CN101608109B - Low-temperature preparation method of super-hydrophobicity film surface - Google Patents
Low-temperature preparation method of super-hydrophobicity film surface Download PDFInfo
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- CN101608109B CN101608109B CN 200910040508 CN200910040508A CN101608109B CN 101608109 B CN101608109 B CN 101608109B CN 200910040508 CN200910040508 CN 200910040508 CN 200910040508 A CN200910040508 A CN 200910040508A CN 101608109 B CN101608109 B CN 101608109B
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- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 239000000463 material Substances 0.000 claims abstract description 25
- 238000000034 method Methods 0.000 claims abstract description 16
- 230000002209 hydrophobic effect Effects 0.000 claims abstract description 11
- 150000001875 compounds Chemical class 0.000 claims abstract description 7
- 125000000217 alkyl group Chemical group 0.000 claims abstract description 5
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 claims abstract description 5
- 238000004140 cleaning Methods 0.000 claims abstract description 4
- 238000002309 gasification Methods 0.000 claims abstract description 3
- 239000000758 substrate Substances 0.000 claims description 11
- 230000004913 activation Effects 0.000 claims description 7
- 230000035484 reaction time Effects 0.000 claims description 7
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 6
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical group CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 claims description 4
- RSKGMYDENCAJEN-UHFFFAOYSA-N hexadecyl(trimethoxy)silane Chemical compound CCCCCCCCCCCCCCCC[Si](OC)(OC)OC RSKGMYDENCAJEN-UHFFFAOYSA-N 0.000 claims description 3
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 claims description 2
- 229910052809 inorganic oxide Inorganic materials 0.000 claims description 2
- 235000006408 oxalic acid Nutrition 0.000 claims description 2
- 229940095064 tartrate Drugs 0.000 claims description 2
- 239000011368 organic material Substances 0.000 claims 1
- 239000000835 fiber Substances 0.000 abstract description 5
- 238000009423 ventilation Methods 0.000 abstract description 3
- 238000010924 continuous production Methods 0.000 abstract description 2
- 239000003054 catalyst Substances 0.000 abstract 3
- 238000000889 atomisation Methods 0.000 abstract 1
- 238000006243 chemical reaction Methods 0.000 description 6
- 230000003075 superhydrophobic effect Effects 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 4
- 238000000967 suction filtration Methods 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 239000002253 acid Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- 239000000376 reactant Substances 0.000 description 3
- -1 synthon Polymers 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 230000002378 acidificating effect Effects 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 238000005234 chemical deposition Methods 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 239000002932 luster Substances 0.000 description 2
- 235000019476 oil-water mixture Nutrition 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000002028 Biomass Substances 0.000 description 1
- 229920000742 Cotton Polymers 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 1
- 241001122767 Theaceae Species 0.000 description 1
- 125000001931 aliphatic group Chemical group 0.000 description 1
- 239000003125 aqueous solvent Substances 0.000 description 1
- 235000013353 coffee beverage Nutrition 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 150000007520 diprotic acids Chemical class 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 238000010574 gas phase reaction Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229920001600 hydrophobic polymer Polymers 0.000 description 1
- 230000002706 hydrostatic effect Effects 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- 230000008595 infiltration Effects 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 235000011149 sulphuric acid Nutrition 0.000 description 1
- 239000001117 sulphuric acid Substances 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
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- Paints Or Removers (AREA)
Abstract
The invention relates to a low-temperature preparation method of a super-hydrophobicity film surface, comprising the following steps: cleaning and actively processing a base material surface by ultraviolet light in humidity of 10 percent to 60 percent at the temperature of 10 DEG C to 25 DEG C; putting the activated base material in an atomized catalyst environment so as to adsorb the catalyst on the base material; and putting the base material which adsorbs the catalyst into a gasification or atomization state of a siloxane molecular compound with hydrophobic alkyl to react at the temperature of 10 DEG C to 80 DEG C. The base material surface treated by the low-temperature preparation method has good hydrophobicity, can reach above 100 DEG C generally and can reach 160 DEG C ultimately, a processing process has low temperature, different base material surfaces can achieve hydrophobization at lower temperature, the color of the treated base material surface is not obviously changed, and the treated fiber base material can maintain ventilation property. The low-temperature preparation method of a super-hydrophobicity film surface has simple operation and can be used for industrial continuous production.
Description
Technical field
The present invention relates under a kind of lower temperature condition the super hydrophobic surface preparation method.
Background technology
The super hydrophobic surface material has very wide application prospect, but the preparation of super hydrophobic surface, and the reaction of need heating has usually limited its application.The papery of for example using in our life; Materials such as biomass fiber are the ep-type materials of reproducible utilization; But because of its surface is by the molecular composition that contains hydrophilic chemical functional group; It does not have water tolerance not have resistance to crocking yet, and owing to heatproof not is difficult to prepare super-hydrophobicization surface.The wet-strong paper that is widely used now, hydrophobic polymer material are the synthetic products; Because the problems such as Carbon emission that burning disposal was produced after the minimizing of petrochemical material was used with this type paper, synthetic materials are considered to be non-environmental protection; In addition, the problem in environmental protection, also there are airtight, non-infiltration and the lower problem of hydrophobicity.Use nanotechnology to study more in recent years to super-hydrophobicization method; Like damp process-use molecule self-assembling reaction; Receive micron particle coating, drying process-low-temperature plasma chemical deposition is made super hydrophobic surface paper and low-temperature plasma chemical deposition and the logotype of gas-phase chemical reaction method and is formed super hydrophobic surface paper.The super-hydrophobicity paper that these methods form all is the shoe technology that is coated with that on paper surface, forms one deck super-hydrophobic coating; Damp process still be drying process all exist because of film and paper fiber to combine be to be combined into the master with weak physics or intermolecular forces, the problem of the durable difference of hydrophobic layer.
Paper and polymer, filamentary material, very easy to change, physical strength is not high, heatproof not, so the hydrophobic reactant temperature can not be high, raw material can not have the group that causes the paper variable color.These reasons make that the compound molecule that bioaffinity is good is a raw material with nontoxicity, and the research that is lower than 100 ℃ of hydrophobic reactants under the temperature receives publicity.
Summary of the invention
The low-temperature preparation method that the purpose of this invention is to provide a kind of environmental protection, super-hydrophobicity film surface that temperature of reaction is low.
The low-temperature preparation method of super-hydrophobicity film surface of the present invention may further comprise the steps:
(1) with substrate surface in 10～60% humidity, carry out UV-light cleaning and activation treatment under 10～25 ℃ of conditions;
(2) base material after the activation is placed under the atomizing shape catalyzer environment, make catalyzer be attached to substrate surface;
The base material that (3) will be adsorbed with catalyzer places under the gasification or atomizing state of the siloxane molecule compound that contains hydrophobic alkyl, under 10～80 ℃, reacts.
The said UV-light of step (1) is that wavelength is the UV-light of 390～172nm.
The said reaction times of step (2) is 20～60 seconds.
The said reaction times of step (3) is 10～180 minutes.
Said base material is inorganic oxides such as organic materialss such as papery, linen-cotton, synthon, plastics or aluminum oxide, silicon oxide, glass, pottery, carbon fibre.
Said catalyzer is an acidic cpd, like organic acid, and aliphatic monobasic, diprotic acid, polycarboxylic acid such as acetate, tartrate, oxalic acid etc.; Also can be the compound acidic cpds of organic-inorganic such as aromatic organic acid and metatitanic acid.Catalyzer can use stoste also can use with non-aqueous solvent dilution back when using.
Said catalyzer is an acetate.
The said siloxane molecule compound that contains hydrophobic alkyl is the hexadecyl Trimethoxy silane.
Good through method substrates treated hydrophobic properties of the surface of the present invention, generally can reach more than 100 °, high energy reaches 160 °; The treating processes temperature is low, can make the different substrate materials surface be issued to hydrophobization in lower temperature, and treated substrate surface color and luster does not have considerable change; Treated fiber base material can keep its ventilation property; And this method is simple to operate, can be used in the industrialness continuous production.
Embodiment
Through embodiment and Comparative Examples the present invention is done further specific descriptions below, but embodiment of the present invention is not limited thereto.
(model is JC2000C1 to hydrophobic performance described in following examples of the present invention and the Comparative Examples with contact angle instrument; Shanghai Zhongchen digital technology equipment Co., Ltd produces) estimate; Measure down in room temperature (10～30 ℃), each sample is chosen 5 differences at least and is measured, and gets its MV.
Embodiment 1
Get common filter paper and at room temperature carried out UV-light cleaning and activation treatment 20 minutes by the 172nm UV-light; Then filter paper is placed the acetate environment 60 seconds of atomizing shape; Hexadecyl Trimethoxy silane with the atomizing shape reacts again, and temperature of reaction is 60 ℃, and the reaction times is 60 minutes.The result is as shown in table 1.The treated the highest hydrostatic in filter paper surface drips contact angle and reaches 160 °, and the visual color and luster in filter paper surface does not have considerable change.
Above-mentioned filter paper after hydrophobization is handled is placed the filtration mouth place of suction filtration container, carry out the filtration experiment of sky suction filtration and oil-water mixture.The result shows: paper has ventilation property; Oil-water mixture suction filtration result is illustrated under the effect of suction filtration pressure, and water can pass through filter paper.
Table 1
Use pure water, tea, coffee drinks, 5% sulphuric acid soln to drop in filter paper surface observation water droplet the above-mentioned filter paper of handling through hydrophobization and change the about 0.4ml of drop amount.The result is as shown in table 2.
Table 2
Embodiment 2
The hydrophobization treating processes same with embodiment 1 handled the surface of common paper, POLYACTIC ACID macromolecular material, iron plate, pottery, glass and obscure glass.The result is as shown in table 3.Treatment process of the present invention all can make the different substrate materials surface be issued to hydrophobization in lower temperature, and different with the rough degree of substrate surface, contact angle is up to 140 °, and minimum is 106 °.
Table 3
Comparative Examples 1
Clean and activation treatment with embodiment 1 same substrate surface UV-light, do not use catalyzer then, base material and hydrophobizing agent are put into container, carry out gas-phase reaction at 180 ℃, the reaction times is 180 minutes.The result is as shown in table 4, and contact angle is about 100 °, and carries out the glassy phase ratios that the low temperature hydrophobization is handled with method of the present invention at 60 ℃ in the foregoing description 2, and effect is approaching.
Table 4
Comparative Examples 2
Clean and activation treatment with embodiment 1 same filter paper substrate surface UV-light, do not use catalyzer then, directly the hydrophobizing agent with atomizing reacts; Temperature of reaction and time were respectively 60 ℃, 60 minutes, three kinds of 80 ℃, 60 minutes and 80 ℃, 180 minutes; The result is as shown in table 5, and the hydrophobic reactant effect was low when catalyst-free was described.
Table 5
| Sample | Base material | Temperature | Reaction times | Contact angle (°) |
| (℃) | (minute) | Sample 1 | Sample 2 | Sample 3 | ||
| 1 | Filter paper | 60 | 60 | 51 | 60 | 50 |
| 2 | Filter paper | 80 | 60 | 49 | 60 | 50 |
| 3 | Filter paper | 80 | 180 | 42 | 45 | 60 |
Claims (6)
1. the low-temperature preparation method of super-hydrophobicity film surface is characterized in that, may further comprise the steps:
(1) with substrate surface in 10～60% humidity, carry out UV-light cleaning and activation treatment under 10～25 ℃ of conditions;
(2) base material after the activation is placed under the atomizing shape catalyzer environment, make catalyzer be attached to substrate surface;
The base material that (3) will be adsorbed with catalyzer places under the gasification or atomizing state of the siloxane molecule compound that contains hydrophobic alkyl, under 10～80 ℃, reacts;
Above-mentioned catalyzer is acetate, tartrate or oxalic acid.
2. the said method of claim 1 is characterized in that, the said UV-light of step (1) is that wavelength is the UV-light of 390～172nm.
3. the said method of claim 1 is characterized in that, step (2) reaction times is 20～60 seconds.
4. the said method of claim 1 is characterized in that, step (3) reaction times is 10～180 minutes.
5. the said method of claim 1 is characterized in that, said base material is organic materials or inorganic oxide.
6. the said method of claim 1 is characterized in that, the said siloxane molecule compound that contains hydrophobic alkyl is the hexadecyl Trimethoxy silane.
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| CN 200910040508 CN101608109B (en) | 2009-06-20 | 2009-06-20 | Low-temperature preparation method of super-hydrophobicity film surface |
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| CN 200910040508 CN101608109B (en) | 2009-06-20 | 2009-06-20 | Low-temperature preparation method of super-hydrophobicity film surface |
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| CN101608109B true CN101608109B (en) | 2012-06-27 |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1810912A (en) * | 2006-03-03 | 2006-08-02 | 清华大学 | Soft template and ultraviolet curing process to prepare surface super hydrophobic material |
| CN101280155A (en) * | 2007-04-02 | 2008-10-08 | 中国科学院化学研究所 | Self-cleaning film and preparation thereof |
| US7485343B1 (en) * | 2005-04-13 | 2009-02-03 | Sandia Corporation | Preparation of hydrophobic coatings |
| CN101423945A (en) * | 2007-11-02 | 2009-05-06 | 中国科学院宁波材料技术与工程研究所 | Method for preparing light metal super-hydrophobic surface |
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2009
- 2009-06-20 CN CN 200910040508 patent/CN101608109B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7485343B1 (en) * | 2005-04-13 | 2009-02-03 | Sandia Corporation | Preparation of hydrophobic coatings |
| CN1810912A (en) * | 2006-03-03 | 2006-08-02 | 清华大学 | Soft template and ultraviolet curing process to prepare surface super hydrophobic material |
| CN101280155A (en) * | 2007-04-02 | 2008-10-08 | 中国科学院化学研究所 | Self-cleaning film and preparation thereof |
| CN101423945A (en) * | 2007-11-02 | 2009-05-06 | 中国科学院宁波材料技术与工程研究所 | Method for preparing light metal super-hydrophobic surface |
Non-Patent Citations (3)
| Title |
|---|
| Yunying Wu等.Preparation of hard and ultra water-repellent silicon oxide films by microwave plasma-enhanced CVD at low substrate temperatures.《Thin Solid Films》.2003,第435卷(第1-2期),161－164. * |
| Yunying Wu等.Water droplets interaction with super-hydrophobic surfaces.《Surface Science》.2006,第600卷(第18期),3710-3714. * |
| 刘霞等.超疏水性纳米界面材料的制备及其研究进展.《材料导报》.2008,第22卷(第11期),58-61,79. * |
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