CN110670344A - Super-hydrophobic flexible fabric with photocatalysis and oil-water separation performances and preparation method and application thereof - Google Patents

Super-hydrophobic flexible fabric with photocatalysis and oil-water separation performances and preparation method and application thereof Download PDF

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CN110670344A
CN110670344A CN201910982877.8A CN201910982877A CN110670344A CN 110670344 A CN110670344 A CN 110670344A CN 201910982877 A CN201910982877 A CN 201910982877A CN 110670344 A CN110670344 A CN 110670344A
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flexible fabric
hydrophobic
photocatalytic material
super
oil
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CN110670344B (en
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刘恩周
赵月梅
樊君
胡晓云
白雪
何玉东
贺春良
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Northwest University
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Northwest 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
    • D06M11/00Treating 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
    • D06M11/68Treating 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 phosphorus or compounds thereof, e.g. with chlorophosphonic acid or salts thereof
    • D06M11/69Treating 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 phosphorus or compounds thereof, e.g. with chlorophosphonic acid or salts thereof with phosphorus; with halides or oxyhalides of phosphorus; with chlorophosphonic acid or its salts
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    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/30Treatment of water, waste water, or sewage by irradiation
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    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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    • C02F1/40Devices for separating or removing fatty or oily substances or similar floating material
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    • 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
    • D06M11/00Treating 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
    • D06M11/32Treating 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
    • D06M11/36Treating 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
    • D06M11/48Oxides or hydroxides of chromium, molybdenum or tungsten; Chromates; Dichromates; Molybdates; Tungstates
    • 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
    • D06M11/00Treating 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
    • D06M11/77Treating 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 silicon or compounds thereof
    • D06M11/79Treating 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 silicon or compounds thereof with silicon dioxide, silicic acids or their salts
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    • D06M13/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/02Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with hydrocarbons
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    • D06M15/00Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/19Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
    • D06M15/37Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
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    • D06M2101/16Synthetic fibres, other than mineral fibres
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Abstract

The invention provides a super-hydrophobic flexible fabric with photocatalysis and oil-water separation performances, and a preparation method and application thereof, and belongs to the technical field of sewage treatment. According to the invention, the photocatalytic material and the hydrophobic component are loaded on the surface of the flexible fabric, so that the flexible fabric has both photocatalytic and super-hydrophobic oil-water separation performances, wherein the photocatalytic material has a good photodegradation effect on organic pollutants in sewage under the irradiation of visible light; the hydrophobic component has good film forming property and can form a hydrophobic coating on the surface of the flexible fabric. Meanwhile, the preparation method provided by the invention is simple and easy to operate, and the photocatalytic material can be loaded on the surface of the flexible fabric firstly or can be loaded on the surface of the flexible fabric together with the hydrophobic component. The example result shows that the surface water contact angle of the super-hydrophobic flexible fabric obtained by the invention can reach 164 degrees, and the degradation of methylene blue under visible light can be realized within 2 h.

Description

Super-hydrophobic flexible fabric with photocatalysis and oil-water separation performances and preparation method and application thereof
Technical Field
The invention relates to the technical field of sewage treatment, in particular to a super-hydrophobic flexible fabric with photocatalysis and oil-water separation performances, and a preparation method and application thereof.
Background
The photocatalysis technology is one of effective ways for solving the problems of energy shortage and environmental pollution at present, and has good application prospects in the fields of light energy conversion, air purification, sterilization, disinfection, self-cleaning and the like. The development of high-performance photocatalysts is still the focus of research in the field of photocatalysis. Most semiconductor photocatalysts are limited by their band structure, e.g. TiO2、ZnO、ZnS、SrTiO3And the like, can only absorb and utilize ultraviolet light, so that the utilization rate of sunlight is low; visible light catalysts having visible light response, e.g. g-C3N4、CdS、Ag3PO4、Bi2WO6P, etc., although having a high light energy utilization efficiency, they are mainly present in powder form, although having a high specific surfaceThe area and the mass and heat transfer performance are good, but the problems of easy agglomeration, difficult recovery, serious loss, easy secondary pollution and the like exist, and the large-scale application is difficult. Currently, the development of photocatalytic materials in the form of thin films having practical value is one of the research hotspots in this field.
Considering that most industrial sewage contains oil stain and toxic and harmful pollutants, the development of an oil-water separation and pollutant purification integrated technology is undoubtedly beneficial to improving the environmental treatment capability and reducing the production cost. Patent CN201711109397.8 discloses a titanium dioxide/cotton fabric with super-hydrophobic and self-cleaning functions, but only using ultraviolet light, and TiO2The oxidation performance is strong (the position of a valence band is positive), and organic components in the hydrophobic coating can be degraded, so that the stability of the hydrophobic coating is influenced. Patent CN201710894467.9 discloses a super-hydrophobic visible light photocatalytic self-cleaning coating and a preparation method thereof, but the preparation method is complex, and the composite material exists in a microsphere form, so that the problems of recycling and the like cannot be overcome. The literature (Journal of Materials Chemistry A,2015,3: 16958-16945) adopts a screen deposition technique to prepare a PDMS modified CdS thin film on a glass surface, but the thin film cannot realize oil-water separation.
Disclosure of Invention
In view of the above, the present invention aims to provide a super-hydrophobic flexible fabric with photocatalytic and oil-water separation properties, a preparation method and an application thereof, wherein the method is simple to operate and low in cost, and the obtained super-hydrophobic flexible fabric has both photocatalytic and oil-water separation properties and is good in self-cleaning ability.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a preparation method of a super-hydrophobic flexible fabric with photocatalysis and oil-water separation performances, which comprises the following steps:
(1) mixing a photocatalytic material with water, and performing ultrasonic treatment to obtain a photocatalytic material dispersion liquid;
(2) placing the flexible fabric into the photocatalytic material dispersion liquid, and sequentially carrying out sealing heating treatment and drying to obtain the flexible fabric loaded with the photocatalytic material;
(3) mixing polydimethylsiloxane, tetraethoxysilane, catalyst and solvent to obtain hydrophobic solution;
(4) placing the flexible fabric loaded with the photocatalytic material in the hydrophobic solution, and sequentially carrying out sealing heating treatment and drying to obtain a super-hydrophobic flexible fabric with photocatalytic and oil-water separation performances;
or comprises the following steps:
(a) mixing polydimethylsiloxane, tetraethoxysilane, catalyst, solvent and photocatalytic material to obtain hydrophobic solution containing the photocatalytic material;
(b) and placing the flexible fabric in the hydrophobic solution containing the photocatalytic material, and sequentially carrying out sealing heating treatment and drying to obtain the super-hydrophobic flexible fabric with photocatalytic and oil-water separation performances.
Preferably, the photocatalytic material is red phosphorus and/or bismuth tungstate; the flexible fabric is a polyester fabric; the ratio of the mass of the photocatalytic material to the area of the flexible fabric is (0.006-0.016) g:1cm2
Preferably, the temperature of the sealing and heating treatment in the step (2) is 130-160 ℃, and the time is 8-12 hours.
Preferably, the catalyst in step (3) and step (a) is independently di-n-octyltin dilaurate and/or dibutyltin dilaurate, and the solvent is independently at least one of n-hexane, cyclohexane and ethanol.
Preferably, the dosage ratio of the polydimethylsiloxane, the tetraethoxysilane, the catalyst and the solvent in the step (3) and the step (a) is independently 1g, (1-5) g, (0.1-0.2) g and 60 mL.
Preferably, the ratio of the volume of the hydrophobic solution to the area of the flexible fabric loaded with the photocatalytic material in the step (4) is (1.2-1.6) mL:1cm2(ii) a The ratio of the volume of the hydrophobic solution containing the photocatalytic material to the area of the flexible fabric in the step (b) is (1.2-1.6) mL:1cm2
Preferably, the temperature of the sealing and heating treatment in the step (4) and the step (b) is independently 100-120 ℃, and the time is independently 8-16 h.
Preferably, the hydrophobic solution in step (3) and the hydrophobic solution containing the photocatalytic material in step (a) independently further comprise paraffin and/or SiO2
The invention provides application of the super-hydrophobic flexible fabric with photocatalysis and oil-water separation performances prepared by the preparation method in sewage treatment.
The invention also provides the super-hydrophobic flexible fabric with photocatalysis and oil-water separation performances
The invention provides a preparation method of a super-hydrophobic flexible fabric with photocatalysis and oil-water separation performances, the invention can enable the flexible fabric to have photocatalysis and super-hydrophobic oil-water separation performances by loading a photocatalysis material and a hydrophobic component on the surface of the flexible fabric, wherein the photocatalysis material has a good photodegradation effect on organic pollutants in sewage under the irradiation of visible light; the hydrophobic component has good film forming property, can form a hydrophobic coating on the surface of the flexible fabric, has excellent oil-water separation performance, and can remove dust, oil stains and the like on the surface by means of water drop sliding and a photocatalysis process, thereby realizing the self-cleaning effect. Meanwhile, the preparation method provided by the invention is simple and easy to operate, and the photocatalytic material can be loaded on the surface of the flexible fabric firstly or can be loaded on the surface of the flexible fabric together with the hydrophobic component. The surface water contact angle of the super-hydrophobic flexible fabric obtained by the invention can reach 164 degrees, and the degradation of methylene blue under visible light can be realized within 2 h.
Drawings
FIG. 1 is a water drop contact object diagram of the super-hydrophobic flexible fabric obtained in example 1;
FIG. 2 is a contact angle test chart of the superhydrophobic flexible fabric obtained in example 1;
FIG. 3 is a graph showing the fluorescence intensity of methylene blue solution in example 1 at different irradiation times of visible light;
FIG. 4 is a water drop contact object diagram of the super-hydrophobic flexible fabric obtained in example 2;
FIG. 5 is a contact angle test chart of the superhydrophobic flexible fabric obtained in example 2;
FIG. 6 is a graph showing the fluorescence intensity of methylene blue solution in example 2 at different irradiation times of visible light.
Detailed Description
The invention provides a preparation method of a super-hydrophobic flexible fabric with photocatalysis and oil-water separation performances, which comprises the following steps:
(1) mixing a photocatalytic material with water, and performing ultrasonic treatment to obtain a photocatalytic material dispersion liquid;
(2) placing the flexible fabric into the photocatalytic material dispersion liquid, and sequentially carrying out sealing heating treatment and drying to obtain the flexible fabric loaded with the photocatalytic material;
(3) mixing polydimethylsiloxane, tetraethoxysilane, catalyst and solvent to obtain hydrophobic solution;
(4) and placing the flexible fabric loaded with the photocatalytic material in the hydrophobic solution, and sequentially carrying out sealing heating treatment and drying to obtain the super-hydrophobic flexible fabric with photocatalytic and oil-water separation performances.
The invention mixes the photocatalysis material with water, and obtains the photocatalysis material dispersion liquid after ultrasonic treatment. In the present invention, the photocatalytic material is preferably red phosphorus and/or bismuth tungstate, and the particle size of the photocatalytic material is preferably <1 μm. In the invention, the volume ratio of the mass of the photocatalytic material to water is preferably (0.2-2) g: 500mL, more preferably at a concentration of 1g: 500 mL; the frequency of the ultrasonic wave is preferably 20KHz, the power is preferably 300-800W, more preferably 300W, 400W, 500W, 600W, 700W or 800W, and the time is preferably 10 h. The invention changes the grain diameter of the photocatalysis material into nanometer grade by ultrasonic.
After the photocatalytic material dispersion liquid is obtained, the flexible fabric is placed in the photocatalytic material dispersion liquid, and sealing, heating and drying are sequentially carried out to obtain the photocatalytic material loaded flexible fabric. In the invention, the flexible fabric is preferably a polyester fabric, and the polyester fabric is flexible and wear-resistant, has rich pore channels and is uniformly distributed, thereby being beneficial to the load of a photocatalytic material and a hydrophobic component; before the sealing and heating treatment, the flexible fabric is preferably subjected to washing and drying treatment to remove stains on the surface of the flexible fabric. In the present inventionThe mass to area ratio of the photocatalytic material to the flexible fabric is preferably 0.006 g:1cm2. According to the invention, the photocatalytic material dispersion liquid and the flexible fabric are preferably placed in a sealed container for sealing and heating treatment, the temperature of the sealing and heating treatment is preferably 130-160 ℃, more preferably 140-150 ℃, the time is preferably 8-12 h, more preferably 9-11 h, the temperature and the pressure in the sealed container can be increased, and the adhesion of a hydrophobic component on the surface of the fabric is facilitated. The invention preferably cools and washes the flexible fabric after the sealing and heating treatment, and then dries the fabric; the washing detergent is preferably water; the present invention does not require any particular manner of cooling and washing, and cooling and washing means well known to those skilled in the art may be used.
The invention mixes polydimethylsiloxane, tetraethoxysilane, catalyst and solvent to obtain hydrophobic solution. In the present invention, the catalyst is preferably di-n-octyltin dilaurate and/or dibutyltin dilaurate, more preferably di-n-octyltin dilaurate or dibutyltin dilaurate, and the solvent is preferably at least one of n-hexane, cyclohexane and ethanol, more preferably n-hexane, cyclohexane or ethanol; the dosage ratio of the polydimethylsiloxane, the ethyl orthosilicate, the catalyst and the solvent is preferably 1g: (1-5) g: (0.1-0.2) g:60mL, more preferably 1g: 2 g: 0.1 g:60 mL. In the invention, the mixing mode is preferably stirring mixing, and the mixing temperature is preferably 40-60 ℃, and more preferably 50 ℃. During the stirring and mixing process, polydimethylsiloxane and tetraethoxysilane are subjected to polymerization reaction to generate a long-chain cross-linked reticular polymer, and the polymer has good hydrophobic property.
After the hydrophobic solution is obtained, the flexible fabric loaded with the photocatalytic material is placed in the hydrophobic solution, and sealing, heating and drying are sequentially carried out to obtain the super-hydrophobic flexible fabric with photocatalytic and oil-water separation performances. In the invention, the ratio of the volume of the hydrophobic solution to the area of the flexible fabric loaded with the photocatalytic material is preferably (1.2-1.6) mL:1cm2. The hydrophobic solution and the flexible fabric are preferably placed in a sealed containerAnd (3) carrying out sealing and heating treatment, wherein the sealing and heating treatment temperature is preferably 100-120 ℃, more preferably 110 ℃, and the time is preferably 12 h. During sealing and heating treatment, the long-chain cross-linked network polymer in the hydrophobic solution can form a hydrophobic coating on the surface of the flexible fabric, so that the flexible fabric has excellent oil-water separation performance, and dust, oil stains and the like on the surface can be removed by means of water drop sliding and a photocatalysis process, so that a self-cleaning effect is realized. The invention preferably cools and washes the flexible fabric after the sealing and heating treatment, and then dries the fabric; the present invention does not require any particular manner of cooling and washing, and cooling and washing means well known to those skilled in the art may be used.
Or, the invention provides a preparation method of the super-hydrophobic flexible fabric with photocatalysis and oil-water separation performances, which comprises the following steps:
(a) mixing polydimethylsiloxane, tetraethoxysilane, catalyst, solvent and photocatalytic material to obtain hydrophobic solution containing the photocatalytic material;
(b) and placing the flexible fabric in the hydrophobic solution containing the photocatalytic material, and sequentially carrying out sealing heating treatment and drying to obtain the super-hydrophobic flexible fabric with photocatalytic and oil-water separation performances.
The invention mixes polydimethylsiloxane, tetraethoxysilane, catalyst, solvent and photocatalytic material to obtain hydrophobic solution containing the photocatalytic material. In the present invention, the types of the photocatalytic material, the catalyst and the solvent, and the dosage ratio of the polydimethylsiloxane, the tetraethoxysilane, the catalyst and the solvent are the same as those in the above-mentioned scheme, and are not described herein again. In the present invention, the amount of the photocatalytic material is the same as the mass of the photocatalytic material and the area ratio of the flexible fabric in the step (2), and details are not repeated herein. In the present invention, the mixing is preferably performed by stirring; the temperature during mixing is preferably 40-60 ℃, and more preferably 50 ℃. According to the invention, the polydimethylsiloxane, the ethyl orthosilicate, the catalyst and the solvent are preferably firstly mixed and stirred, and then the photocatalytic material is added for secondary stirring and mixing. According to the invention, polydimethylsiloxane and tetraethoxysilane are subjected to polymerization reaction in the first mixing process to generate a long-chain cross-linked reticular polymer, the polymer has good hydrophobic property, and then a catalyst is added to ensure that raw materials are fully dispersed, and catalyst particles participate in the cross-linking reaction, so that the particles finally attached to the surface of the fabric fiber are not easy to fall off. In the invention, the time for the first mixing is preferably 2-4 h, more preferably 2h, and the time for the second mixing is preferably 12-24 h, more preferably 12-18 h.
After the hydrophobic solution containing the photocatalytic material is obtained, the flexible fabric is placed in the hydrophobic solution containing the photocatalytic material, and sealing, heating and drying are sequentially carried out to obtain the super-hydrophobic flexible fabric with photocatalytic and oil-water separation performances. In the present invention, the specific operation manner and conditions of the sealing heat treatment and drying are the same as those in the step (4), and are not described herein again.
In the present invention, the hydrophobic solution in the step (3) and the hydrophobic solution containing the photocatalytic material in the step (a) preferably further include paraffin and/or SiO2The mass ratio of the paraffin to the polydimethylsiloxane is preferably (1.2-2.4): 1, more preferably (1.5 to 2.2): 1, most preferably 2: 1; the SiO2The mass ratio of the polydimethylsiloxane to the polydimethylsiloxane is preferably (0.6-1.4): 1, more preferably (0.8 to 1.2): 1, most preferably 1.2: 1. in the present invention, the paraffin and SiO2Loaded on the surface of flexible fabric, where paraffin is favorable for oil-water separation, SiO2Has higher roughness, and is beneficial to improving the hydrophobic performance of the hydrophobic coating. The invention is directed to the paraffin wax and/or SiO2The adding mode of (2) has no special requirements, and the mixture is directly added into the hydrophobic solution and stirred uniformly.
The invention provides the super-hydrophobic flexible fabric with photocatalysis and oil-water separation performances, which is prepared by the preparation method. In the invention, the surface of the super-hydrophobic flexible fabric is loaded with the photocatalytic material and the hydrophobic coating, so that the super-hydrophobic flexible fabric has both photocatalytic performance and super-hydrophobic oil-water separation performance, has a good photodegradation effect on organic pollutants in sewage under visible light, and can remove dust, oil stains and the like on the surface by means of water drop sliding and a photocatalytic process, thereby realizing a self-cleaning effect.
The invention provides application of the super-hydrophobic flexible fabric with photocatalysis and oil-water separation performances in sewage treatment. The super-hydrophobic flexible fabric provided by the invention can degrade organic pollutants in sewage under visible light, and is more suitable for organic sewage containing oil stains because of good oil-water separation performance.
The following examples are provided to illustrate the super-hydrophobic flexible fabric with photocatalytic and oil-water separation properties, and the preparation method and application thereof in detail, but they should not be construed as limiting the scope of the present invention.
Example 1
Weighing 1.0g of commercially available red phosphorus, ultrasonically pulverizing in 500mL of water for 10h, collecting 60mL of upper layer red phosphorus dispersion (the red phosphorus obtained from the upper layer red phosphorus dispersion has smaller particle size and is more uniformly dispersed) and mixing with 20cm2Placing the cleaned and dried polyester fabric in a closed container, sealing for 12h at 130 ℃, cooling, washing with water, and drying to obtain the polyester fabric loaded with nano red phosphorus; then 1g of polydimethylsiloxane and 2g of ethyl orthosilicate were weighed into 60mL of n-hexane reaction solution, and 0.1g of di-n-octyltin dilaurate catalyst was added. And (3) placing the obtained red phosphorus-loaded polyester fabric in the hydrophobic solution, sealing for 12h at 120 ℃, washing and drying to obtain the super-hydrophobic flexible fabric with photocatalysis and oil-water separation performances.
Water drops are dripped on the surface of the super-hydrophobic flexible fabric, the physical diagram of the super-hydrophobic flexible fabric is shown in figure 1, and as can be seen from figure 1, the super-hydrophobic flexible fabric obtained by the invention can keep the water drops on the surface of the super-hydrophobic flexible fabric spherical.
And (3) carrying out a contact angle test on the obtained super-hydrophobic flexible fabric, wherein the test result is shown in figure 2, and the result shows that the surface water contact angle of the super-hydrophobic flexible fabric can reach 151 degrees, wherein the contact angle test method comprises the following steps: the contact angle between the surface of the modified polyester fabric and a water drop is measured by adopting a full-automatic contact angle measuring instrument (Germany Dataphysics company, the instrument model: OCA20), 1.5 mu L of deionized water is respectively dropped to three different positions on the surface of the fabric by adopting a drop stopping method, the contact angle value is read by utilizing an angle measuring method, and the average value is calculated to be used as the final contact angle data for testing.
The flexible fabric is soaked in a methylene blue solution with the concentration of 10mg/L, the flexible fabric is respectively placed under visible light for irradiation (a 300W xenon lamp is provided with a 400nm optical filter) for 0min, 30min, 60min, 90min, 120min, 140min, 160min and 180min, the methylene blue solution without the flexible fabric is used as a comparison, the fluorescence intensity of the methylene blue solution is respectively tested, and the result is shown in figure 3, and the curve in figure 3 sequentially shows the fluorescence intensity of the methylene blue solution without the flexible fabric and with the flexible fabric added for 0min, 30min, 60min, 90min, 120min, 140min, 160min and 180 min. As can be seen from FIG. 3, the super-hydrophobic flexible fabric with photocatalysis and oil-water separation performances can successfully realize the degradation of methylene blue under visible light.
The flexible fabric is used for oil-water separation, and tests show that the separation efficiency of gasoline and water can reach 87%.
The oil-water separation test method comprises the following steps: selecting crude oil, diesel oil, peanut oil, normal hexane, cyclohexane and water as experimental liquid by using an oil-water separation device (self-made and volume method), placing the prepared super-hydrophobic fabric in a device with the diameter of a pipe of 30mm, preparing an oil-water solution in a certain proportion, and separating oil from water under the action of gravity, wherein the calculation formula of the separation efficiency eta is as follows:
η=V1/V0×100%,
wherein, V0Denotes the volume of oil of the oil before separation of the oil-water mixture, V1The volume of oil after separation of the oil-water mixture is shown.
Example 2
Weighing 1g of polydimethylsiloxane and 3g of ethyl orthosilicate, placing the weighed materials in 60mL of n-hexane reaction liquid, adding 0.2g of di-n-octyltin dilaurate catalyst, stirring for 2 hours, adding 2.0g of paraffin solid into the solution, and stirring at 50 ℃ until the paraffin is fully dissolved; then, 1.2g of SiO were weighed out separately20.4g of bismuth tungstate is put into the dispersion liquid and stirred for 12 hours, and then the mixture is put into a container with the length of 20cm2Cleaning dried polyester fabric, sealing at 120 deg.C for 12 hr, cooling, and washingWashing and drying to obtain the super-hydrophobic flexible fabric with photocatalysis and oil-water separation performances.
Water drops are dripped on the surface of the super-hydrophobic flexible fabric, the physical diagram of the super-hydrophobic flexible fabric is shown in FIG. 4, and as can be seen from FIG. 4, the super-hydrophobic flexible fabric obtained by the invention can keep the water drops on the surface of the super-hydrophobic flexible fabric spherical.
The contact angle test of the obtained super-hydrophobic flexible fabric is carried out, the result is shown in figure 5, and the result shows that the surface water contact angle of the super-hydrophobic flexible fabric can reach 164 degrees.
The fabric is soaked in a methylene blue solution with the concentration of 20mg/L, the fabric is respectively placed under full spectrum irradiation (300W xenon lamp) for 0min, 15min, 30min, 45min, 60min, 75min, 90min, 105min, 120min and 135min, the methylene blue solution without the flexible fabric is used as a comparison, the fluorescence intensity of the methylene blue solution is respectively tested, and the result is shown in figure 6, and the curve in figure 6 is the fluorescence intensity of the methylene blue solution after the flexible fabric is not added and the flexible fabric is added for 0min, 15min, 30min, 45min, 60min, 75min, 90min, 105min, 120min and 135min from top to bottom in sequence. As can be seen from FIG. 6, the super-hydrophobic flexible fabric with photocatalytic and oil-water separation performances can completely degrade methylene blue within 2 h.
The flexible fabric is used for oil-water separation, and tests show that the separation efficiency of gasoline and water can reach 90%.
The above embodiments show that the super-hydrophobic flexible fabric with the photocatalysis and oil-water separation performances has the photocatalysis and super-hydrophobic oil-water separation performances, and has a good photodegradation effect on organic pollutants in sewage under visible light.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.

Claims (10)

1. A preparation method of a super-hydrophobic flexible fabric with photocatalysis and oil-water separation performances is characterized by comprising the following steps:
(1) mixing a photocatalytic material with water, and performing ultrasonic treatment to obtain a photocatalytic material dispersion liquid;
(2) placing the flexible fabric into the photocatalytic material dispersion liquid, and sequentially carrying out sealing heating treatment and drying to obtain the flexible fabric loaded with the photocatalytic material;
(3) mixing polydimethylsiloxane, tetraethoxysilane, catalyst and solvent to obtain hydrophobic solution;
(4) placing the flexible fabric loaded with the photocatalytic material in the hydrophobic solution, and sequentially carrying out sealing heating treatment and drying to obtain a super-hydrophobic flexible fabric with photocatalytic and oil-water separation performances;
or comprises the following steps:
(a) mixing polydimethylsiloxane, tetraethoxysilane, catalyst, solvent and photocatalytic material to obtain hydrophobic solution containing the photocatalytic material;
(b) and placing the flexible fabric in the hydrophobic solution containing the photocatalytic material, and sequentially carrying out sealing heating treatment and drying to obtain the super-hydrophobic flexible fabric with photocatalytic and oil-water separation performances.
2. The production method according to claim 1, wherein the photocatalytic material is red phosphorus and/or bismuth tungstate; the flexible fabric is a polyester fabric; the ratio of the mass of the photocatalytic material to the area of the flexible fabric is (0.006-0.016) g:1cm2
3. The preparation method according to claim 1, wherein the temperature of the sealing heat treatment in the step (2) is 130 to 160 ℃ and the time is 8 to 12 hours.
4. The method of claim 1, wherein the catalyst in step (3) and step (a) is independently di-n-octyltin dilaurate and/or dibutyltin dilaurate, and the solvent is independently at least one of n-hexane, cyclohexane, and ethanol.
5. The production method according to claim 1 or 4, characterized in that the amounts of polydimethylsiloxane, tetraethoxysilane, catalyst and solvent used in the step (3) and the step (a) are, independently, 1g: (1-5) g: (0.1-0.2) g:60 mL.
6. The preparation method according to claim 1, wherein the ratio of the volume of the hydrophobic solution to the area of the flexible fabric loaded with the photocatalytic material in the step (4) is (1.2-1.6) mL:1cm2(ii) a The ratio of the volume of the hydrophobic solution containing the photocatalytic material to the area of the flexible fabric in the step (b) is (1.2-1.6) mL:1cm2
7. The method according to claim 1, wherein the temperature of the sealing heat treatment in the step (4) and the step (b) is independently 100 to 120 ℃ and the time is independently 8 to 16 hours.
8. The method according to claim 1, wherein the hydrophobic solution in the step (3) and the hydrophobic solution containing the photocatalytic material in the step (a) independently further comprise paraffin and/or SiO2
9. The super-hydrophobic flexible fabric with photocatalysis and oil-water separation performances prepared by the preparation method of any one of claims 1 to 8.
10. The use of the superhydrophobic flexible fabric having photocatalytic and oil-water separation properties of claim 9 in sewage treatment.
CN201910982877.8A 2019-10-16 2019-10-16 Super-hydrophobic flexible fabric with photocatalysis and oil-water separation performances and preparation method and application thereof Active CN110670344B (en)

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