CN111441166A - Oil-water separation fabric and preparation method thereof - Google Patents

Oil-water separation fabric and preparation method thereof Download PDF

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Publication number
CN111441166A
CN111441166A CN202010256384.9A CN202010256384A CN111441166A CN 111441166 A CN111441166 A CN 111441166A CN 202010256384 A CN202010256384 A CN 202010256384A CN 111441166 A CN111441166 A CN 111441166A
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fabric
oil
titanium dioxide
dioxide sol
water separation
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CN111441166B (en
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沈黎
计虎泉
张德锁
周枫
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Haitai Textile Suzhou Co ltd
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Haitai Textile Suzhou Co ltd
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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
    • D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/32—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
    • D06M11/36—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
    • D06M11/46—Oxides or hydroxides of elements of Groups 4 or 14 of the Periodic Table; Titanates; Zirconates; Stannates; Plumbates
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D17/00—Separation of liquids, not provided for elsewhere, e.g. by thermal diffusion
    • B01D17/02—Separation of non-miscible liquids
    • B01D17/0202—Separation of non-miscible liquids by ab- or adsorption
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06B—TREATING TEXTILE MATERIALS USING LIQUIDS, GASES OR VAPOURS
    • D06B3/00—Passing of textile materials through liquids, gases or vapours to effect treatment, e.g. washing, dyeing, bleaching, sizing, impregnating
    • D06B3/10—Passing of textile materials through liquids, gases or vapours to effect treatment, e.g. washing, dyeing, bleaching, sizing, impregnating of fabrics
    • D06B3/18—Passing of textile materials through liquids, gases or vapours to effect treatment, e.g. washing, dyeing, bleaching, sizing, impregnating of fabrics combined with squeezing, e.g. in padding machines
    • 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
    • D06M10/00—Physical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. ultrasonic, corona discharge, irradiation, electric currents, or magnetic fields; Physical treatment combined with treatment with chemical compounds or elements
    • D06M10/02—Physical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. ultrasonic, corona discharge, irradiation, electric currents, or magnetic fields; Physical treatment combined with treatment with chemical compounds or elements ultrasonic or sonic; Corona discharge
    • D06M10/025—Corona discharge or low temperature plasma
    • 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
    • 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
    • D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
    • D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M15/643—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain
    • 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
    • D06M2101/16—Synthetic fibres, other than mineral fibres
    • D06M2101/30—Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M2101/32—Polyesters
    • 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
    • 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
    • D06M2200/35—Abrasion, pilling or fibrillation resistance

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Thermal Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Organic Chemistry (AREA)
  • Plasma & Fusion (AREA)
  • Chemical Or Physical Treatment Of Fibers (AREA)
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Abstract

The invention provides a preparation method of an oil-water separation fabric and a super-hydrophobic fabric thereof, wherein the method comprises the following steps: s1, hydrolyzing tetrabutyl titanate to obtain titanium dioxide sol; s2, adding siloxane into the titanium dioxide sol for reaction to obtain modified titanium dioxide sol; and S3, finishing the profiled fiber fabric by adopting the modified titanium dioxide sol to obtain the oil-water separation fabric. The method has simple preparation process, and the prepared fabric has excellent wear resistance, durability, renewable cyclicity and high oil-water separation efficiency.

Description

Oil-water separation fabric and preparation method thereof
Technical Field
The invention relates to a preparation method of an oil-water separation fabric and the oil-water separation fabric, in particular to a preparation method of an oil-water separation functional fabric which is constructed based on a profiled polyester fiber fabric, has wear resistance, durability, renewable circulation and high separation efficiency and the oil-water separation fabric.
Background
The treatment of oily sewage is always an important problem in production and life, and the discharge of oil stains seriously affects the ecological environment. Particularly, when severe oil drainage accidents are encountered, efficient oil-water separation materials and oil stain recovery technology are very important. At present, the widely used oil-water separation method is to utilize porous oil absorption materials to absorb oil stains so as to achieve the purpose of separating the oil stains from water, such as oil absorption felt, oil absorption sponge, oil absorption paper and the like, but the method has low separation efficiency, needs a large amount of oil absorption materials, has high cost, is difficult to treat after recovery, and is easy to cause secondary pollution. Inspired by the fact that the natural biological material has special wettability, the oil-water filtering and separating material constructed based on the super-hydrophobic super-oleophilic or super-oleophobic and super-hydrophilic interface performance receives more and more attention. Compared with other oil-water separation materials, the method has the advantages of simple separation treatment process, high separation efficiency, time and labor saving, no need of complicated secondary treatment and the like.
The textile is essential in daily life of people, has the basis of large-scale industrial production, and has low cost, firmness, durability and wide source. And the textile is formed by processing and combining fiber materials, and a large number of gaps are formed among fibers, so that a good filtering effect can be achieved. The flexible textile is used as a base material to prepare the oil-water separation material, so that the oil-water separation material has a good application prospect. The wetting performance of the material surface has direct correlation with the surface microstructure and the surface energy, the micro-nano structure is usually required to be constructed on the fiber and the fabric to improve the specific surface area of the material when the textile is used for preparing the oil-water separation material, meanwhile, the fabric is modified by using a low-surface energy reagent, so that the fabric with super-hydrophobic and super-lipophilic properties is obtained, and the purpose of separating oil and water is achieved by using the hydrophobic and lipophilic properties of the fabric.
At present, in order to improve the roughness of the surface of a textile fiber material, the surface modification is usually performed by adding some micro-nano particles, such as silicon dioxide, zinc oxide, titanium dioxide and other micro-nano particles. However, for fiber materials, the micro-nano particles have low bonding strength with fiber base materials, are easy to wear and fall off in the using process, and are particularly chemical fiber materials with smooth surfaces. The destruction of the surface structure leads to a decrease in hydrophobic properties, thereby losing the oil-water separation function. In addition, the fabric is utilized for oil-water filtration separation, so that one fabric can permeate through the fabric and the other fabric cannot permeate through the fabric due to different oil and water infiltration performances of the fabric, for example, hydrophobic and oleophylic fabric oil can permeate through the fabric and water cannot permeate through the fabric. However, a large amount of water-in-oil or oil-in-water emulsion often exists in the oil-water mixture, and the fine emulsion can easily pass through the pores among the fibers of the fabric, so that the aim of effective separation cannot be achieved, and the oil-water separation efficiency is reduced. In addition, the stability, the number of recycling times, the regeneration performance, etc. of the oil-water separation functional fabric are all the focus of attention for the technical development.
The terylene is a commonly used chemical synthetic fiber, has good mechanical property, controllable fineness length, excellent chemical corrosion resistance and stability compared with natural fiber, and is a good base material for preparing the oil-water filtering and separating material. How to modify polyester fibers to construct a micro-nano structure and prepare a high-efficiency oil-water separation fabric with excellent wear resistance, good stability and reproducibility is still a technical problem faced at present.
Disclosure of Invention
In order to solve the technical problems in the prior art, the invention discloses a preparation method of an oil-water separation fabric and the oil-water separation fabric, the preparation process is simple, and the prepared fabric has excellent wear resistance, durability, renewable cyclicity and high oil-water separation efficiency. The specific technical scheme is as follows:
in a first aspect, the invention provides a preparation method of an oil-water separation fabric, which comprises the following steps:
s1, hydrolyzing tetrabutyl titanate to obtain titanium dioxide sol;
s2, adding siloxane into the titanium dioxide sol for reaction to obtain modified titanium dioxide sol;
and S3, finishing the profiled fiber fabric by adopting the modified titanium dioxide sol to obtain the oil-water separation fabric.
Further, step S1 specifically includes:
s11, adding tetrabutyl titanate into an absolute ethanol solution to obtain a tetrabutyl titanate absolute ethanol solution, wherein the concentration of the tetrabutyl titanate absolute ethanol solution is 200-400 g/L;
s12, adding an anhydrous ethanol solution of tetrabutyl titanate into a mixed solution formed by anhydrous ethanol, glacial acetic acid and deionized water, and stirring and hydrolyzing at room temperature to generate titanium dioxide sol, wherein the volume ratio of the anhydrous ethanol solution of tetrabutyl titanate to the mixed solution is 1: 1-1: 2; in the mixed solution, the volume ratio of the absolute ethyl alcohol to the glacial acetic acid to the deionized water is 3:1: 1-6: 1: 1.
Further, in step S2, the volume ratio of the titanium dioxide sol to the siloxane is 50:1 to 50: 6.
Further, in step S2, the reaction temperature is 30-70 ℃ and the reaction time is 5-10 hours.
Further, the siloxane comprises one or more of dodecyl trimethoxy silane, hexadecyl trimethoxy silane and polydimethylsiloxane.
Further, in step S3, the profiled fiber fabric is a profiled polyester fiber fabric.
Further, the profiled polyester fiber fabric comprises a cross-shaped polyester fiber fabric and/or a Mi-shaped polyester fiber fabric.
Further, step S3 specifically includes:
s31, pretreating the profiled polyester fiber fabric by using low-temperature oxygen plasma with the power of 100-300W and the treatment time of 5-20 minutes to obtain a pretreated fabric;
s32, performing padding finishing on the fabric pretreated by the modified titanium dioxide sol obtained in the step S2, wherein the padding pressure is 100-500N, and the padding circulation is performed for 2-4 times;
s33, treating the padded and finished fabric at 120-150 ℃ for 30-120 min, taking out, and sequentially cleaning with absolute ethyl alcohol and deionized water to obtain the oil-water separation fabric.
Further, the water contact angle of the oil-water separating fabric obtained in step S3 reaches 150 ° to 162 °.
In a second aspect, the invention also provides an oil-water separation fabric, which is prepared by the method of the first aspect.
The invention has the following beneficial effects:
1. according to the preparation method, the super-hydrophobic super-oleophylic fabric constructed by taking the special-shaped polyester fiber fabric as the substrate has a multi-stage micro-nano structure, so that the hydrophobic property is good, and the wear resistance and the durability of the fabric are improved by burying titanium dioxide nano particles in the fiber.
2. According to the preparation method, the super-hydrophobic super-oleophylic fabric constructed by taking the special-shaped polyester fiber fabric as the substrate can form compact fiber gaps and a good fiber capillary effect, and can obtain higher oil-water separation efficiency.
3. According to the preparation method, titanium dioxide is fixed in fabric fibers through crosslinking of siloxane, a stable hydrophobic layer is formed on the fabric, the preparation method has a lasting and efficient hydrophobic effect, and self-repairing of the hydrophobic performance of the fabric is realized through rotation and transfer of a hydrophobic chain under the action of heat.
4. The preparation method can realize the finishing of the fabric through simple padding and high-temperature curing, and has short process flow and high production efficiency.
Additional aspects and advantages of the invention will be set forth in part in the description which follows and, in part, will be obvious from the description, or may be learned by practice of the invention.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and other drawings can be obtained by those skilled in the art without creative efforts.
FIG. 1 is an SEM image of the longitudinal appearance of the Mi-shaped polyester fiber prepared by the invention.
FIG. 2 is a SEM image of a transverse section of a Mi-shaped polyester fiber prepared by the invention.
Detailed Description
Reference will now be made in detail to embodiments of the present invention, examples of which are illustrated in the accompanying drawings, wherein like or similar reference numerals refer to the same or similar elements or elements having the same or similar function throughout. The embodiments described below with reference to the drawings are illustrative and intended to be illustrative of the invention and are not to be construed as limiting the invention.
In the description of the present invention, it is to be understood that the terms "upper", "lower", "top", "bottom", "inner", "outer", and the like, indicate orientations or positional relationships based on those shown in the drawings, and are used only for convenience in describing the present invention and for simplicity in description, and do not indicate or imply that the referenced devices or elements must have a particular orientation, be constructed and operated in a particular orientation, and thus, are not to be construed as limiting the present invention. In the description of the present invention, "a plurality" means two or more unless specifically defined otherwise. In the present invention, unless otherwise expressly stated or limited, the terms "mounted," "connected," "secured," and the like are to be construed broadly and can, for example, be fixedly connected, detachably connected, or integrally formed; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or may be connected through the interior of two elements or in interactive relation with one another. The specific meanings of the above terms in the present invention can be understood by those skilled in the art according to specific situations.
Example 1
S1, hydrolyzing tetrabutyl titanate to obtain titanium dioxide sol.
S11, adding tetrabutyl titanate into an absolute ethanol solution to obtain a tetrabutyl titanate absolute ethanol solution, wherein the concentration of the tetrabutyl titanate absolute ethanol solution is 200-400 g/L;
s12, dropwise adding 100ml of tetrabutyl titanate absolute ethyl alcohol solution with the concentration of 300 g/L into a mixed solution consisting of 80ml of absolute ethyl alcohol, 20ml of glacial acetic acid and 20ml of deionized water at room temperature, stirring while dropwise adding, and continuously stirring at room temperature until the solution is light blue after dropwise adding is finished, thereby preparing the titanium dioxide sol.
And S2, adding siloxane into the titanium dioxide sol for reaction to obtain the modified titanium dioxide sol.
13ml of hexadecyl trimethoxy silane is dripped into the titanium dioxide sol, and the mixture is stirred and reacts for 6 hours at the temperature of 30 ℃ to obtain the modified titanium dioxide sol.
And S3, finishing the polyester fabric by using the modified titanium dioxide sol to obtain the oil-water separation fabric.
And S31, placing the Mi-shaped polyester fiber fabric into low-temperature oxygen plasma equipment, and treating for 6 minutes under 200W power.
And S32, padding the fabric subjected to plasma treatment in the step S31 with modified titanium dioxide sol, wherein the padding pressure is 300N, and the padding cycle is performed for 3 times.
S33, placing the padded and finished fabric in a drying oven at 140 ℃ for high-temperature treatment for 1h, taking out, cleaning with absolute ethyl alcohol for three times, and then cleaning with deionized water to obtain the oil-water separation fabric with wear-resistant, durable, reproducible, recyclable and high-separation-efficiency super-hydrophobic and super-oleophylic characteristics.
Through detection, the water contact angle of the oil-water separation fabric prepared in the embodiment is 161.3 degrees, and the oil-water separation efficiency reaches 99.8 percent. After 5000 times of circulating dry friction, the water contact angle of the fabric is 146.8 degrees, and after the abraded fabric is heated in an oven at 80 ℃ for 30 minutes, the water contact angle can be restored to 155.2 degrees.
Example 2
S1, hydrolyzing tetrabutyl titanate to obtain titanium dioxide sol.
S11, adding tetrabutyl titanate into an absolute ethanol solution to obtain a tetrabutyl titanate absolute ethanol solution, wherein the concentration of the tetrabutyl titanate absolute ethanol solution is 200-400 g/L;
s12, dropwise adding 100ml of tetrabutyl titanate absolute ethyl alcohol solution with the concentration of 300 g/L into a mixed solution consisting of 80ml of absolute ethyl alcohol, 20ml of glacial acetic acid and 20ml of deionized water at room temperature, stirring while dropwise adding, and continuously stirring at room temperature until the solution is light blue after dropwise adding is finished, thereby preparing the titanium dioxide sol.
And S2, adding siloxane into the titanium dioxide sol for reaction to obtain the modified titanium dioxide sol.
And (3) dropwise adding 20ml of hexadecyl trimethoxy silane into the titanium dioxide sol, and stirring and reacting for 6 hours at the temperature of 30 ℃ to obtain the modified titanium dioxide sol.
In this example, the volume ratio of the prepared titania sol to hexadecyl trimethoxysilane was 11: 1; in other embodiments, the volume ratio of the prepared titanium dioxide sol to hexadecyl trimethoxy silane can also be 50: 1; in another embodiment, the volume ratio of the prepared titanium dioxide sol to hexadecyl trimethoxy silane can also be 50: 6.
In other embodiments, the reaction temperature of step S2 may also be 70 °, and the reaction time is 5 h; in another embodiment, the reaction temperature of step S2 may also be 30 ° and the reaction time 10 h.
And S3, finishing the polyester fabric by using the modified titanium dioxide sol to obtain the oil-water separation fabric.
And S31, placing the Mi-shaped polyester fiber fabric into low-temperature oxygen plasma equipment, and treating for 6 minutes under 200W power.
And S32, padding the fabric subjected to plasma treatment in the step S31 with modified titanium dioxide sol, wherein the padding pressure is 300N, and the padding cycle is performed for 3 times.
S33, placing the padded and finished fabric in a drying oven at 140 ℃ for high-temperature treatment for 1h, taking out, cleaning with absolute ethyl alcohol for three times, and then cleaning with deionized water to obtain the oil-water separation fabric with wear-resistant, durable, reproducible, recyclable and high-separation-efficiency super-hydrophobic and super-oleophylic characteristics.
Through detection, the water contact angle of the oil-water separation fabric prepared in the embodiment is 153.8 degrees, the oil-water separation efficiency reaches 99.3 percent, the water contact angle of the fabric after 5000 times of circulating dry friction is 142.7 degrees, and the water contact angle of the worn fabric can be restored to 152.1 degrees after the fabric is heated in an oven at 80 ℃ for 30 minutes.
Example 3
S1, hydrolyzing tetrabutyl titanate to obtain titanium dioxide sol.
S11, adding tetrabutyl titanate into an absolute ethanol solution to obtain a tetrabutyl titanate absolute ethanol solution, wherein the concentration of the tetrabutyl titanate absolute ethanol solution is 200-400 g/L;
s12, dropwise adding 100ml of tetrabutyl titanate absolute ethyl alcohol solution with the concentration of 300 g/L into a mixed solution consisting of 80ml of absolute ethyl alcohol, 20ml of glacial acetic acid and 20ml of deionized water at room temperature, stirring while dropwise adding, and continuously stirring at room temperature until the solution is light blue after dropwise adding is finished, thereby preparing the titanium dioxide sol.
And S2, adding siloxane into the titanium dioxide sol for reaction to obtain the modified titanium dioxide sol.
6ml of hexadecyl trimethoxy silane is dripped into the titanium dioxide sol, and the mixture is stirred and reacts for 6 hours at the temperature of 30 ℃ to obtain the modified titanium dioxide sol.
And S3, finishing the polyester fabric by using the modified titanium dioxide sol to obtain the oil-water separation fabric.
And S31, placing the Mi-shaped polyester fiber fabric into low-temperature oxygen plasma equipment, and treating for 6 minutes under 200W power.
And S32, padding the fabric subjected to plasma treatment in the step S31 with modified titanium dioxide sol, wherein the padding pressure is 300N, and the padding cycle is performed for 3 times.
S33, placing the padded and finished fabric in a drying oven at 140 ℃ for high-temperature treatment for 1h, taking out, cleaning with absolute ethyl alcohol for three times, and then cleaning with deionized water to obtain the oil-water separation fabric with wear-resistant, durable, reproducible, recyclable and high-separation-efficiency super-hydrophobic and super-oleophylic characteristics.
Through detection, the water contact angle of the oil-water separation fabric prepared in the embodiment is 154.6 degrees, the oil-water separation efficiency reaches 99.4 percent, the water contact angle of the fabric after 5000 times of circulating dry friction is 143.2 degrees, and the water contact angle of the worn fabric can be restored to 152.6 degrees after the fabric is heated in an oven at 80 ℃ for 30 minutes.
Example 4
S1, hydrolyzing tetrabutyl titanate to obtain titanium dioxide sol.
S11, adding tetrabutyl titanate into an absolute ethanol solution to obtain a tetrabutyl titanate absolute ethanol solution, wherein the concentration of the tetrabutyl titanate absolute ethanol solution is 200-400 g/L;
s12, dropwise adding 100ml of tetrabutyl titanate absolute ethyl alcohol solution with the concentration of 300 g/L into a mixed solution consisting of 80ml of absolute ethyl alcohol, 20ml of glacial acetic acid and 20ml of deionized water at room temperature, stirring while dropwise adding, and continuously stirring at room temperature until the solution is light blue after dropwise adding is finished, thereby preparing the titanium dioxide sol.
And S2, adding siloxane into the titanium dioxide sol for reaction to obtain the modified titanium dioxide sol.
And (3) dropwise adding 20ml of hexadecyl trimethoxy silane into the titanium dioxide sol, and stirring and reacting for 6 hours at the temperature of 30 ℃ to obtain the modified titanium dioxide sol.
And S3, finishing the polyester fabric by using the modified titanium dioxide sol to obtain the oil-water separation fabric.
S31, placing the mi-shaped polyester fiber fabric in a low-temperature oxygen plasma device, and treating for 12 minutes under 200W power. In other embodiments, the power of the low-temperature oxygen plasma equipment for processing the mi-shaped polyester fiber fabric can be also 100, and the processing time can be 20 minutes; in another embodiment, the power of the low-temperature oxygen plasma equipment for treating the polyester fiber fabric in the shape of a Chinese character 'mi' can be 300W, and the treatment time is 5 minutes.
And S32, padding the fabric subjected to plasma treatment in the step S31 with modified titanium dioxide sol, wherein the padding pressure is 300N, and the padding cycle is performed for 3 times.
S33, placing the padded and finished fabric in a drying oven at 140 ℃ for high-temperature treatment for 1h, taking out, cleaning with absolute ethyl alcohol for three times, and then cleaning with deionized water to obtain the oil-water separation fabric with wear-resistant, durable, reproducible, recyclable and high-separation-efficiency super-hydrophobic and super-oleophylic characteristics.
Through detection, the water contact angle of the oil-water separation fabric prepared in the embodiment is 158.2 degrees, the oil-water separation efficiency reaches 99.6 percent, the water contact angle of the fabric after 5000 times of circulating dry friction is 145.4 degrees, and the water contact angle of the worn fabric can be recovered to 153.8 degrees after the fabric is heated in an oven at 80 ℃ for 30 minutes.
Example 5
In this example, the modified titanium dioxide sol was used to finish the cross-shaped polyester fiber fabric, and the rest was the same as in example 1.
Through detection, the water contact angle of the oil-water separation fabric prepared in the embodiment is 160.3 degrees, and the oil-water separation efficiency reaches 99.3 percent. The water contact angle of the fabric after 5000 times of circulating dry friction is 144.7 degrees, and the water contact angle of the abraded fabric can recover 154.5 degrees after the fabric is heated in an oven at 80 ℃ for 30 minutes.
Example 6
The invention also provides an oil-water separation fabric which is prepared by adopting the method of the embodiment.
The separation efficiency of the oil-water separation fabric prepared by the method reaches more than 99%.
According to the invention, the polyester fabric is pretreated by low-temperature oxygen plasma, and then the modified titanium dioxide sol is padded and cured at high temperature, and is cross-linked and fixed to form the super-hydrophobic and super-oleophylic polyester fabric. The fiber surface can be etched by low-temperature oxygen plasma treatment, the formed microstructure is beneficial to the adhesion of the generated nano titanium dioxide on the fiber surface, and the problem that the micro-nano particles on the smooth surface of the polyester fiber are difficult to adhere is solved; meanwhile, the low-temperature oxygen plasma can activate the surface groups of the fibers, the generated active-COOH can react with-Ti-OH and-Si-OH on the modified titanium dioxide sol, the nano titanium dioxide and the siloxane are fixed on the fibers, and the siloxane is crosslinked on the surfaces of the fibers to form a compact hydrophobic layer. The special-shaped polyester fiber fabric is used as a base material, such as the Mi-shaped polyester fiber and the cross-shaped polyester fiber, and the specific surface area of the special-shaped polyester fiber fabric is 4-8 times that of the common round polyester fiber, so that the micro-size structure and the high specific surface area of the special-shaped polyester fiber fabric are more beneficial to improving the hydrophobic property of the fabric; secondly, by low-temperature oxygen plasma treatment and nano titanium dioxide modification with smaller size, a multi-level micro-nano composite structure surface consisting of profiled fibers, plasma etching microstructures and nano titanium dioxide can be formed, and the hydrophobicity of the multi-level micro-nano composite structure surface is effectively improved; referring to fig. 1 and 2 again, as shown in fig. 1 and 2, the polyester fiber in a shape like a Chinese character mi and a cross shape has a deeper groove structure, and the friction and wear area of the nano titanium dioxide is only the outermost part in the daily use process after the nano titanium dioxide is finished, and most of the area is effectively protected, so that the fabric finished by the preparation method of the invention has excellent wear resistance, and the outermost hydrophobic layer can achieve high-efficiency self-repair through the rotation and displacement of the hydrophobic chain under the action of heat after the hydrophobic layer is worn and damaged. In addition, the profiled polyester fiber is thinner, the fiber is softer, the woven fabric is tighter, the separation effect of the fabric on oil-water emulsion is favorably improved, meanwhile, a plurality of groove structures on the surface of the profiled fiber form a good capillary channel in oil-water filtration separation, and the fine oil-water emulsion has a good separation effect. Therefore, the super-hydrophobic super-oleophylic polyester fabric with wear-resistant, durable, reproducible, cyclic and efficient oil-water separation functions is obtained by taking the special-shaped polyester fabric as a base material through low-temperature oxygen plasma pretreatment and padding and curing treatment of the modified nano titanium dioxide sol.
In the description herein, references to the description of the term "one embodiment," "some embodiments," "an example," "a specific example" or "some examples" or the like are intended to mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above are not necessarily intended to refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Furthermore, various embodiments or examples described in this specification can be combined and combined by one skilled in the art.
While embodiments of the present invention have been shown and described above, it is to be understood that the above embodiments are exemplary and not to be construed as limiting the present invention, and that changes, modifications and variations may be made therein by those of ordinary skill in the art within the scope of the present invention.

Claims (10)

1. The preparation method of the oil-water separation fabric is characterized by comprising the following steps of:
s1, hydrolyzing tetrabutyl titanate to obtain titanium dioxide sol;
s2, adding siloxane into the titanium dioxide sol for reaction to obtain modified titanium dioxide sol;
and S3, finishing the profiled fiber fabric by adopting the modified titanium dioxide sol to obtain the oil-water separation fabric.
2. The method according to claim 1, wherein step S1 specifically comprises:
s11, adding tetrabutyl titanate into an absolute ethanol solution to obtain a tetrabutyl titanate absolute ethanol solution, wherein the concentration of the tetrabutyl titanate absolute ethanol solution is 200-400 g/L;
s12, adding an anhydrous ethanol solution of tetrabutyl titanate into a mixed solution formed by anhydrous ethanol, glacial acetic acid and deionized water, and stirring and hydrolyzing at room temperature to generate titanium dioxide sol, wherein the volume ratio of the anhydrous ethanol solution of tetrabutyl titanate to the mixed solution is 1: 1-1: 2; in the mixed solution, the volume ratio of the absolute ethyl alcohol to the glacial acetic acid to the deionized water is 3:1: 1-6: 1: 1.
3. The method according to claim 1, wherein in step S2, the volume ratio of the titanium dioxide sol to the siloxane is 50:1 to 50: 6.
4. The method according to claim 3, wherein the reaction temperature is 30 to 70 ℃ and the reaction time is 5 to 10 hours in step S2.
5. The method of claim 3,
the siloxane comprises one or more of dodecyl trimethoxy silane, hexadecyl trimethoxy silane and polydimethylsiloxane.
6. The method according to claim 1, wherein in step S3, the profiled fiber fabric is a profiled polyester fiber fabric.
7. The method of claim 6, wherein the profiled polyester fabric comprises a cruciform polyester fabric and/or a mitre polyester fabric.
8. The method according to claim 6, wherein step S3 specifically comprises:
s31, pretreating the profiled polyester fiber fabric by using low-temperature oxygen plasma with the power of 100-300W and the treatment time of 5-20 minutes to obtain a pretreated fabric;
s32, performing padding finishing on the fabric pretreated by the modified titanium dioxide sol obtained in the step S2, wherein the padding pressure is 100-500N, and the padding circulation is performed for 2-4 times;
s33, treating the padded and finished fabric at 120-150 ℃ for 30-120 min, taking out, and sequentially cleaning with absolute ethyl alcohol and deionized water to obtain the oil-water separation fabric.
9. The method as claimed in claim 6, wherein the water contact angle of the fabric for oil-water separation obtained in step S3 is 150 ° to 162 °.
10. An oil-water separating fabric produced by the method according to any one of claims 1 to 9.
CN202010256384.9A 2020-04-02 2020-04-02 Preparation method of oil-water separation fabric and oil-water separation fabric thereof Active CN111441166B (en)

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