CN112252036A - Fluorine-free self-repairing-super-hydrophobic finishing agent and preparation method and application thereof - Google Patents
Fluorine-free self-repairing-super-hydrophobic finishing agent and preparation method and application thereof Download PDFInfo
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/50—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with organometallic compounds; with organic compounds containing boron, silicon, selenium or tellurium atoms
- D06M13/51—Compounds with at least one carbon-metal or carbon-boron, carbon-silicon, carbon-selenium, or carbon-tellurium bond
- D06M13/513—Compounds with at least one carbon-metal or carbon-boron, carbon-silicon, carbon-selenium, or carbon-tellurium bond with at least one carbon-silicon bond
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M23/00—Treatment of fibres, threads, yarns, fabrics or fibrous goods made from such materials, characterised by the process
- D06M23/12—Processes in which the treating agent is incorporated in microcapsules
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/02—Natural fibres, other than mineral fibres
- D06M2101/04—Vegetal fibres
- D06M2101/06—Vegetal fibres cellulosic
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
- D06M2200/01—Stain or soil resistance
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
- D06M2200/10—Repellency against liquids
- D06M2200/12—Hydrophobic properties
Abstract
The invention discloses a fluorine-free self-repairing-super-hydrophobic finishing agent, a preparation method and application thereof, and belongs to the field of functional auxiliaries. The synthesis method for preparing the self-repairing-super-hydrophobic emulsion comprises the following steps: preparing a super-hydrophobic solution → treating by oxygen plasma → uniformly mixing by a micro-reactor → ultrasonically dispersing to obtain the self-repairing super-hydrophobic emulsion. The preparation method disclosed by the invention is simple in preparation process, easy to operate, free of special and complex instruments and equipment, low in cost, and capable of ensuring that the contact angle of the finished cotton fabric with water is more than 158.7 degrees, and the static contact angle of the finished cotton fabric with water is kept more than 153.0 degrees after washing for 30 times. The fabric shows excellent repairing performance, the fabric shows a hydrophilic state after 8 times of oxygen plasma etching or 1000 standard friction experiments, the fabric is placed in an environment with the temperature of 80 ℃ for 30min, and the static contact angle of the fabric can be restored to be more than 153.0 degrees. Meanwhile, the self-repairing super-hydrophobic cotton fabric has excellent washing resistance and stain resistance.
Description
Technical Field
The invention relates to a fluorine-free self-repairing-super-hydrophobic finishing agent and a preparation method and application thereof, belonging to the field of functional additives.
Background
In recent years, the design of similar materials has had a major impact on human life, mimicking certain unique properties and functions of organisms in nature. The super-hydrophobic surface is successfully constructed by the inspiration of 'sludge but not dyeing' on the surface of the lotus leaf. When the super-hydrophobic material is applied to the textile field, the super-hydrophobic property of the surface of the fabric is determined by the surface roughness and the surface free energy, and the excellent hydrophobic property of the super-hydrophobic material has important application prospects in the aspects of self-cleaning, stain resistance, oil-water separation and other functions in the textile field. But the non-durability of superhydrophobic fabrics limits their practical application in real life. Low surface energy substances on the surface of the super-hydrophobic fabric are decomposed under the etching of strong light and strong oxidant, and the micro-nano structure on the surface is damaged by mechanical friction or scraping in the using process, so that the hydrophobic property is lost. Organisms in nature can repair the structural and functional damages spontaneously, are inspired by nature, combine the super-hydrophobic property and the self-repairing property, and improve the safety, the stability, the utilization rate and the service cycle of the super-hydrophobic fabric.
The self-repairing super-hydrophobic fabric at present is mainly divided into two types: one is to repair the low surface energy of the fabric, and the other is to repair the micro-nano structure of the surface of the fabric. The low surface energy process for repairing the fabric is as follows: under the drive of free energy, the low surface energy molecules coated inside the super-hydrophobic fabric move and migrate to the surface of the fabric, and a layer of low surface energy molecules is formed on the damaged surface again, so that the super-hydrophobic performance of the surface of the fabric is recovered. Some hydrophobic substances are usually stored in the interior of the material in advance, and when the super-hydrophobicity of the surface of the material is destroyed under the external condition, the original super-hydrophobic state can be restored through the migration of the internal hydrophobic substances. At present, containers for storing low surface energy substances are generally provided with mesoporous materials, micro/nanocapsules and self-similar network structures. The preparation process of the self-repairing super-hydrophobic fabric is complex, or a fluorine-containing low-surface-energy substance is used, so that the self-repairing super-hydrophobic fabric is not fully developed, and the application of the self-repairing super-hydrophobic fabric is limited. The micro-nano structure for repairing the surface of the fabric can be divided into two types: one is that under the external stimulation, the surrounding substances migrate to the gap of the damaged micro-nano structure to form a new micro-nano rough structure; and the other is that under the external stimulation, a new micro-nano coarse structure is reconstructed by using methods of etching, degrading and the like in the damaged in-situ. The method needs large amount of substance macroscopic migration or large amount of energy input, so the self-repairing super-hydrophobic fabric is rarely reported, most repairing conditions are harsh or only superficial structural damage can be repaired, and the application of the self-repairing super-hydrophobic fabric is also limited.
The commonly adopted repairing agent of the self-repairing super-hydrophobic cotton fabric is a fluorine-containing long-chain compound which is difficult to degrade and has bioaccumulation, durability and the like. Traces of such compounds are now occurring in many organisms, bodies of water worldwide, and even in the rare arctic region of the human world. And the preparation has the problems of complex process and the like, and the wide application of the self-repairing super-hydrophobic cotton fabric in industrial production is limited.
Disclosure of Invention
In order to solve at least one problem, the invention provides a preparation method and application of a fluorine-free self-repairing-super-hydrophobic finishing agent with simple process and low cost.
The first purpose of the invention is to provide a preparation method of a fluorine-free self-repairing-super-hydrophobic finishing agent, which comprises the following steps: preparing a certain concentration of super-hydrophobic solution → oxygen plasma treatment → mixing of a micro-reactor → ultrasonic emulsification, thus obtaining the self-repairing-super-hydrophobic emulsion.
A method of making a fluorine-free self-healing-superhydrophobic finish, the method comprising the steps of:
(1) dispersing the prepared super-hydrophobic compound in water to prepare 6.0-20.0 wt% of super-hydrophobic solution;
(2) and then carrying out oxygen plasma treatment, uniform mixing and ultrasonic dispersion on the obtained super-hydrophobic solution to obtain stable emulsion, namely the fluorine-free self-repairing-super-hydrophobic finishing agent.
In one embodiment of the present invention, the super-hydrophobic compound is one or more of silicone materials or long-chain alkane materials.
In one embodiment of the present invention, the concentration of the superhydrophobic solution is preferably 9.0-18.0 wt%.
In one embodiment of the present invention, the superhydrophobic compound is one or more of octadecylamine, triethoxyoctylsilane, dodecyltrimethoxysilane, hexadecyltrimethoxysilane.
In one embodiment of the present invention, the oxygen plasma treatment time is 100 to 300s and the power is 100 to 300W.
In one implementation method of the invention, the uniformly mixing is performed by stirring and mixing for 10-30 min at 500-1000 rpm.
In one implementation method of the invention, the ultrasonic treatment time is 10-60 min, and the power is 200-500W.
In one implementation method of the invention, the temperature of the ultrasonic treatment is 30-60 ℃.
In one embodiment, the method specifically comprises: treating 6.0-20.0 wt% of super-hydrophobic solution by oxygen plasma to increase hydrophilic groups on the surface of the super-hydrophobic solution, uniformly mixing the super-hydrophobic solution by a micro reactor, and uniformly dispersing super-hydrophobic molecules in water by ultrasonic emulsification to obtain the stable self-repairing super-hydrophobic finishing agent.
The second purpose of the invention is to provide a fluorine-free self-repairing-super-hydrophobic finishing agent by utilizing the preparation method.
The third purpose of the invention is to provide a method for finishing cotton fabric by using the fluorine-free self-repairing-super-hydrophobic finishing agent.
In one embodiment, a method for hydrophobic finishing of cotton fabric comprises: the cotton fabric is soaked in the self-repairing super-hydrophobic finishing agent prepared by the invention, and the cotton fabric with fluorine-free self-repairing super-hydrophobic performance is obtained after pre-baking and baking.
In one embodiment of the present invention, the specific finishing method is: soaking cotton fabrics in the self-repairing super-hydrophobic finishing agent for 30-60 min, wherein the pre-drying temperature is 80 ℃, the pre-drying time is 4min, the baking temperature is 100-150 ℃, and the baking time is 3-5 min, so that the self-repairing super-hydrophobic cotton fabrics are obtained after baking.
The fourth purpose of the invention is to provide the fluoride-free self-repairing super-hydrophobic cotton fabric by using the finishing method. The fluorine-free self-repairing super-hydrophobic cotton fabric prolongs the service life and the period of the super-hydrophobic fabric, and can be applied to the fields of functional clothing, tents, industrial waterproof cloth, medical materials or self-cleaning materials.
Has the advantages that:
(1) the self-repairing super-hydrophobic finishing agent disclosed by the invention is used for treating a certain proportion of super-hydrophobic compounds by oxygen plasma, uniformly mixing and ultrasonically dispersing to prepare stable emulsion, a complex chemical modification process is not required, and the preparation method is simple in process and low in cost.
(2) The contact angle of the cotton fabric finished by the self-repairing super-hydrophobic finishing agent and water can reach more than 158 degrees, and the hydrophobic property is excellent.
(3) After the cotton fabric finished by the self-repairing super-hydrophobic finishing agent is subjected to oxygen plasma treatment or friction test, the contact angle of the fabric is reduced, or the super-hydrophobic performance is lost. But the fabric can restore super hydrophobicity after being repaired by specific conditions.
(4) The self-repairing super-hydrophobic cotton fabric loses hydrophobic performance after 8 times of oxygen plasma etching or 200 times of friction test cycles.
(5) After losing the super-hydrophobic performance, the self-repairing super-hydrophobic cotton fabric is heated for 30min at the temperature of 80 ℃ or placed for 12h at room temperature, and the super-hydrophobic performance can be recovered.
(6) The self-repairing super-hydrophobic cotton fabric has better stain resistance, the soil release grade can reach 5 grades, and the grade can reach 4-5 after 30 times of washing.
(7) The hydrophobic molecules selected by the invention are organic silicon or long-chain alkane, so that the environmental problem caused by fluorine-containing chemical reagents is avoided.
(8) The super-hydrophobic finishing agent prepared by the invention adopts water as a solvent, so that the cost and the pollution to the environment are reduced.
(9) Compared with other hydrophobic finishing methods, the method can reduce the complexity of actual production and reduce the energy consumed in multi-step production.
Drawings
FIG. 1 is a scanning electron microscope picture of cotton fabrics before and after finishing; wherein (a) is an SEM image of the fabric before finishing, and (b) is an SEM image of the fabric after finishing.
FIG. 2 is a graph of the repaired condition of the finished fabric after oxygen plasma etching.
Fig. 3 shows the repaired condition of the finished fabric after friction.
FIG. 4 is a flow chart of finishing cotton fabric with the fluorine-free self-repairing super-hydrophobic finishing agent.
Detailed Description
Embodiments of the present invention will be described in detail below with reference to examples, but those skilled in the art will appreciate that the following examples are only illustrative of the present invention and should not be construed as limiting the scope of the present invention.
Static contact Angle test: the cloth was placed on a glass slide, 10. mu.L of deionized water was dropped, and the static contact angle of the water drop was measured by a contact angle measuring instrument (DSA 25, Kruss, Germany). Each swatch was tested for 6 different sites and averaged.
And (3) testing the water washing resistance: the water washing resistance of the fabric is tested according to the AATCC Test Method 61-2003 standard, the washing time is 15min each time, the washing temperature is 40 ℃, the adopted detergent is ECE non-phosphorus standard detergent, and 1 washing cycle is equivalent to 5 daily household washing cycles.
Hydrophobic abrasion resistance test: the super-hydrophobic cotton fabric is tested by an HZ-8029A Martindel fabric abrasion resistance tester to analyze the abrasion resistance of the super-hydrophobic cotton fabric. The test conditions were standard atmospheric pressure, room temperature, and air humidity of 60%. The used abrasive is cotton fabric, the diameter of the abrasive is 120mm, the diameter of a sample for friction test is 30mm, the load pressure of the sample is 12KPa, and the abrasion rotation speed is 50 rpm.
Self-repairing performance test: self-repair capability of super-hydrophobic cotton fabric O with several cycles of micro-plasma jet generator under vacuum pressure2Plasma treatment. In each cycle, cotton fabric is placed in O2Exposure to plasma at 15WFor 60 s. After plasma treatment, the WCA of the cotton fabric was measured. The cotton fabric was then heated at 80 ℃ for 30min, or left at room temperature for 12h to recover its superhydrophobicity.
Example 1
Fabric: cotton woven cloth (C14.5X C14.5tex, 133X 172 pieces/cm)
A hexadecyltrimethoxysilane solution with a concentration of 9.0 wt% was prepared, and the solution was subjected to oxygen plasma treatment: treating the mixture for 300s at the power of 300W, uniformly mixing the mixture by a microreactor at the rotating speed of 600rpm for 30min, and finally preparing the self-repairing fluorine-free super-hydrophobic finishing agent by the ultrasonic dispersion rate of 500W for 60 min.
Soaking the cotton fabric in the prepared self-repairing fluorine-free super-hydrophobic finishing agent for 40min, wherein the pre-drying temperature is 80 ℃, the pre-drying time is 4min, the baking temperature is 150 ℃, and the baking time is 3min, so that the self-repairing super-hydrophobic cotton fabric is obtained.
Example 2
Fabric: cotton woven cloth (C14.5X C14.5tex, 133X 172 pieces/cm)
An aqueous solution of hexadecyltrimethoxysilane was prepared at a concentration of 12.0% by weight, and the solution was subjected to oxygen plasma treatment: processing with the power of 250W for 180s, uniformly mixing by a microreactor at the rotating speed of 700rpm for 20min, and finally performing ultrasonic dispersion at the power of 400W and the processing temperature of 60 ℃ for 30min to prepare the self-repairing fluorine-free super-hydrophobic finishing agent.
Soaking the cotton fabric in the prepared fluorine-free self-repairing-super-hydrophobic finishing agent for 40min, wherein the pre-drying temperature is 80 ℃, the pre-drying time is 4min, the baking temperature is 130 ℃, and the baking time is 5min, so as to obtain the self-repairing super-hydrophobic cotton fabric.
Example 3
Fabric: cotton woven cloth (C14.5X C14.5tex, 133X 172 pieces/cm)
Preparing a hexadecyl trimethoxy silane aqueous solution with the concentration of 15.0 wt%, and then subjecting the solution to oxygen plasma treatment: processing with the power of 300W for 240s, uniformly mixing through a microreactor at the rotating speed of 800rpm for 25min, and finally performing ultrasonic dispersion at the power of 300W and the processing temperature of 30 ℃ for 60min to obtain the self-repairing fluorine-free super-hydrophobic finishing agent.
Soaking the cotton fabric in the prepared fluorine-free self-repairing-super-hydrophobic finishing agent for 60min, at the pre-drying temperature of 80 ℃, for 4min, at the baking temperature of 120 ℃, for 5min, thus obtaining the self-repairing super-hydrophobic cotton fabric.
Example 4
Fabric: cotton woven cloth (C14.5X C14.5tex, 133X 172 pieces/cm)
Preparing an aqueous solution of hexadecyl trimethoxy silane with the concentration of 18.0 wt%, and then subjecting the solution to oxygen plasma treatment: treating for 300s at the power of 300W, uniformly mixing through a microreactor at the rotating speed of 750rpm for 30min, and finally performing ultrasonic dispersion at the power of 450W and the treatment temperature of 45 ℃ for 60min to prepare the self-repairing fluorine-free super-hydrophobic finishing agent.
Soaking the cotton fabric in the prepared fluorine-free self-repairing-super-hydrophobic finishing agent for 50min, at the pre-drying temperature of 80 ℃, for 4min, at the curing temperature of 140 ℃, for 4min, so as to obtain the self-repairing super-hydrophobic cotton fabric.
Example 5
The hydrophobic compound in example 3 was changed from hexadecyl trimethoxysilane to triethoxy octyl silane, and other parameters were kept unchanged to prepare a superhydrophobic cotton fabric.
Comparative example 1
In example 3, the concentration of hexadecyl trimethyl silane is 0.9 wt%, and other parameters are kept unchanged, so that the self-repairing super-hydrophobic cotton fabric is prepared.
Comparative example 2
In example 3, the concentration of hexadecyl trimethyl silane is 21.0 wt%, and other parameters are kept unchanged, so that the self-repairing super-hydrophobic cotton fabric is prepared.
Comparative example 3
In the example 3, the oxygen plasma treatment process is omitted, and other parameters are kept unchanged to prepare the self-repairing super-hydrophobic cotton fabric.
Fabric: cotton woven cloth (C14.5X C14.5tex, 133X 172 pieces/cm)
Preparing a hexadecyl trimethoxy silane aqueous solution with the concentration of 15.0 wt%, uniformly mixing through a micro-reactor at the rotating speed of 800rpm for the following time: and (3) performing ultrasonic dispersion for 25min, wherein the treatment temperature is 30 ℃ and the treatment time is 60min, so as to prepare the self-repairing fluorine-free super-hydrophobic finishing agent.
Soaking the cotton fabric in the prepared fluorine-free self-repairing-super-hydrophobic finishing agent for 60min, at the pre-drying temperature of 80 ℃, for 4min, at the baking temperature of 120 ℃, for 5min, thus obtaining the self-repairing super-hydrophobic cotton fabric.
Comparative example 4
In example 3, the micro-reactor blending process was omitted, and other parameters were kept unchanged to prepare a self-repairing superhydrophobic cotton fabric:
fabric: cotton woven cloth (C14.5X C14.5tex, 133X 172 pieces/cm)
Preparing a hexadecyl trimethoxy silane aqueous solution with the concentration of 15.0 wt%, treating the solution by oxygen plasma for 240s under the condition of 300W, and then performing ultrasonic dispersion at the treatment temperature of 30 ℃ for 60min to prepare the self-repairing fluorine-free super-hydrophobic finishing agent.
Soaking the cotton fabric in the prepared fluorine-free self-repairing-super-hydrophobic finishing agent for 60min, at the pre-drying temperature of 80 ℃, for 4min, at the baking temperature of 120 ℃, for 5min, thus obtaining the self-repairing super-hydrophobic cotton fabric.
Comparative example 5
In example 3, the ultrasonic dispersion treatment process was omitted, and other parameters were kept unchanged to prepare a self-repairing superhydrophobic cotton fabric.
Fabric: cotton woven cloth (C14.5X C14.5tex, 133X 172 pieces/cm)
Preparing a hexadecyl trimethoxy silane aqueous solution with the concentration of 15.0 wt%, then treating the solution by oxygen plasma for 240s under the condition of 300W, uniformly mixing the solution by a micro reactor at the rotating speed of 800rpm for 25min, and preparing the self-repairing fluorine-free super-hydrophobic finishing agent.
Soaking the cotton fabric in the prepared fluorine-free self-repairing-super-hydrophobic finishing agent for 60min, at the pre-drying temperature of 80 ℃, for 4min, at the baking temperature of 120 ℃, for 5min, thus obtaining the self-repairing super-hydrophobic cotton fabric.
The cotton fabrics obtained in examples 1 to 7 and comparative examples 1 to 5 were subjected to the property measurement, and the specific results are shown in Table 1.
Table 1 fabric performance results before and after treatment
As can be seen from table 1: the fluorine-free self-repairing and super-hydrophobic finishing agent is finally obtained by treating the super-hydrophobic compound with a certain concentration in the embodiments 1 to 5 by oxygen plasma, uniformly mixing the compound in a micro reactor and ultrasonically emulsifying the compound. The super-hydrophobic cotton fabric is obtained by finishing the cotton fabric, and the static contact angle can reach over 160.0 degrees. After 30 washing cycles, the static contact angle of the cotton fabric and water is kept above 153.0 degrees, and the cotton fabric shows excellent water washing resistance. The fabric was rendered hydrophilic after 8 oxygen plasma etches. The etched cotton fabric is placed in an environment with the temperature of 80 ℃ for 30min, and the static contact angle can be restored to be more than 153.0 degrees. Through 1000 times of standard friction experiments, the static contact angle of the fabric and water is lower than 150.0 degrees, the fabric is placed in an environment of 80 ℃ for 30min, the fabric recovers the super-hydrophobicity, and the static contact angle is higher than 155.0 degrees.
As can be seen from comparative examples 1-2: the concentration range of the super-hydrophobic compound is higher or lower than 6.0-20.0 wt%, and the finished fabric does not have super-hydrophobicity, water washing resistance and self-repairing performance.
From comparative example 3, it can be seen that: the super-hydrophobic compound is insoluble in water, the hydrophilic group on the surface of the super-hydrophobic compound can be increased by oxygen plasma treatment, and the hydrophilic group (-OH) and the hydrophobic group (-CH) exist on the surface of the super-hydrophobic compound treated by the oxygen plasma3) Is easy to be wrapped by water, forms uniform emulsion under the action of ultrasound, and obtains self-repairing through a soaking-drying processSuperhydrophobic cotton fabrics, but fabrics prepared without the oxygen plasma process, did not have superhydrophobicity, water-wash resistance, and self-healing properties (example 3 and control 3).
From comparative example 4, it can be seen that: the mixing step can make the super-hydrophobic compound fully contact with water, and the fabric prepared without the mixing step has certain hydrophobicity but does not have washing resistance and self-repairing performance (example 4 and comparison 3).
From comparative example 5, it can be seen that: the ultrasonic emulsification can enable two immiscible liquids of water and a hydrophobic compound to be uniformly mixed under the action of ultrasonic energy to form an oil-in-water emulsion, and the fabric finished by the super hydrophobic agent and prepared without the ultrasonic emulsification process has no super hydrophobicity, water washing resistance and self-repairing performance.
As can be seen from examples 1 to 5 and comparative examples 1 to 5: no matter which operation step or which technical parameter of the application is changed, the final self-repairing-super-hydrophobic agent finished cotton fabric is greatly reduced in super-hydrophobicity, water washing resistance and self-repairing performance, and therefore the fact that the preparation parameters and the steps are combined is very important.
Testing the uniformity of the hydrophobic effect of the cotton fabric: the finished sample is taken according to example 1 to test the static water contact angles of 5 different positions, the fluctuation range of the static water contact angles is 158.7 degrees +/-1.2, the sample does not have the water drop permeation phenomenon, and the hydrophobic effect is good. In addition, other protocols of examples 2-3 were repeated, and the results were substantially in accordance with Table 1, with a small fluctuation range.
And (3) testing the repeatability of the hydrophobic effect of the cotton fabric: a hydrophobic cotton fabric prepared according to example 3 was finished 10 times in batches and the static water contact angle range of 158.4 ° ± 1.5 was tested for each sample batch. In addition, other schemes of examples 1-2 were repeated, with results substantially consistent with those of Table 1, with a small fluctuation range.
Although the present invention has been described with reference to the preferred embodiments, it should be understood that various changes and modifications can be made therein by those skilled in the art without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (10)
1. A method of making a fluorine-free self-healing-superhydrophobic finish, the method comprising the steps of:
(1) dispersing a hydrophobic compound in water to prepare a 6.0-20.0 wt% super-hydrophobic solution;
(2) and (3) carrying out oxygen plasma treatment on the super-hydrophobic solution, and after the treatment is finished, uniformly mixing and ultrasonically dispersing to obtain stable emulsion, namely the fluorine-free self-repairing-super-hydrophobic finishing agent.
2. The method of claim 1, wherein the superhydrophobic compound is one or more of a silicone or long chain alkane compound.
3. The method of claim 1, wherein the oxygen plasma treatment is performed for 100 to 300 seconds at a power of 100 to 300W.
4. The method according to claim 1, wherein the kneading step is carried out at 500 to 1000rpm for 10 to 30 min.
5. The method according to any one of claims 1 to 4, wherein the temperature of the sonication is: the temperature is 30-60 ℃, the power is 200-500W, and the ultrasonic treatment time is 10-60 min.
6. The fluorine-free self-repairing-super-hydrophobic finishing agent prepared by the method of any one of claims 1 to 5.
7. The use of the fluorine-free self-repairing-superhydrophobic finishing agent of claim 6 in the finishing of cotton fabrics.
8. A cotton fabric hydrophobic finishing method is characterized in that a cotton fabric is soaked in the fluorine-free self-repairing-super-hydrophobic finishing agent disclosed by claim 6, and after the soaking is finished, the cotton fabric with fluorine-free self-repairing-super-hydrophobic performance is obtained through pre-baking and baking.
9. A fluorine-free self-healing-superhydrophobic cotton fabric obtained by the process of claim 8.
10. The use of the fluorine-free self-healing-superhydrophobic cotton fabric of claim 9 in the field of functional apparel, tents, industrial tarpaulins, medical materials or self-cleaning materials.
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| CN113930861A (en) * | 2021-10-25 | 2022-01-14 | 中山尚洋科技股份有限公司 | Cosmetic brush hair and preparation method thereof |
| CN115321829A (en) * | 2022-02-22 | 2022-11-11 | 江苏铁锚玻璃股份有限公司 | Fluoride-free and self-repairable super-hydrophobic glass and preparation method thereof |
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| CN110512428A (en) * | 2019-08-12 | 2019-11-29 | 江苏理工学院 | A kind of method of durable floride-free super-hydrophobic fabric finishing liquor and its finish fabric |
| CN110714325A (en) * | 2019-10-30 | 2020-01-21 | 江南大学 | Nano silicon dioxide-fluorine-free super-hydrophobic finishing agent and preparation method and application thereof |
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| CN115321829A (en) * | 2022-02-22 | 2022-11-11 | 江苏铁锚玻璃股份有限公司 | Fluoride-free and self-repairable super-hydrophobic glass and preparation method thereof |
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