CN104610875A - Super-hydrophilic and underwater super-oleophobic coating, as well as preparation method and application thereof - Google Patents
Super-hydrophilic and underwater super-oleophobic coating, as well as preparation method and application thereof Download PDFInfo
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Abstract
The invention relates to a super-hydrophilic and underwater super-oleophobic coating, as well as a preparation method and application thereof. According to the invention, an organic/inorganic hybrid sol preparation method and a surface coating method are adopted, an organic/inorganic hybrid coating containing zwitter-ion groups with a certain thickness is constructed on the material surface, and is prepared through mixing alkoxy silane functionalized glycine betaine type zwitter-ion compound and silicon dioxide particles with other auxiliaries and performing hydrolysis, coating and thermal treatment. The functional coating provided by the invention is super-hydrophilic in air and super-oleophobic underwater; as the glycine betaine type zwitter-ion compound simulating the cell outer membrane molecular structure is introduced in the prepared super-hydrophilic underwater super-oleophobic coating, the prepared functional coating has the self-cleaning function, the antifogging function, the underwater oil resistance function, and the like, and has excellent bioadhesive resistance; the coating, the method and the application thereof have the advantages that the technology is simple, raw materials are easy to obtain, the equipment is simple, the cost is low, and the coating can be large-area prepared.
Description
Technical field
The invention belongs to nano-material surface preparing technical field, particularly there is special wetting property surface, namely there is super hydrophilic and super oleophobic coating and its production and use under water.
Background technology
Surface wettability is one of key character of solid surface, jointly determines primarily of surface chemistry and surface micro-structure.By surface chemistry composition and the regulation and control of microstructure, dissimilar special wetting property can be formed at body surface surperficial, comprise super-hydrophobic, Superhydrophilic, super oleophobic and super-oleophilic etc., have a wide range of applications in daily life and industrial production.Such as super hydrophobic surface has the self_cleaning effect of similar lotus leaf, can be used for anti-freeze, waterproof and antifouling etc.; Super water wetted material can make small droplets pave rapidly, namely little water droplet contact angle on the glass surface levels off to zero degree, forms uniform moisture film, would not affect mirror image and light transmission like this, and take away spot by the gravity fall of uniform water film, reach automatically cleaning effect; Super oleophobic surface in water surrounding, because oil droplet can not at its surface spreading, make to surpass oleophobic surface under water at boats and ships, oceanographic equipment antifouling coating, in body, the field such as antibiont pasting material and oily water separation is with a wide range of applications.
By this special sexual enlightenment of anticoagulation of membrane surface, betaine type amphoteric ionic compound like people's Design and synthesis hydrophilic radical and phospholipid, as Phosphorylcholine (PC), sulphonic acid betaine (SB) and carboxylic acid trimethyl-glycine (CB), research shows, this kind of zwitterionic compound can form strong hydrophilicity surface by the hydration Bound Water Molecules of electrostatic induction, and the water molecules of intimate surface absorption imparts the characteristic that the oleophobic property of material surface and antibiont stick.In recent years, the research of the wetting ability biomimetic material based on the betaine type amphoteric ionic compound of imitating cell outer-layer membrane molecule structure obtains great concern.The zwitterionic monomer that Design and synthesis is novel or compound, explore simple, feasible, effective surface modifying method, constructing zwitterionic compound layer securely on different substrate materials surface is the important channel that the novel oleophobic surface under water of preparation and bionical antibiont stick surface.
Disclose the oil-water separating net adopting the preparation of various different methods to have super oleophobic properties under water in Chinese patent CN102029079B, CN102716676A, CN103100239A and CN103111096A, but all do not relate to the preparation aspect of flat surface coating; Chinese patent CN 101704955B openly adopts self-assembling technique and heterogeneous nucleation technology, with chitosan and silicon-dioxide for rough surface structure constructed by raw material, obtain the material surface with super oleophobic under water, but the preparation process of this material is comparatively loaded down with trivial details.In addition, (Wu Yalu on the basis of previous work, Li Guangji, Liu Yunhong, Deng. the preparation of zwitter-ion self-assembly bionic surface, characterize and anti-Adhesion property [J]. SCI, 2014:1484-1491.), design and synthesized a kind of zwitterionic compound of sulphonic acid betaine type, and by self-assembling technique, compound is constructed at glass substrate surface, the bionic surface of analog cell outer membrane, prepared bionic surface has excellent anti-fog properties and antibacterium Adhesion property, but the technical process on this molecular self-assembling method preparation surface is comparatively loaded down with trivial details, and rete is thin, less stable.In order to improve the stability of surface property, bionical zwitterionic materials can be built into certain thickness coating, certain actual application value can be had.
Summary of the invention
The present invention aims to provide one and has super hydrophilic and super oleophobic coating under water, and provide that a kind of technical process is simple, low cost there is super hydrophilic and super oleophobic and have the preparation method of multi-functional coatings and the purposes of antibiont adhesion characteristics under water.
For solving above-mentioned purpose, the present inventor have employed following technical scheme:
Adopt the method for hybrid colloidal sol preparation method and surface self-organization coating, construct the certain thickness hybrid coating containing zwitter-ion group at material surface, by functionalized with alkoxysilane betaine type amphoteric ionic compound, silicon dioxide granule and other auxiliary agents, mixed merga pass hydrolysis, self-assembly coating and thermal treatment are prepared from described hybrid coating mutually.
Through repetition test, finally confirm following preparation method:
1, under room temperature, be dissolved in alcoholic solvent, be configured to the solution of 0.1 ~ 30.0 wt% by functionalized with alkoxysilane betaine type amphoteric ionic compound, with hydrochloric acid soln regulator solution pH to 2 ~ 7 of 0.01 ~ 0.5 M, hydrolysis ageing 1 ~ 8 h, obtains solution A;
2, joining in alcoholic solvent by the nano silicon being of a size of 5nm ~ 300nm, obtain the solution that concentration is 0.1 ~ 20 wt%, is B solution;
3, under room temperature, solution A, B solution, thinner, water and adhesive aid mixed and stirs, obtaining mixing solutions; Wherein, the content of the solution A in mixing solutions is 10.0 ~ 90.0wt%, the content of B solution is 0 ~ 80 wt%, the content of thinner is 0 ~ 50.0wt%, the content of water is 0.1 ~ 10.0wt%, the content of adhesive aid is 0 ~ 20.0wt%.
4, substrate surface is cleaned up, dry under normal temperature;
5, adopt self-assembly coating method, mixing solutions film step 3 obtained, at substrate surface, processes 1 ~ 100min under 20 DEG C ~ 160 DEG C conditions, obtains super hydrophilic and super oleophobic coating under water.
At least one in the group that described alcoholic solvent is selected from methyl alcohol, ethanol, propyl carbinol, Virahol form;
Described thinner is selected from least one in the group that methyl alcohol, ethanol, propyl carbinol, Virahol, acetone, ethyl acetate, normal hexane, methylethylketone, tetrahydrofuran (THF), toluene and dimethylbenzene forms;
Described adhesive aid is selected from tetraethoxy, methyl silicate, aminopropyl triethoxysilane, 1, at least one in the group that the two silica-based ethane of triethoxy of 2-, 1,2-two silica-based ethane of trimethoxy, two-(γ-triethoxysilylpropyl) – tetrasulfide form;
Coating method described in step (5) comprises dip coating, spread coating or spraying method.
Described functionalized with alkoxysilane betaine type amphoteric ionic compound, is characterized in that the structural formula of this compound is:
Wherein R
1and R
2for H or the alkyl containing 1 ~ 3 carbon atom, a is 0,1,2 or 3; R
3for-NHCOO-or
—NHCONH(CH
2)—；
The described super thickness that is hydrophilic and super oleophobic coating under water that has can be controlled in 500nm ~ 100 μm.
Described have super hydrophilic and under water super oleophobic coating in atmosphere to the contact angle of water close to 0 °;
Described described have super hydrophilic and under water super oleophobic coating under water 150 ° are greater than to the contact angle of oil droplet;
Described oil droplet is any one in methylene dichloride, trichloromethane, tetracol phenixin, ethylene dichloride, n-Hexadecane, octane, whiteruss.
Of the present invention have super hydrophilic and under water super oleophobic coating and preparation method thereof advantage be:
1, method technique of the present invention is simple, raw material is easy to get, equipment is simple, with low cost, functional coating can be prepared in different substrate materials surface big area, reach super hydrophilic and super oleophobic property under water;
2, prepared super hydrophilic and introduce the betaine type amphoteric ionic compound of imitating cell outer-layer membrane molecule structure under water in super oleophobic coating, make the functional coating prepared not only have automatically cleaning, the antifog and effect such as oil-stain-preventing under water, there is the performances such as excellent antibiont adhesion simultaneously.
Accompanying drawing explanation
The present invention has accompanying drawing 6 width:
Fig. 1 is embodiment 1 coatingsurface three-dimensional microstructures atomic force microscope figure;
Fig. 2 be embodiment 1 coatingsurface in atmosphere with the contact angle figure of water;
Fig. 3 be embodiment 1 coatingsurface under water with the contact angle figure of oil droplet;
Fig. 4 is the bacterial adhesion design sketch of embodiment 1 empty glass surface;
Fig. 5 is the bacterial adhesion design sketch of embodiment 1 coatingsurface;
Fig. 6 is embodiment 2 coatingsurface three-dimensional microstructures atomic force microscope figure.
embodiment:
Below in conjunction with embodiment, technical scheme of the present invention is described further.
Embodiment 1:
(1), under room temperature, 5.0g functionalized with alkoxysilane betaine type amphoteric ionic compound is dissolved in 95.0g ethanol, with the hydrochloric acid soln regulator solution pH to 2 of 0.1M, hydrolysis ageing 4 hours, obtains solution A;
(2) nano silicon 5.0g being of a size of 50nm joins in 95.0g methanol solvate, obtains B solution;
(3), under room temperature, 10.0gA solution, 2.0gB solution, 0.2g Virahol, 0.1g water and 2g tetraethoxy are mixed and stir, obtains mixing solutions;
(4) glass surface is cleaned up, dry under normal temperature;
(5) adopt spraying method, by the mixing solutions film of step (3) at clean glass surface, process 30min under being placed in 80 DEG C of conditions, obtain super hydrophilic and super oleophobic coating under water, the three-dimensional microstructures of coatingsurface as shown in Figure 1.
Prepared coat-thickness is 10 μm, and surface is 1 ° with the contact angle of water in atmosphere, as shown in Figure 2; It is 175 ° with the contact angle of n-Hexadecane under water, as shown in Figure 3.
The functionalized with alkoxysilane betaine type amphoteric ionic compound structure adopted is as shown below,
Configuration concentration is streptococcus aureus (the S. aureus of 1 × 109 CFU/L, ATCC 29213) bacteria suspension, above-mentioned coated material surface through ultraviolet-ray sterilizing is placed in the container of bacteria suspension and the 200 ml sterile vegetative meat soups that the above-mentioned preparation of 2 ml is housed, 24 h are cultivated under 37 ° of C, take out sample, rinse 3 times with aseptic phosphate buffer solution, remove the bacterium that specimen surface does not stick.Then sample is slightly heated on flame, fix bacterium, and to dye 1 min with Viola crystallina dye liquor, use thin running water, dry under 37 ° of C.Adopt the bacterial adhesion situation of microscopic examination material surface, use lens,oil immersion during observation, a slide glass on first fixing in coupons, directly drips cedar oil on slide glass, is then immersed in cedar oil by oily lens head, carry out observing and gathering photo.Accompanying drawing 4 is the adhesion situation of blank glass sheet surface bacteria, and accompanying drawing 5 is for being coated with the adhesion situation of the bacterium of above-mentioned functions coatingsurface.
Embodiment 2:
(1), under room temperature, 5.0g functionalized with alkoxysilane betaine type amphoteric ionic compound is dissolved in 450.0g methyl alcohol, with the hydrochloric acid soln regulator solution pH to 5 of 0.1M, hydrolysis ageing 1 hour, obtains solution A;
(2) nano silicon 5.0g being of a size of 100nm joins in 450.0g alcohol solvent, obtains B solution;
(3), under room temperature, 50.0gA solution, 1.0gB solution, 0.2 propyl carbinol, 0.1g water are mixed and stirs, obtains mixing solutions;
(4) glass surface is cleaned up, dry under normal temperature;
(5) adopt showering mode, by the mixing solutions film of step (3) at clean glass surface, process 100min under being placed in 160 DEG C of conditions, obtain super hydrophilic and super oleophobic coating under water, the three-dimensional microstructures of coatingsurface as shown in Figure 6.
Prepared coat-thickness is 100 μm, and surface is 2 ° with the contact angle of water in atmosphere; It is 160 ° with the contact angle of whiteruss under water.
The functionalized with alkoxysilane betaine type amphoteric ionic compound structure adopted is:
Embodiment 3:
(1), under room temperature, 20.0g functionalized with alkoxysilane betaine type amphoteric ionic compound is dissolved in 95.0g methyl alcohol, with the hydrochloric acid soln regulator solution pH to 7 of 0.1M, hydrolysis ageing 5 hours, obtains solution A;
(2) nano silicon 5.0g being of a size of 50nm joins in 145.0g isopropanol solvent, obtains B solution;
(3) under room temperature, by 10.0gA solution, 20.0gB solution, 10.0g water and 2g methyl silicate mix and stir, and obtains mixing solutions;
(4) glass surface is cleaned up, dry under normal temperature;
(5) adopt spraying method, by the mixing solutions film of step (3) at clean glass surface, under being placed in 120 DEG C of conditions, process 30min, obtain super hydrophilic and super oleophobic coating under water.
Prepared coat-thickness is 50 μm, and surface is 3 ° with the contact angle of water in atmosphere; It is 150 ° with the contact angle of n-Hexadecane under water.
The functionalized with alkoxysilane betaine type amphoteric ionic compound structure adopted is:
Embodiment 4:
(1), under room temperature, 15.0g functionalized with alkoxysilane betaine type amphoteric ionic compound is dissolved in 95.0g ethanol, with the hydrochloric acid soln regulator solution pH to 5 of 0.1M, hydrolysis ageing 4 hours, obtains solution A;
(2) nano silicon 15.0g being of a size of 50nm joins in 95.0g methanol solvate, obtains B solution;
(3), under room temperature, two to 10.0gA solution, 8.0gB solution, 5 Virahols, 0.8g water and 3.5g1,2-silica-based ethane of trimethoxy is mixed and stirs, obtains mixing solutions;
(4) glass surface is cleaned up, dry under normal temperature;
(5) adopt spin coating mode, by the mixing solutions film of step (3) at clean glass surface, under being placed in 90 DEG C of conditions, process 90min, obtain super hydrophilic and super oleophobic coating under water.
Prepared coat-thickness is 500nm, and surface is 1 ° with the contact angle of water in atmosphere; It is 175 ° with the contact angle of trichloromethane under water.
The functionalized with alkoxysilane betaine type amphoteric ionic compound structure adopted is:
Embodiment 5:
(1), under room temperature, 5.0g functionalized with alkoxysilane betaine type amphoteric ionic compound is dissolved in 95.0g ethanol, with the hydrochloric acid soln regulator solution pH to 5 of 0.05M, hydrolysis ageing 3.5 hours, obtains solution A;
(2) nano silicon 5.0g being of a size of 80nm joins in 95.0g alcohol solvent, obtains B solution;
(3), under room temperature, 10.0gA solution, 2.0gB solution, 0.5 ethyl acetate, 0.1g water and 2g1 aminopropyl triethoxysilane are mixed and stir, obtains mixing solutions;
(4) glass surface is cleaned up, dry under normal temperature;
(5) adopt dip coating manner, by the mixing solutions film of step (3) at clean glass surface, under being placed in 1250 DEG C of conditions, process 10min, obtain super hydrophilic and super oleophobic coating under water.
Prepared coat-thickness is 5 μm, and surface is 5 ° with the contact angle of water in atmosphere; It is 160 ° with the contact angle of octane under water.
The functionalized with alkoxysilane betaine type amphoteric ionic compound structure adopted is:
Embodiment 6:
(1), under room temperature, 15.0g functionalized with alkoxysilane betaine type amphoteric ionic compound is dissolved in 95.0g ethanol, with the hydrochloric acid soln regulator solution pH to 5 of 0.5M, hydrolysis ageing 8 hours, obtains solution A;
(2) nano silicon 0.8g being of a size of 300nm joins in 95.0g n-butanol solvent, obtains B solution;
(3) under room temperature, by two to 10.0gA solution, 2.0gB solution, 20.0g Virahol, 10.0g water and 2g-(γ-triethoxysilylpropyl) – tetrasulfide mixes and stirs, and obtains mixing solutions;
(4) glass surface is cleaned up, dry under normal temperature;
(5) adopt spraying method, by the mixing solutions film of step (3) at clean glass surface, under being placed in 145 DEG C of conditions, process 100min, obtain super hydrophilic and super oleophobic coating under water.
Prepared coat-thickness is 100 μm, and surface is 5 ° with the contact angle of water in atmosphere; It is 160 ° with the contact angle of methylene dichloride under water.
The functionalized with alkoxysilane betaine type amphoteric ionic compound structure adopted is:
Claims (5)
1. one kind has super hydrophilic and super oleophobic coating under water, it is characterized in that: described have super hydrophilic and under water super oleophobic coating be, in substrate surface self-assembly coating, there is the certain thickness hybrid coating containing zwitter-ion group, by functionalized with alkoxysilane betaine type amphoteric ionic compound, silicon dioxide granule and other auxiliary agents, mixed merga pass is hydrolyzed described hybrid coating mutually, self-assembly coating and thermal treatment is prepared from;
Described functionalized with alkoxysilane betaine type amphoteric ionic compound, is characterized in that the structural formula of this compound is:
Wherein R
1and R
2for H or the alkyl containing 1 ~ 3 carbon atom, a is 0,1,2 or 3; R
3for-NHCOO-or
—NHCONH(CH
2)—；
Described nano silicon is hydrophilic nano silicon dioxide granule;
Described base material is glass, marble, ceramic tile, metal, plastics and rubber etc.
2. according to claim 1 have super hydrophilic and super oleophobic coating under water, it is characterized in that: described have super hydrophilic and under water super oleophobic coating in atmosphere to the contact angle of water close to 0 °; Described have super hydrophilic and under water super oleophobic coating under water 150 ° are greater than to the contact angle of oil droplet; Described oil droplet is any one in methylene dichloride, trichloromethane, tetracol phenixin, ethylene dichloride, n-Hexadecane, octane, whiteruss.
3. according to claim 1 have super hydrophilic and super oleophobic coating under water, it is characterized in that: described to have super thickness that is hydrophilic and super oleophobic coating under water be 500nm ~ 100 μm.
4. according to claim 1 ~ 3 any one, have a super preparation method that is hydrophilic and super oleophobic coating under water, it is characterized in that, the method comprises the following steps:
(1) under room temperature, functionalized with alkoxysilane betaine type amphoteric ionic compound is dissolved in alcoholic solvent, is configured to the solution of 0.1 ~ 30.0 wt%, with hydrochloric acid soln regulator solution pH to 2 ~ 7 of 0.01 ~ 0.5 M; Hydrolysis ageing 1 ~ 8 h, obtains solution A;
(2) nano silicon being of a size of 5nm ~ 300nm is joined in alcoholic solvent, obtain the solution that concentration is 0.1 ~ 20 wt%, obtain B solution;
(3), under room temperature, solution A, B solution, thinner, water and adhesive aid mixed and stirs, obtaining mixing solutions; Wherein, the content of the solution A in mixing solutions is 10.0 ~ 90.0wt%, the content of B solution is 0 ~ 80 wt%, the content of thinner is 0 ~ 50.0wt%, the content of water is 0.1 ~ 10.0wt%, the content of adhesive aid is 0 ~ 20.0wt%;
(4) substrate surface is cleaned up, dry under normal temperature;
(5) adopt self-assembly coating method, mixing solutions film step (3) obtained, at substrate surface, processes 1 ~ 100min under 20 DEG C ~ 160 DEG C conditions, obtains super hydrophilic and super oleophobic coating under water;
At least one in the group that described alcoholic solvent is selected from methyl alcohol, ethanol, propyl carbinol, Virahol form;
Described thinner is selected from least one in the group that methyl alcohol, ethanol, propyl carbinol, Virahol, acetone, ethyl acetate, normal hexane, methylethylketone, tetrahydrofuran (THF), toluene and dimethylbenzene forms;
Described adhesive aid is selected from tetraethoxy, methyl silicate, aminopropyl triethoxysilane, 1, at least one in the group that the two silica-based ethane of triethoxy of 2-, 1,2-two silica-based ethane of trimethoxy, two-(γ-triethoxysilylpropyl) – tetrasulfide form;
Coating method described in step (5) comprises dip coating, spread coating or spraying method.
5. a kind of according to claim 1 ~ 4 any one has a super purposes that is hydrophilic and super oleophobic coating under water, it is characterized in that: described have super hydrophilic and under water super oleophobic coating realize the effects such as automatically cleaning, antifog, antibiont adhesion for various material surface.
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| CN105641973A (en) * | 2016-01-25 | 2016-06-08 | 四川大学 | Preparation method of nano-structure oil-water separation net membrane with self-cleaning and underwater super-oleophobic characteristics |
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| CN105641973A (en) * | 2016-01-25 | 2016-06-08 | 四川大学 | Preparation method of nano-structure oil-water separation net membrane with self-cleaning and underwater super-oleophobic characteristics |
| CN105797592B (en) * | 2016-04-18 | 2019-08-02 | 江苏大学 | A kind of Preparation method and use of super hydrophilic-underwater superoleophobic stainless steel cloth |
| CN105797592A (en) * | 2016-04-18 | 2016-07-27 | 江苏大学 | Preparation method and application of superhydrophilic and underwater superoleophobic stainless steel screen |
| CN106634275A (en) * | 2016-12-15 | 2017-05-10 | 复旦大学 | Superhydrophilic/underwater superoleophobic coating material and preparation method thereof |
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| CN109487234A (en) * | 2018-12-18 | 2019-03-19 | 湖北大学 | Super oleophobic coating and its preparation method and application |
| CN110484121A (en) * | 2019-08-27 | 2019-11-22 | 广州大学 | A kind of superoleophobic coating and the preparation method and application thereof under water |
| CN110484121B (en) * | 2019-08-27 | 2021-04-02 | 广州大学 | Underwater super-oleophobic coating and preparation method and application thereof |
| CN115667453A (en) * | 2020-05-29 | 2023-01-31 | 日涂表面处理化工有限公司 | Hydrophilizing agent |
| CN112982030A (en) * | 2021-02-04 | 2021-06-18 | 西安理工大学 | Preparation method of super-hydrophilic/underwater super-oleophobic filter paper |
| CN115463453A (en) * | 2022-09-08 | 2022-12-13 | 同济大学 | Fluorine-free hydrophilic oleophobic particle for oily sewage and preparation method and application thereof |
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