by using a peristaltic pump at a height of 20cm from the fabric, as shown in fig. 13, it can be seen that the original fabric is completely wetted and the wetted back is covered with a large amount of ice. As shown in FIG. 14, it can be seen that most of the droplets on the surface of the superhydrophobic anti-icing fabric are bounced off, a part of the droplets stay on the surface and cannot be wetted into the fabric, and only a small part of the back surface of the superhydrophobic anti-icing fabric is frozen. The super-hydrophobic anti-icing fabric surface is proved to have strong ice-thinning performance.
In order to show that the super-hydrophobic anti-icing spray has practical value, the invention is used for processing the white cap and testing the waterproof performance of the white cap.
The untreated cap and the treated white cap were each showered with 80mL of methylene blue aqueous solution, as shown in FIG. 15, it can be seen that the treated white cap had an obvious water-proof property, proving that the present invention has a very strong practical value. The super-hydrophobic anti-icing spray prepared by the method of example 1 is sprayed on medical gauze, old clothes, boxboard paper, cotton, printing paper, textile fabrics and toilet paper, as shown in (a), (b), (c), (d), (e), (f) and (g) of fig. 16, so that the surfaces of the gauze, the old clothes, the boxboard paper, the cotton, the printing paper, the textile fabrics and the toilet paper show strong hydrophobicity after being treated, namely, the liquid drops are in a bead shape.
Example 5
Firstly, preparing a solution A;
4g of PDMS and 2g of DGEBA are placed in 30mL of ethanol, the suspension is stirred on a magnetic stirrer for half an hour at 800r/min to be fully dissolved, and after standing for half an hour and solid precipitation, supernatant liquid is taken to obtain PDMS and bisphenol A diglycidyl ether solution.
Step two, preparing a solution B;
0.2g of Nano-SiO 2 (nanosilica) and 1.6g of APTES (3-aminopropyltriethoxysilane) were placed in 8.2g of ethanol. Then the mixture is dispersed for half an hour by ultrasonic waves to obtain uniformly dispersed nano SiO 2 And (3) mixing.
Thirdly, cleaning the original textile and spraying a super-hydrophobic spray;
and (3) respectively and sequentially cleaning the surface fabric by using deionized water and ethanol ultrasonic waves, removing dust and organic matters on the surface of the fabric, and drying to obtain the clean fabric. And storing the solution A and the solution B in a spray bottle, and preparing the final mixture with the mass fraction of silicon dioxide of 1%. And (3) after the final mixed solution is subjected to ultrasonic dispersion for 60min, spraying the fabric for 3 times at a position 10cm away from the fabric, and putting the fabric into a constant-temperature drying box for 4h for heat preservation at 70 ℃ to obtain the high-robustness superhydrophobic anti-icing fabric.
Example 6
Firstly, preparing a solution A;
4g of PDMS and 2g of DGEBA are placed in 30mL of ethanol, the suspension is stirred on a magnetic stirrer for half an hour at the speed of 800r/min to be fully dissolved, and after the suspension is kept still for half an hour and solid precipitates, the supernatant is taken to obtain the PDMS and bisphenol A diglycidyl ether solution.
Step two, preparing a solution B;
0.3g of Nano-SiO 2 (nanosilica) and 1.6g of APTES (3-aminopropyltriethoxysilane) were placed in 8.1g of ethanol. Then the mixture is dispersed for half an hour by ultrasonic waves to obtain uniformly dispersed nano SiO 2 And (3) mixing.
Thirdly, cleaning the original textile and spraying a super-hydrophobic spray;
and (3) respectively and sequentially cleaning the surface fabric by using deionized water and ethanol through ultrasonic waves, removing dust and organic matters on the surface of the fabric, and drying to obtain the clean fabric. And storing the solution A and the solution B in a spray bottle, and preparing the final mixture with the mass fraction of silicon dioxide of 2%. And (3) after the final mixed solution is subjected to ultrasonic dispersion for 50min, spraying the fabric for 5 times at a position 10cm away from the fabric, putting the fabric into a constant-temperature drying oven for 4h, and keeping the temperature for 70 ℃ to obtain the high-robustness superhydrophobic anti-icing fabric.
Example 7
The difference from example 6 is that in the third step, the silica mass fraction in the final mixture is 0.5%.
Example 8
The difference from example 1 is that in the third step, the mass fraction of silica in the final mixture is 3%.
The invention uses 3-aminopropyl triethoxysilane as a cross-linking agent to cross-link the epoxy resin and the polydimethylsiloxane. Because of the action of the epoxy resin and the 3-aminopropyl triethoxysilane, a firm molecular bridge is formed between the coating and the base material, and the adhesive force between the coating and the fiber is improved. Inspired by the micro-nano structure on the surface of the lotus leaf, low surface energy is formed through PDMS and modified epoxy resin, and nano silicon dioxide is introduced to construct a micro-emulsion structure on the surface of the fiber. The contact angle of the super-hydrophobic fabric is as high as 162 degrees, and the contact angle of the super-hydrophobic fabric can still be kept above 150 degrees even after the super-hydrophobic fabric is worn 1200 times by using sandpaper. In addition, the surface still exhibits excellent hydrophobicity as tested by other extreme physical and chemical environments. Also, such coatings can be easily grafted onto garments and paper by a two-step spray drying process. More importantly, the super-hydrophobic surface has obvious anti-icing and self-cleaning performances. Therefore, the high-robustness super-hydrophobic anti-icing fabric spray and the preparation method thereof have a good application scene in real life.
The invention is not limited to the fabric used in the embodiments of the invention, but is still useful on various papers and textiles.
Claims (8)
1. A preparation method of a high-robustness superhydrophobic anti-icing fabric is characterized by comprising the following steps:
adding PDMS and bisphenol A epoxy resin into absolute ethyl alcohol to obtain PDMS and bisphenol A epoxy resin solution;
adding the nano particles and 3-aminopropyltriethoxysilane into absolute ethanol, and uniformly dispersing to obtain a nano silicon dioxide mixed solution;
mixing PDMS, bisphenol A epoxy resin solution and nano-silica mixed solution, and dispersing the mixture uniformly by ultrasonic waves to obtain a spray; and spraying the spray on the fabric, and drying to obtain the high-robustness super-hydrophobic anti-icing fabric.
2. The method for preparing the highly robust superhydrophobic anti-icing fabric according to claim 1, wherein the bisphenol A epoxy resin is bisphenol A diglycidyl ether.
3. The method of claim 1, wherein the PDMS and the bisphenol A epoxy resin are saturated in the PDMS and bisphenol A epoxy resin solution.
4. The method for preparing the highly robust superhydrophobic anti-icing fabric according to claim 1, wherein the nanoparticles are nanosilica.
5. The method for preparing the highly robust superhydrophobic anti-icing fabric according to claim 1, wherein the mass fraction of the nano-silica in the nano-silica mixed solution is 2-4%.
6. The method for preparing the highly robust superhydrophobic anti-icing fabric according to claim 1, wherein the mass fraction of 3-aminopropyltriethoxysilane is 16%.
7. The preparation method of the highly robust superhydrophobic anti-icing fabric according to claim 1, wherein the mass concentration of the nano-silica in the spray is 0.5-3%.
8. The method for preparing the highly robust superhydrophobic anti-icing fabric according to claim 1, wherein the ultrasonic dispersion time is 30-60 min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211517997.9A CN115787306A (en) | 2022-11-29 | 2022-11-29 | Preparation method of high-robustness super-hydrophobic anti-icing fabric |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211517997.9A CN115787306A (en) | 2022-11-29 | 2022-11-29 | Preparation method of high-robustness super-hydrophobic anti-icing fabric |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN115787306A true CN115787306A (en) | 2023-03-14 |
Family
ID=85443572
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202211517997.9A Pending CN115787306A (en) | 2022-11-29 | 2022-11-29 | Preparation method of high-robustness super-hydrophobic anti-icing fabric |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN115787306A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116855174A (en) * | 2023-07-21 | 2023-10-10 | 齐鲁工业大学(山东省科学院) | Anti-icing lignin super-hydrophobic coating and preparation method and application thereof |
Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106380945A (en) * | 2016-10-27 | 2017-02-08 | 重庆大学 | Anti-pollution-flashover superhydrophobic paint, and preparation method and application thereof |
| CN106883650A (en) * | 2017-04-21 | 2017-06-23 | 黑龙江凯恩琪新材料科技有限公司 | It is a kind of can the lasting super-hydrophobic coat of freezing preparation method |
| US20190233675A1 (en) * | 2016-10-18 | 2019-08-01 | Siemens Gamesa Renewable Energy Innovation &Technology, S.L. | Polymeric composition with anti-icing and self-cleaning properties |
| CN111299104A (en) * | 2020-03-17 | 2020-06-19 | 陕西科技大学 | Super-hydrophobic composite coating and preparation method thereof |
| CN112210272A (en) * | 2020-10-08 | 2021-01-12 | 苏州大学 | Wear-resistant super-hydrophobic composite material and preparation method thereof |
| CN112852289A (en) * | 2021-01-12 | 2021-05-28 | 陕西科技大学 | Super-hydrophobic anti-icing and deicing coating with photo-thermal effect and preparation method thereof |
| CN113293607A (en) * | 2021-05-31 | 2021-08-24 | 方俊 | Super-hydrophobic polyester fabric and preparation method thereof |
| CN113980576A (en) * | 2021-12-02 | 2022-01-28 | 大连理工大学 | Preparation method of anti-icing durable super-hydrophobic coating |
| CN114713479A (en) * | 2022-04-14 | 2022-07-08 | 扬州大学 | Liquid material spraying improvement EP + PDMS/SiO through laser curing2Method for durability of super-hydrophobic coating |
| CN114752275A (en) * | 2022-03-07 | 2022-07-15 | 吉林大学 | Preparation method of bionic super-hydrophobic coating capable of being sprayed on various substrates |
-
2022
- 2022-11-29 CN CN202211517997.9A patent/CN115787306A/en active Pending
Patent Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20190233675A1 (en) * | 2016-10-18 | 2019-08-01 | Siemens Gamesa Renewable Energy Innovation &Technology, S.L. | Polymeric composition with anti-icing and self-cleaning properties |
| CN106380945A (en) * | 2016-10-27 | 2017-02-08 | 重庆大学 | Anti-pollution-flashover superhydrophobic paint, and preparation method and application thereof |
| CN106883650A (en) * | 2017-04-21 | 2017-06-23 | 黑龙江凯恩琪新材料科技有限公司 | It is a kind of can the lasting super-hydrophobic coat of freezing preparation method |
| CN111299104A (en) * | 2020-03-17 | 2020-06-19 | 陕西科技大学 | Super-hydrophobic composite coating and preparation method thereof |
| CN112210272A (en) * | 2020-10-08 | 2021-01-12 | 苏州大学 | Wear-resistant super-hydrophobic composite material and preparation method thereof |
| CN112852289A (en) * | 2021-01-12 | 2021-05-28 | 陕西科技大学 | Super-hydrophobic anti-icing and deicing coating with photo-thermal effect and preparation method thereof |
| CN113293607A (en) * | 2021-05-31 | 2021-08-24 | 方俊 | Super-hydrophobic polyester fabric and preparation method thereof |
| CN113980576A (en) * | 2021-12-02 | 2022-01-28 | 大连理工大学 | Preparation method of anti-icing durable super-hydrophobic coating |
| CN114752275A (en) * | 2022-03-07 | 2022-07-15 | 吉林大学 | Preparation method of bionic super-hydrophobic coating capable of being sprayed on various substrates |
| CN114713479A (en) * | 2022-04-14 | 2022-07-08 | 扬州大学 | Liquid material spraying improvement EP + PDMS/SiO through laser curing2Method for durability of super-hydrophobic coating |
Non-Patent Citations (2)
| Title |
|---|
| 李战胜;: "基于纳米二氧化硅的防冰疏水涂层的制备及性能研究", 电镀与涂饰, no. 04, pages 201 - 205 * |
| 李超逸 等: "配电网线路防结冰涂层构筑及其性能评价", 中国表面工程, vol. 34, no. 3, pages 66 - 73 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116855174A (en) * | 2023-07-21 | 2023-10-10 | 齐鲁工业大学(山东省科学院) | Anti-icing lignin super-hydrophobic coating and preparation method and application thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Xue et al. | Fabrication of superhydrophobic cotton fabrics by grafting of POSS-based polymers on fibers | |
| Yu et al. | SiO2 nanoparticle-based superhydrophobic spray and multi-functional surfaces by a facile and scalable method | |
| Qiang et al. | Robust UV-cured superhydrophobic cotton fabric surfaces with self-healing ability | |
| Luo et al. | Robust and durable fluorinated 8-MAPOSS-based superamphiphobic fabrics with buoyancy boost and drag reduction | |
| CN104449357A (en) | Transparent super-hydrophobic coating material and method for preparing transparent super-hydrophobic coating by transparent super-hydrophobic coating material | |
| Li et al. | Durable superhydrophobic and oleophobic cotton fabric based on the grafting of fluorinated POSS through silane coupling and thiol-ene click reaction | |
| EP1802721A1 (en) | Hydrophobic and lyophobic coating | |
| WO2016115980A1 (en) | Method for constructing surface of fabric with ultraviolet protection and wash-resistant special wetting functions | |
| Kong et al. | Robust fluorine-free superhydrophobic coating on polyester fabrics by spraying commercial adhesive and hydrophobic fumed SiO2 nanoparticles | |
| CN115787306A (en) | Preparation method of high-robustness super-hydrophobic anti-icing fabric | |
| CN111270514B (en) | Preparation method of stable superhydrophobic antibacterial cotton fabric based on glutaraldehyde crosslinking | |
| Tian et al. | Efficient scald-preventing enabled by robust polyester fabrics with hot water repellency and water impalement resistance | |
| CN105152546A (en) | Transparent antifouling coating material used for glass, and transparent antifouling coating and preparation method thereof | |
| Xing et al. | Universal fabrication of superhydrophobic and UV resistant cotton fabric with polyphenols | |
| CN108822712A (en) | A kind of super-hydrophilic coating agent and preparation method thereof | |
| Lu et al. | Superhydrophobic wood fabricated by epoxy/Cu2 (OH) 3Cl NPs/stearic acid with performance of desirable self-cleaning, anti-mold, dimensional stability, mechanical and chemical durability | |
| CN109322144A (en) | A kind of durability super-hydrophobic textile finishing agent and its method for sorting | |
| CN108676482B (en) | Self-repairing coating and preparation method thereof | |
| Li et al. | Development of high performance superhydrophobic coating with excellent corrosion resistance, durability, and self-cleaning properties using M-TiO2@ EP composites | |
| CN110396308A (en) | A kind of preparation method of ice-covering-proof coatings | |
| Xie et al. | Novel fabrication of robust superhydrophobic polyester fabric with eugenol based on thiol-ene click chemistry for self-cleaning and water–oil separation | |
| Li et al. | Durable, self-cleaning and anti-fouling superhydrophobic coating based on double epoxy layer | |
| Zheng et al. | Heating repairable superamphiphobic coatings for long-lasting antifouling application | |
| DE102006030055A1 (en) | Process for the preparation of a removable, anti-fouling coating | |
| CN107201173A (en) | It is a kind of to can be applied to south of the Five Ridges area iron cultural relic anticorrosion organic/inorganic composite material of high-temperature high humidity climate and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |