CN112376273A - Preparation method of super-hydrophobic fabric - Google Patents

Preparation method of super-hydrophobic fabric Download PDF

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Publication number
CN112376273A
CN112376273A CN202011337396.0A CN202011337396A CN112376273A CN 112376273 A CN112376273 A CN 112376273A CN 202011337396 A CN202011337396 A CN 202011337396A CN 112376273 A CN112376273 A CN 112376273A
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fabric
super
hydrophobic
octadecylamine
preparation
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Inventor
刘艳花
崔佩
胥慧
徐应锋
史雪婷
王彦平
冯利邦
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Lanzhou Jiaotong University
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Lanzhou Jiaotong University
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    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M13/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/322Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing nitrogen
    • D06M13/325Amines
    • D06M13/328Amines the amino group being bound to an acyclic or cycloaliphatic carbon atom
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M23/00Treatment of fibres, threads, yarns, fabrics or fibrous goods made from such materials, characterised by the process
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2101/00Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/02Natural fibres, other than mineral fibres
    • D06M2101/04Vegetal fibres
    • D06M2101/06Vegetal fibres cellulosic
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2101/00Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/16Synthetic fibres, other than mineral fibres
    • D06M2101/30Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M2101/32Polyesters
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2200/00Functionality of the treatment composition and/or properties imparted to the textile material
    • D06M2200/10Repellency against liquids
    • D06M2200/12Hydrophobic properties
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2200/00Functionality of the treatment composition and/or properties imparted to the textile material
    • D06M2200/25Resistance to light or sun, i.e. protection of the textile itself as well as UV shielding materials or treatment compositions therefor; Anti-yellowing treatments
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2200/00Functionality of the treatment composition and/or properties imparted to the textile material
    • D06M2200/35Abrasion, pilling or fibrillation resistance

Abstract

The invention relates to the technical field of super-hydrophobic materials, in particular to a preparation method of a super-hydrophobic fabric, which comprises the following steps: (1) preparing a nano octadecylamine finishing agent by using an ultrasonic dispersion method by taking octadecylamine as a raw material; (2) carrying out suction filtration and deposition on the nano octadecylamine finishing agent obtained in the step (1) to the surface of the fabric by using a vacuum filtration method; (3) and (3) heating the fabric obtained in the step (2) to obtain the super-hydrophobic fabric. The preparation method of the super-hydrophobic fabric realizes the super-hydrophobic performance of the surface of the fabric, the static contact angle of the surface of the prepared super-hydrophobic fabric can reach 152 degrees, and the prepared super-hydrophobic fabric has good friction resistance, washing resistance and ultraviolet resistance.

Description

Preparation method of super-hydrophobic fabric
Technical Field
The invention belongs to the technical field of super-hydrophobic materials, and particularly relates to a preparation method of a super-hydrophobic fabric.
Background
Based on the inspiration of the super-hydrophobic surfaces of natural lotus leaves, water strider legs, butterfly wings, mosquito compound eyes and the like, the bionic construction of the super-hydrophobic surface becomes an important research direction in the surface interface field in recent years. The bionic super-hydrophobic surface has wide application prospect in the fields of self-cleaning, antifouling, drag reduction, antifogging, icing prevention, corrosion resistance, oil-water separation and the like. However, most artificial superhydrophobic surfaces are complex in construction process, poor in stability of surface microstructures and low-surface-energy chemical substances, short in service life, and prone to losing superhydrophobic performance under the action of external force, so that preparation and application of superhydrophobic materials are limited. Therefore, the development of a simple and easy method for constructing a superhydrophobic surface, and the improvement of the durability of the superhydrophobic surface are urgent needs for the practicability of the superhydrophobic material, and are important problems to be solved urgently in the field of surface interfaces.
The super-hydrophobic fabric with the lotus leaf effect can be widely used as clothes and decorative materials for water resistance, oil resistance, stain resistance and the like due to the advantages of dirt resistance, no washing and the like, and has wide development and application prospects. The existing super-hydrophobic fabric is based on a bionic concept and a rough structure formed by fibers on the surface of the fabric, a nano-scale rough structure is constructed on the surface of a micro-scale structure to obtain a micro-nano double-stage structure, and the fabric with super-hydrophobic performance is obtained by modifying a low-surface-energy substance. Patent CN201811364381.6 discloses a preparation method of a temperature response type self-repairing super-hydrophobic fabric, belonging to the field of super-hydrophobic fabrics. According to the invention, dopamine hydrochloride and tris (hydroxymethyl) aminomethane are adopted to prepare a bionic polydopamine solution, polycarbonate is firmly adhered to the surface of the fabric by virtue of the high adhesiveness of polydopamine, namely, the polydopamine serves as a double-sided adhesive, a better rough structure is constructed on the fabric cotton cloth due to the fact that the polycarbonate can swell in paraxylene, and then the surface of the fabric is modified by using low-surface-energy substances, namely octadecylamine and dodecanethiol, so that the temperature-response type self-repairing super-hydrophobic fabric is prepared. Although the hydrophobic fabric can still meet the requirement of superhydrophobicity after being subjected to 100 times of friction and 30 times of water washing, and the fabric does not have superhydrophobic property when being wetted by water, the superhydrophobic property can be recovered after being dried at the temperature of 60 ℃ for 80min, so that the conversion between the superhydrophobic fabric and the non-superhydrophobic fabric is realized, but in the preparation method of the superhydrophobic fabric, the raw materials are various, the operation steps are complex, and the problem of any step can cause the unrealizability of the superhydrophobic fabric, so that the practical application of the superhydrophobic fabric is limited. Therefore, how to prepare a fabric with long-lasting durability by using as few raw materials as possible through simple operation steps is a technical problem to be solved by those skilled in the art.
Disclosure of Invention
Aiming at the problems that the existing preparation method of the super-hydrophobic fabric is relatively complex, and the super-hydrophobic performance of the super-hydrophobic fabric is easily damaged by the actions of mechanical force, chemical action, ultraviolet light, high temperature and the like to cause failure, the invention provides a simple preparation method of the durable super-hydrophobic fabric. The specific technical scheme is as follows:
a preparation method of a super-hydrophobic fabric comprises the following steps:
(1) preparing a nano octadecylamine finishing agent by using an ultrasonic dispersion method by taking octadecylamine as a raw material;
(2) carrying out suction filtration and deposition on the nano octadecylamine finishing agent obtained in the step (1) to the surface of the fabric by using a vacuum filtration method;
(3) and (3) heating the fabric obtained in the step (2) to obtain the super-hydrophobic fabric.
Preferably, the nano-octadecylamine finishing agent in the step (1) is prepared by emulsifying octadecylamine in water, wherein the emulsifying ratio of octadecylamine to water is 1-5 g: 100 mL.
Preferably, the fabric in the step (2) is one or more of commercially available cotton fabric, polyester fabric, nylon fabric, wool fabric, silk fabric, polyester-viscose fabric, polyester-nitrile fabric and polyester-cotton fabric.
Preferably, the mass ratio of the nano-octadecylamine finishing agent to the fabric in the step (2) is 10-50: 1.
preferably, the mass ratio of the nano-octadecylamine finishing agent to the fabric in the step (2) is 30-50: 1.
preferably, when the vacuum filtration is performed in the step (2), the vacuum degree is 0.098MPa, the pumping speed of the vacuum pump is 60L/min, and the filtration time is 30-60 min.
Preferably, the heating temperature for heating and drying the fabric in the step (3) is 50-80 ℃, and the heating time is 30-60 min.
The super-hydrophobic fabric prepared by the preparation method.
Clothes containing the super-hydrophobic fabric prepared by the preparation method.
The invention has the beneficial effects that: according to the preparation method of the super-hydrophobic fabric, the low surface energy and the chemical characteristics of the surface alkyl chain of the nano octadecylamine finishing agent deposited on the surface of the fabric through vacuum filtration generate a synergistic effect, a micro-nano double-stage structure and low surface free energy are endowed to the surface of the fabric, the super-hydrophobic performance of the surface of the fabric is realized, the static contact angle of the surface of the prepared super-hydrophobic fabric can reach 152 degrees, and the prepared super-hydrophobic fabric has good friction resistance, washing resistance and ultraviolet resistance and has a good self-repairing function. Meanwhile, the preparation method of the super-hydrophobic fabric provided by the invention has the advantages of few instruments and equipment, simple steps, short time, no change of the original color of the fabric, simple and convenient operation, and simple and environment-friendly preparation method because the preparation process is carried out in a water system.
Drawings
FIG. 1 is a total reflection infrared spectrum of a blank polyester fabric and a super-hydrophobic polyester fabric
FIG. 2 is a scanning electron microscope picture of a blank polyester fabric and a super-hydrophobic polyester fabric
(a) The blank polyester fabric has the magnification of 1000 times; (b) the magnification of the blank polyester fabric is 10000 times; (c) the magnification of the super-hydrophobic polyester fabric is 1000 times; (d) the magnification of the super-hydrophobic polyester fabric is 10000 times.
FIG. 3 is a photograph showing the surface wetting of the blank polyester fabric and the super-hydrophobic polyester fabric by the liquid drops
(a) Completely soaking the cotton fabric by the liquid drops on the surface of the blank sample; (b) the liquid drops on the surface of the super-hydrophobic polyester fabric are spherical on the surface of the fabric.
FIG. 4 is a graph showing the relationship between the contact angle and the rubbing distance of the super-hydrophobic polyester fabric
FIG. 5 is a graph showing the relationship between the contact angle of the super-hydrophobic polyester fabric and the number of times of washing
FIG. 6 is a graph showing the relationship between the contact angle and the standing time of the super-hydrophobic polyester fabric irradiated by ultraviolet light
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and do not limit the scope of the invention.
The fabric is a flat soft piece block formed by connecting fine and flexible objects through crossing, winding and knotting.
The ultrasonic dispersion of the invention is to place the particle suspension to be treated in an ultrasonic field directly and to perform 'irradiation' treatment by using high-power ultrasonic waves, and is a dispersion means with high intensity and best effect.
The emulsification of the present invention is the effect of dispersing one liquid in very small droplets uniformly in another liquid which is not mutually soluble. Emulsification is a liquid-liquid interface phenomenon, in which two immiscible liquids, such as oil and water, are separated into two layers in a container, with less dense oil on the upper layer and more dense water on the lower layer. If a suitable surfactant is added, the oil is dispersed in water under vigorous stirring to form an emulsion, a process called emulsification.
The octadecylamine is white waxy crystal, is very easy to dissolve in chloroform, alcohol, ether and benzene, is slightly soluble in acetone, is insoluble in water, has the general property of amine, and is obtained by ammoniating and hydrogenating stearic acid. It is mainly used for preparing octadecane quaternary ammonium salt and various auxiliary agents, such as cation lubricating grease thickening agent, mineral flotation agent, asphalt emulsifier, antistatic agent, corrosion inhibitor for water treatment, surfactant, bactericide, color coupler of color film, etc.
Example 1 preparation of a superhydrophobic cotton fabric 1
(1) Ultrasonically dispersing 1g of octadecylamine into 100ml of deionized water to form a nano octadecylamine finishing agent;
(2) combining a sand core funnel filtration bottle and a vacuum pump into a vacuum filtration device, placing cotton fabrics with the diameter of 50mm on a sand core of the sand core funnel, soaking the cotton fabrics with deionized water, and mixing the cotton fabrics with a nano octadecylamine finishing agent according to the mass ratio of 50: weighing nano octadecylamine finishing agent, pouring the nano octadecylamine finishing agent onto a sand core funnel, and carrying out vacuum filtration, wherein the vacuum degree is 0.098MPa, the vacuum pump pumping speed is 60L/min, and the filtration time is 60 min.
(3) And (3) heating and drying the fabric obtained in the step (2), wherein the heating temperature is 50 ℃, and the heating time is 60min, so that the super-hydrophobic fabric can be obtained.
Example 2 preparation method of super-hydrophobic cotton fabric 2
(1) Ultrasonically dispersing 1g of octadecylamine into 100ml of deionized water to form a nano octadecylamine finishing agent;
(2) combining a sand core funnel filtration bottle and a vacuum pump into a vacuum filtration device, placing cotton fabrics with the diameter of 50mm on a sand core of the sand core funnel, soaking the cotton fabrics with deionized water, and mixing the cotton fabrics with the nano octadecylamine finishing agent according to the mass ratio of 30: weighing nano octadecylamine finishing agent, pouring the nano octadecylamine finishing agent onto a sand core funnel, and performing vacuum filtration, wherein the vacuum degree is 0.098MPa, the vacuum pump pumping speed is 60L/min, and the filtration time is 30 min;
(3) and (3) heating and drying the fabric obtained in the step (2), wherein the heating temperature is 80 ℃, and the heating time is 30min, so that the super-hydrophobic fabric can be obtained.
Example 3 preparation method of super-hydrophobic polyester fabric 3
(1) Ultrasonically dispersing 1g of octadecylamine into 100ml of deionized water to form a nano octadecylamine finishing agent;
(2) a vacuum filtration device is formed by combining a sand core funnel filtration bottle and a vacuum pump, a polyester fabric with the diameter of 50mm is placed on a sand core of the sand core funnel and is soaked by deionized water, and the mass ratio of a nano octadecylamine finishing agent to a cotton fabric is 50: weighing nano octadecylamine finishing agent, pouring the nano octadecylamine finishing agent onto a sand core funnel, and performing vacuum filtration, wherein the vacuum degree is 0.098MPa, the vacuum pump pumping speed is 60L/min, and the filtration time is 60 min;
(3) and (3) heating and drying the fabric obtained in the step (2), wherein the heating temperature is 50 ℃, and the heating time is 60min, so that the super-hydrophobic fabric can be obtained. And the total reflection infrared test is carried out as shown in figure 1, the scanning electron microscope test is carried out as shown in figure 2, and the contact angle measurement is carried out as shown in figure 3.
From FIG. 1, it can be seen that the blank polyester fabric is 2800cm-1No obvious C-H stretching vibration peak is nearby, and the ODA modified super-hydrophobic polyester fabric of the embodiment is 2750cm-1An obvious C-H stretching vibration peak appears, which indicates that the polyester fabric is successfully modified by the ODA.
As can be seen from fig. 2, the fiber surface of the blank polyester fabric is relatively smooth, the surface of the fiber of the super-hydrophobic polyester fabric in this embodiment has a layer of nano-attachment, and the two-stage structure of the micro-scale polyester fiber and the nano-scale attachment provides a structural basis for realizing super-hydrophobicity.
As can be seen from fig. 3, the droplets on the surface of the blank sample completely soaked the cotton fabric and showed a hydrophilic state; the liquid drops on the surface of the super-hydrophobic polyester fabric prepared in the embodiment are spherical and show a hydrophobic state.
Example 4 detection of Superhydrophobic Fabric Properties
1. Contact angle measurement
The super-hydrophobic technology combines physical and chemical methods, so that a micro-nano rough surface is formed, and the surface energy of the fabric is reduced. Contact angle is generally used to characterize whether a solid surface can be wetted by a liquid at rest, and when the contact angle is less than 90 °, the solid surface is a hydrophilic surface; when the contact angle is larger than 90 degrees, the surface is hydrophobic. Whereas a superhydrophobic surface refers to a surface having a static contact angle of a solid surface to water above 150 ° and a sliding angle of less than 10 °.
The contact angles of the superhydrophobic fabrics prepared in examples 1-3 of the invention and the blank control were compared and are shown in table 1.
Table 1 contact angle of superhydrophobic fabrics with blank control
Figure BDA0002797554870000041
As can be seen from Table 1, the contact angles of the superhydrophobic fabrics prepared in examples 1-3 of the invention are all larger than 150 degrees, and the superhydrophobic fabrics have excellent superhydrophobic performance.
2. Friction resistance test
The super-hydrophobic polyester fabric prepared in example 3 is used as a sample, the sample is fixed on a glass dish, the super-hydrophobic polyester fabric sample prepared in example 3 fixed on the glass dish is placed on a clean polyester fabric, a weight with the mass of 100g is placed, the sample is pulled by tweezers to rub on the clean fabric, the change of the contact angle of water drops on the surface of the polyester fabric sample prepared in example 3 is observed after 20cm of rubbing along one direction, the optical photo is shot, and the data is recorded repeatedly.
As can be seen from FIG. 4, the contact angle of the water drop floats above 150 degrees after 180cm of friction, and after the contact angle is over 180cm, the contact angle is slightly reduced, but the contact angle is kept about 145 degrees, and the water-repellent ink still has good hydrophobic property.
3. Wash resistance test
And (3) putting the super-hydrophobic polyester fabric prepared in the embodiment 3 into a washing machine, washing with clear water for 20min, naturally airing, observing the change of the contact angle of the super-hydrophobic polyester fabric, taking an optical photo of the super-hydrophobic polyester fabric, putting the super-hydrophobic polyester fabric into an oven at 80 ℃ for drying for 0.5-1h, observing the change of the contact angle of the super-hydrophobic polyester fabric, taking the optical photo of the super-hydrophobic polyester fabric, and circularly recording data for multiple times.
As can be seen from FIG. 5, after 20min of machine washing, the contact angle of the surface of the super-hydrophobic polyester fabric is reduced to about 130 degrees, the super-hydrophobic polyester fabric is changed into a hydrophobic state from a super-hydrophobic state, but after heating and self-repairing, the contact angle is over 150 degrees, the contact angle is changed into hydrophilic after three times of continuous washing, but after heating and self-repairing, the contact angle is still restored to over 150 degrees and is restored into a super-hydrophobic state, which shows that the super-hydrophobic polyester fabric prepared by the invention has good washing resistance, can be washed for many times and has long service life.
4. Ultraviolet resistance test
The super-hydrophobic polyester fabric prepared in example 3 was placed in an ultraviolet analyzer, irradiated under 254nm ultraviolet light, and the contact angle change was observed every 24 hours, and its optical photograph was taken, and data was recorded for a number of cycles.
Fig. 6 shows that after the fabric is continuously irradiated by ultraviolet light for 24 hours, 48 hours, 72 hours, 96 hours and 120 hours, the contact angles of the surfaces of the fabric are all more than 150 degrees, and the superhydrophobic state is maintained, which shows that the superhydrophobic polyester fabric prepared by the invention has good ultraviolet resistance effect and can be used for a long time.
In conclusion, the preparation method of the super-hydrophobic fabric provided by the invention realizes the super-hydrophobic performance of the surface of the fabric, the static contact angle of the surface of the prepared super-hydrophobic fabric can reach 152 degrees, and the super-hydrophobic fabric has good friction resistance, washing resistance and ultraviolet resistance and good self-repairing function. Meanwhile, the method has the advantages of few used instruments and equipment, concise steps, short time, simple and convenient operation, no change of the original color of the fabric, and simple and environment-friendly preparation method because the preparation process is carried out in a water system.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, so any modification, equivalent replacement or improvement made within the spirit and principle of the present invention should be included in the scope of the present invention.

Claims (9)

1. The preparation method of the super-hydrophobic fabric is characterized by comprising the following steps of:
(1) preparing a nano octadecylamine finishing agent by using an ultrasonic dispersion method by taking octadecylamine as a raw material;
(2) carrying out suction filtration and deposition on the nano octadecylamine finishing agent obtained in the step (1) to the surface of the fabric by using a vacuum filtration method;
(3) and (3) heating the fabric obtained in the step (2) to obtain the super-hydrophobic fabric.
2. The preparation method of claim 1, wherein the nano-octadecylamine finishing agent in the step (1) is prepared by emulsifying octadecylamine in water, wherein the emulsifying ratio of octadecylamine to water is 1-5 g: 100 mL.
3. The preparation method according to claim 1, wherein the fabric in the step (2) is one or more of a commercially available cotton fabric, a polyester fabric, a nylon fabric, a wool fabric, a silk fabric, a polyester-viscose fabric, a polyester-nitrile fabric and a polyester-cotton fabric.
4. The preparation method of claim 1, wherein the mass ratio of the nano-octadecylamine finish to the fabric in the step (2) is 10-50: 1.
5. the preparation method of claim 4, wherein the mass ratio of the nano-octadecylamine finish to the fabric in the step (2) is 30-50: 1.
6. the process according to claim 1, wherein the vacuum filtration in the step (2) is carried out under a vacuum of 0.098MPa, at a vacuum pump speed of 60L/min, for a filtration time of 30-60 min.
7. The method of claim 1, wherein the fabric is dried by heating in step (3) at a temperature of 50 to 80 ℃ for a time of 30 to 60 min.
8. A superhydrophobic fabric prepared by the preparation method of any one of claims 1-7.
9. Clothing comprising the superhydrophobic fabric prepared by the preparation method of any one of claims 1-7.
CN202011337396.0A 2020-11-25 2020-11-25 Preparation method of super-hydrophobic fabric Pending CN112376273A (en)

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