CN102978954B - Method for preparing good-stability super-hydrophobic fabrics - Google Patents
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Abstract
The invention discloses a method for preparing good-stability super-hydrophobic fabrics, which comprises the following steps: dispersing organosilane polymers into an organic solvent so as to obtain 2-50 mg/mL of an organosilane polymer solution; coating the organosilane polymer solution on the surface of a fabric in a dip-coating or spray-coating mode; and carrying out curing processing on the fabric in an ultrasonic and/or heat treatment mode so as to obtain a super-hydrophobic fabric. The super-hydrophobic fabric prepared by using the method disclosed by the invention is excellent in super-hydrophobicity and hydrophobic stability, and keeps the natural mechanical properties and luster and the like of fabrics, therefore, the fabric has wide application in the fields of self-cleaning fibers and fabrics. In addition, the method disclosed by the invention is simple in preparation process, mild in reaction conditions, low in cost, and convenient for mass production.
Description
Technical field
The present invention relates to a kind of preparation method with good stability superhydrophobic fabric, relate in particular to a kind of method of preparing stable ultra-hydrophobic fabric with organosilane polymer.
Background technology
Super hydrophobic surface refers to that water droplet is greater than 150 ° at its surface contact angle, the surface that roll angle is lower.Inspired by lotus leaf effect, rapidly, base material micro-nano structure and the effect of low-surface-energy material in constructing super-drainage surface are clear and definite in super hydrophobic surface development.But still there is the defects such as preparation method's complex and expensive, poor stability and poor solvent resistance in existing super hydrophobic surface technology of preparing, has greatly limited its practical application.Constructing of super hydrophobic surface often need to be by technological means such as laser ablation, electrostatic spinning, vapour deposition, template and offset printings.There is the problems such as complex and expensive, manufacturing cycle length, base material character and size limitations are large in these technology.Poor stability is one of greatest drawback of super hydrophobic surface, and slight touching, swipe, wear and tear can cause the permanent loss of its ultra-hydrophobicity.In US Patent No. 8292404, take monocrystalline silicon as base material, by photoetching technique, obtain suitable surface roughness, and then obtain super hydrophobic surface by low-surface-energy modification, but do not inquire into its stability.In US Patent No. 7651760, by electrostatic spinning technique and chemical vapour deposition (CVD), combine, adopt poly-fluoro-alkyl acrylate to modify, the super hydrophobic surface of guessing right, does not relate to the discussion of its stability yet.In world patent WO2004113456, adopt the vapour deposition of little mol-chloric silane, generate organosilane polymer nanofiber, obtained super hydrophobic surface, but its less stable, simple finger pressure, hand touch and can cause the forfeiture of its super-hydrophobicity.
In recent years, fabric, owing to having certain surface roughness and Application Areas widely, is getting the attention aspect constructing super-drainage surface.By means of the texture structure of fabric, can realize super hydrophobic surface fast, simply construct, simplify preparation process.Because fabric has possessed certain surface roughness, so the preparation method of superhydrophobic fabric concentrates on the preparation of novel low surface energy compounds and how to improve it and is combined fastness aspect with fabric.Patent CN102352549A, at fabric face dip-coating inorganic nano-particle, is then coated, and then carries out low-surface-energy modification, obtains superhydrophobic fabric.It is catalyst that patent CN100595373C be take gold chloride and citric acid, at surface of cotton fabric loaded with nano gold grain, then carries out low-surface-energy modification, obtains superhydrophobic fabric, repeatedly folding after, ultra-hydrophobicity is good.Patent CN102174737A, by irradiation grafting technology, at fabric face covalent bond polyalkyl methacrylate, has certain water-fastness stability.Although these methods are simplified constructing of super hydrophobic surface, still need just can complete through a plurality of steps such as fabric face activation, x ray irradiation x and low-surface-energy modifications.The made low surface energy compounds of what is more important is combined mostly firm not with fabric fibre, the stability of super hydrophobic surface is still poor, and especially friction stability and solvent resistance, seriously limit the practical application of superhydrophobic fabric.Therefore, how by simple method, obtaining stable superhydrophobic fabric is this area problem demanding prompt solution.
Summary of the invention
The object of the invention is the problem existing for prior art, a kind of method with good stability superhydrophobic fabric of preparing is provided.
(1) preparation of stability superhydrophobic fabric
The present invention's preparation has the method for good stability superhydrophobic fabric, that organosilane polymer is scattered in to the machine silane polymer solution that is made into 2 ~ 50mg/mL in organic solvent, mode by dip-coating or spraying is coated on fabric face by machine silane polymer solution again, then by ultrasonic and/or heat treatment mode, be cured processing, both obtained superhydrophobic fabric.
Described fabric is polyester, cotton, wool, silk, acrylic fibers, nylon, polyurethane and BLENDED FABRIC thereof.
Its concrete preparation method comprises following processing step:
(1) preparation of organosilane polymer: the mixture of organosilan is joined in water-ol-ammono-system to hydrolytic condensation 6 ~ 48h at 30 ~ 100 ℃; Be cooled to room temperature, obtain crude product; Washing, 30 ~ 70 ℃ of vacuumizes, obtains organosilane polymer after filtration.
The mixture of described organosilan comprises that at least one hydrophobicity organosilan is (as MTES, ethyl triethoxysilane, vinyltriethoxysilane, phenyl triethoxysilane, octyltri-ethoxysilane, dodecyl triethoxysilane, cetyl triethoxysilane, octadecyltriethoxy silane and corresponding methoxy silane) and at least one hydrophily silicon-containing compound (as sodium metasilicate, potassium silicate, tetraethoxysilane, aminopropyl triethoxysilane, mercaptopropyltriethoxysilane, 3-(2, 3-epoxy the third oxygen) propyl-triethoxysilicane and corresponding methoxy silane).Hydrophobicity organosilan is 1:10 ~ 10:1 with the amount of substance ratio of hydrophily silicon-containing compound.The mixture of organosilan comprises 2 ~ 5 kinds of organosilans.
In described water-ol-ammono-system, the mass ratio of water, alcohol, ammonia is (0.2 ~ 3.6): 8:(0.03 ~ 0.5).The percentage by volume of the mixture of organosilan is 4 ~ 25%.
(2) fabric is applied: organosilane polymer is scattered in to the machine silane polymer solution that is made into 2 ~ 50mg/mL in organic solvent, then by the mode of dip-coating or spraying, machine silane polymer solution is coated on to fabric face.
Above-mentioned organic solvent is: fatty alcohol and the aromatic alcohols such as methyl alcohol, ethanol and isopropyl alcohol, benzene, toluene and homologue thereof, the alkane such as cyclohexane and octane, the halogenated hydrocarbons such as chloroform and carbon tetrachloride, ethyl acetate and acetone.
The dipping process of organosilane polymer: fabric is immersed in machine silane polymer solution, add the catalyst of organic solvent volume 0 ~ 10%, standing 2 ~ 20min.Catalyst can adopt chloracetic acid, acetic acid, trifluoroacetic acid, formic acid, benzene sulfonic acid, salicylic acid, sulfosalicylic acid, ammoniacal liquor, ethylenediamine, triethylamine, aniline, dopamine etc.
The spraying coating process of organosilane polymer is: by organosilane polymer solution spraying, to fabric, the distance of fabric and nozzle is 1 ~ 20cm.
(3) curing process: comprise two kinds of modes of ultrasonic processing and heat treatment, two kinds of modes can be carried out separately, also can process successively.
Wherein, heat cure treatment process is: after fabric is taken out from organosilane polymer solution, and heat treatment 1 ~ 100min at 25 ~ 120 ℃.
Ultrasonic curing treatment process is: fabric is immersed in organosilane polymer solution, and at 20 ~ 60 ℃, ultrasonic processing 1 ~ 60min.
(2) performance evaluation of stability superhydrophobic fabric
The method that the present invention evaluates fabric property comprises: contact angle and roll angle are measured, reciprocating friction, organic solvent, machine washing and the x ray irradiation x impact on contact angle and roll angle under load-up condition.The present invention represents hydrophobicity with contact angle and the roll angle of 10 μ L water droplets, and contact angle is higher, roll angle is lower, shows that super-hydrophobicity is better.Specific as follows:
Friction stability: by fabric under 5000Pa, reciprocating friction 200 times (reciprocal distance 20cm); Measure contact angle and roll angle.
Solvent stability: fabric is soaked in toluene 2 weeks; Measure contact angle and roll angle.
Ultraviolet irradiation stability: by (apart from light source 2cm) irradiation 24h under fabric 314nm; Measure contact angle and roll angle.
Washing machine wash stability: fabric is mixed with other fabrics, wash 30min, repeated washing 10 times at 30 ℃; Measure contact angle and roll angle.
The evaluation result of fabric super-hydrophobicity and stability: superhydrophobic fabric prepared by the present invention has excellent super-hydrophobicity: contact angle >155 °, roll angle <10 °; And under 5000Pa after reciprocating friction 200 times, contact angle is unchanged, roll angle is lower than 15 °, and can recover easily as before by repetitive coatings; It is unchanged that organic solvent soaks 2 weeks rear ultra-hydrophobicities; After long-time ultraviolet irradiation, ultra-hydrophobicity is without significant change; After washing machine washing 10 times, contact angle is unchanged, and roll angle is lower than 15 °; Thereby there is good stability.
The present invention has following beneficial effect with respect to prior art:
(1) will contain hydrophilic radical and hydrophobic grouping organosilane polymer is coated on fabric face, both can improve the associativity of itself and fabric, and can fall low-surface-energy again, thereby reach super-hydrophobic effect; By solidifying, make machine silane polymer and fabric strong bonded, improved the stability of fabric hydrophobic performance, the practical application of having expanded superhydrophobic fabric.
(2) superhydrophobic fabric of preparing has good pliability and transparent preferably, has kept the performances such as the intrinsic mechanical performance of fabric and gloss.
(3) preparation technology is simple, and reaction condition is gentle; Cost is lower, is convenient to large-scale production.
Accompanying drawing explanation
Fig. 1 is water droplet contact angle photo (from left to right) after embodiment 1 sample, reciprocating friction, toluene immersion, ultraviolet irradiation and washing;
Fig. 2 is the photo of embodiment 2 samples;
Fig. 3 is the photos of embodiment 2 samples after 200 frictions;
Fig. 4 is the photo (from left to right) of embodiment 3 ~ 5 samples.
The specific embodiment
The present invention represents hydrophobicity with contact angle and the roll angle of 10 μ L water droplets, and contact angle is higher, roll angle is lower, shows that super-hydrophobicity is better.
embodiment 1
Measure 96 μ L tetraethoxysilanes and 392 μ L MTESs, join in the round-bottomed flask that fills the saturated ethanol-ammonia solution of 20mL, magnetic agitation 10min obtains the alcohol-ammonia solution of the organosilan of homogeneous; Add 1.5mL water, in 0.5h, be warming up to 50 ℃, and keep this thermotonus 48h; Be cooled to room temperature, through suction filtration, obtain crude product; After employing 10mL methanol wash-suction filtration three times, at 50 ℃ of vacuumize 3h, obtain organosilane polymer.Take 60mg organosilane polymer, be dissolved in 10mL toluene, magnetic agitation 5min, ultrasonic dispersion 5min, then by 2 * 2cm
2polyester textile is immersed, after standing 5min, and ultrasonic processing 20min.Fabric is taken out and dried, it is carried out to performance evaluation.
The evaluation result table 1 of this sample super-hydrophobicity and stability.After sample reciprocating friction, toluene immersion, ultraviolet irradiation and washing, Fig. 1 (from left to right) is shown in by water droplet contact angle photo.
embodiment 2
Measure 538 μ L tetraethoxysilanes, 122 μ L aminopropyl trimethoxysilane and 264 μ L octyltri-ethoxysilane, join in the round-bottomed flask that fills the saturated ethanol-ammonia solution of 40mL, magnetic agitation 10min obtains the alcohol-ammonia solution of the organosilan of homogeneous; Add 6.5mL water, in 0.5h, be warming up to 50 ℃, and keep this thermotonus 24h; Be cooled to room temperature, through suction filtration, obtain crude product; After employing 10mL methanol wash-suction filtration three times, at 50 ℃ of vacuumize 3h, obtain organosilane polymer.Take this polymer of 40mg, be dissolved in 5mL toluene, magnetic agitation 5min, ultrasonic dispersion 5min, then by 2 * 2 cm
2cOTTON FABRIC is immersed, after standing 5min, and ultrasonic processing 30min.Fabric is taken out and dried, it is carried out to performance evaluation.
Evaluation result is in Table 1.Fig. 2 is shown in by the photo of sample, and Fig. 3 is shown in by the photo after 200 frictions.
embodiment 3
Measure 282 μ L tetraethoxysilanes, 118 μ L 3-(2,3-epoxy the third oxygen) propyl trimethoxy silicane and and 418 μ L cetyl triethoxysilanes, join in the round-bottomed flask that fills the saturated ethanol-ammonia solution of 20mL, magnetic agitation 10min obtains the alcohol-ammonia solution of the organosilan of homogeneous; Add 2.8mL water, in 0.5h, be warming up to 40 ℃, and keep this thermotonus 48h; Be cooled to room temperature, through suction filtration, obtain crude product; After employing 10mL methanol wash-suction filtration three times, at 50 ℃ of vacuumize 3h, obtain organosilane polymer.Take this polymer of 40mg, be dissolved in 5mL toluene, magnetic agitation 5min, ultrasonic dispersion 5min, then by this solution spraying to 2 * 2cm
2on silk fabric.After ultrasonic processing 10min, fabric is processed to 1h at 80 ℃, it is carried out to performance evaluation.
Evaluation result is in Table 1.Fig. 4 is shown in by the photo of sample.
embodiment 4
Measure 213 μ L tetraethoxysilanes, 118 μ L 3-(2,3-epoxy the third oxygen) propyl trimethoxy silicane and 512 μ L phenyl triethoxysilanes, join in the round-bottomed flask that fills the saturated ethanol-ammonia solution of 30mL, magnetic agitation 10min obtains the alcohol-ammonia solution of the organosilan of homogeneous; Add 2.5mL water, in 0.5h, be warming up to 90 ℃, and keep this thermotonus 24h; Be cooled to room temperature, through suction filtration, obtain crude product; After employing 10mL methanol wash-suction filtration three times, at 50 ℃ of vacuumize 3h, obtain organosilane polymer.Take this polymer of 20mg, be dissolved in 5mL toluene, magnetic agitation 5min, ultrasonic dispersion 5min.Then by 2 * 2cm
2wool fabric is immersed, after standing 5min, and ultrasonic processing 10min.Fabric is processed to 1h at 60 ℃, it is carried out to performance evaluation.
Evaluation result is in Table 1.Fig. 4 is shown in by the photo of sample.
embodiment 5
Measure 0.2 sodium metasilicate, 100 μ L tetraethoxysilanes, 52 μ L 3-(2,3-epoxy the third oxygen) propyl trimethoxy silicane and 672 μ L dodecyl triethoxysilanes, join in the round-bottomed flask that fills the saturated ethanol-ammonia solution of 40mL, magnetic agitation 10min obtains the alcohol-ammonia solution of the organosilan of homogeneous; Add 4.0mL water, in 0.5h, be warming up to 50 ℃, and keep this thermotonus 18h; Be cooled to room temperature, through suction filtration, obtain crude product; After employing 10mL methanol wash-suction filtration three times, at 50 ℃ of vacuumize 3h, obtain organosilane polymer.Take this polymer of 60mg, be dissolved in 5mL toluene, magnetic agitation 5min, ultrasonic dispersion 5min.Then by 2 * 2cm
2acrylic fabric is immersed, after standing 5min, and ultrasonic processing 30min.Fabric is processed to 1h at 80 ℃, it is carried out to performance evaluation.
Evaluation result is in Table 1.Fig. 4 is shown in by the photo of sample.
The hydrophobicity of table 1 superhydrophobic fabric and comprehensive stability
Note: CA/ ° is the contact angle of 10 μ L water droplets, and SA/ ° is the roll angle of 10 μ L water droplets.
Claims (6)
1. a preparation method with good stability superhydrophobic fabric, that organosilane polymer is scattered in to the organosilane polymer solution that is made into 2 ~ 50mg/mL in organic solvent, mode by dip-coating or spraying is coated on fabric face by organosilane polymer solution again, then by ultrasonic and/or heat treatment mode, be cured processing, both obtained superhydrophobic fabric;
Described organosilane polymer is prepared and obtained by following methods: the mixture of organosilan is joined in water-ol-ammono-system to hydrolytic condensation 6 ~ 48h at 30 ~ 100 ℃; Be cooled to room temperature, obtain crude product; Washing, 30 ~ 70 ℃ of vacuumizes, obtains organosilane polymer after filtration; The mixture of described organosilan comprises at least one hydrophobicity organosilan and at least one hydrophily silicon-containing compound; In described water-ol-ammono-system, the mass ratio of water, alcohol, ammonia is (0.2 ~ 3.6): 8: (0.03 ~ 0.5), the percentage by volume of the mixture of organosilan is 4 ~ 25%.
2. there is as claimed in claim 1 the preparation method of good stability superhydrophobic fabric, it is characterized in that: described dipping process is: fabric is immersed in organosilane polymer solution, add the catalyst of organic solvent volume 0 ~ 10%, standing 2 ~ 20min.
3. there is as claimed in claim 2 the preparation method of good stability superhydrophobic fabric, it is characterized in that: described catalyst is at least one in chloracetic acid, acetic acid, trifluoroacetic acid, formic acid, benzene sulfonic acid, salicylic acid, sulfosalicylic acid, ammoniacal liquor, ethylenediamine, triethylamine, aniline, dopamine.
4. there is as claimed in claim 1 the preparation method of good stability superhydrophobic fabric, it is characterized in that: described fabric is polyester, cotton, wool, silk, acrylic fibers, nylon, polyurethane and BLENDED FABRIC thereof.
5. there is as claimed in claim 1 the preparation method of good stability superhydrophobic fabric, it is characterized in that: the ultrasonic curing technique of described fabric is: fabric is immersed in organosilane polymer solution, at 20 ~ 60 ℃, ultrasonic processing 1 ~ 60min.
6. there is as claimed in claim 1 the preparation method of good stability superhydrophobic fabric, it is characterized in that: the heat cure treatment process of described fabric is: after fabric is taken out from organosilane polymer solution, heat treatment 1 ~ 100min at 25 ~ 120 ℃.
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| CN111663323A (en) * | 2019-03-08 | 2020-09-15 | 天津大学 | Clothing based on super-hydrophobic composite material |
| CN111501352B (en) * | 2020-04-24 | 2022-05-17 | 山东鑫纳超疏新材料有限公司 | Preparation method of water-based fluorine-free stable super-hydrophobic fabric |
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| CN113249972B (en) * | 2021-06-11 | 2022-02-01 | 中国科学院兰州化学物理研究所 | Preparation method of high-pressure-resistance easy-to-clean super-hydrophobic fabric |
| CN114457592B (en) * | 2022-03-10 | 2023-04-25 | 中国科学院兰州化学物理研究所 | Method for preparing super-amphiphobic fabric by using semitransparent fluorosilane polymer emulsion |
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