CN110565385A - F-SiO2Nano particle and PDMS modified PET mesh fabric - Google Patents
F-SiO2Nano particle and PDMS modified PET mesh fabric Download PDFInfo
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- CN110565385A CN110565385A CN201910992112.2A CN201910992112A CN110565385A CN 110565385 A CN110565385 A CN 110565385A CN 201910992112 A CN201910992112 A CN 201910992112A CN 110565385 A CN110565385 A CN 110565385A
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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
- D06M11/77—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 silicon or compounds thereof
- D06M11/79—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 silicon or compounds thereof with silicon dioxide, silicic acids or their salts
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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
- 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
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/16—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
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Abstract
The invention discloses F-SiO2The preparation method of the nano-particle and PDMS modified PET mesh fabric comprises the following specific steps: (1) mixing SiO2The nano particles are added into a mixed solution containing ammonia water and deionized water to prepare SiO by ultrasonic2Suspension A; adding perfluorodecyl triethoxysilane (PFDTES) into ethanol to obtain a fluorosilane mixed solution B; dripping the suspension A into fluorosilane mixed solution B to prepare F-SiO2(ii) a (2) Weighing PDMS and a curing agent according to a mass ratio of 10: 1, respectively adding Tetrahydrofuran (THF), magnetically stirring for 5min, and performing ultrasonic treatment to obtain solutions a and b; mixing the solution a and the solution b to obtain a PDMS solution; then, putting the PET mesh fabric into PDMS solution for ultrasonic treatment, and precuring for 5-15min at 70-90 ℃ to obtain PDMS @ PET mesh fabric; (3) F-SiO2Adding into THF, and ultrasonic treatingImmersing hydrophobic PDMS @ PET mesh fabric into the solution containing F-SiO twice2THF solution for 10-20min, drying at 70-90 deg.C for 5min, and drying at 70-90 deg.C for 1 hr.
Description
Technical Field
The invention relates to F-SiO2A method for preparing nano particles and PDMS modified PET mesh fabric.
Background
The rapid development of the industry greatly promotes the progress of society, but the oily wastewater also brings unprecedented pressure to ecological environments such as oceans and the like. How to effectively solve this problem is a huge challenge, but researchers are still required to further strive to develop advanced technologies. Among them, membrane technology has made great progress in continuing academic research and industrial development as an effective strategy for the green, economical separation of oil/water mixtures. For example, the polymer film may achieve hydrophobicity and anti-fouling properties by mixing with hydrophobic additives or by altering its surface properties by chemical or physical modification. At present, the preparation method of the oil-water separation membrane is various. The core idea is that the membrane material plays the role of a semipermeable membrane to regulate the transportation of oil and water phases. In general, a semipermeable layer will allow the oil phase to flow through, trapping the water phase above the membrane material, where the separation capacity is highly dependent on the apparent surface energy (synergy between membrane microstructure and surface energy). As the apparent surface energy approaches the oil phase, the oil will flow through the membrane material. On the contrary, water will flow through the membrane material, but the large-scale preparation and practical application of the functional membrane at present have many limitations due to the expensive and complicated preparation process, the poor stability and flexibility of the modified membrane and the poor selectivity and recyclability.
The application potential of the super-hydrophobic material in the field of oil-water separation is more and more emphasized by researchers in various countries around the world. Super-hydrophobic coatings have been extensively studied in the modification of membranes as a commonly used enhancement technique. Numerous reports or documents indicate the possibility of using low surface energy in combination with suitable roughness profiles to prepare hydrophobic and superhydrophobic functional materials, and the potential for efficient oil-water separation using these materials. Zhang et al (Advanced Materials, 2013, 25 (14): 2071-2076) prepared a composite membrane composed of two inexpensive Materials, porous Polyurethane (PU) and Polystyrene (PS) microspheres, which had special non-wetting properties of super-hydrophobicity and super-lipophilicity. The composite membrane with the intelligent wettability can effectively separate an oil-water system. In addition, Feng et al (Macromol. Rapid Comm.2006, 27, 804-808) developed a new type of hard coating interface material and coated it on the surface of the mesh membrane to make it super-hydrophobic and super-oleophilic. In addition, the material is mainly prepared by constructing a rough surface of a micro-nano structure on a fluorine-containing material, and the separation efficiency of a diesel oil and water mixture in an experiment is very high, so that the material is suitable for many practical applications. At present, the functional materials mainly focus on methods for preparing metal mesh fabrics by a copper-plated mesh and low-energy polyurethane sponge prepared by a solution impregnation method, an electrochemical deposition method, a wet chemical method and the like, and a plurality of limitations still exist on the large-scale preparation of the functional materials.
On this basis, many researchers have begun to consider directly imparting superhydrophobicity to ordinary textiles. The nano-coating super-hydrophobic and super-oleophylic textile can be effectively used for oil-water separation, and the membrane material is prepared by means of the existing textile industry, so that the large-scale production is relatively easy to realize. Zhang et al (NPG Asia mater.2012, 4, e8.) prepared intelligent textiles with switchable super-lipophilicity and super-lipophilicity in an aqueous medium by grafting on the fabric a block copolymer containing pH-responsive poly-2-vinylpyridine (P2VP) and lipophilic/hydrophobic Polydimethylsiloxane (PDMS) blocks. The functional materials have strong application capability in the field of oil-water separation. Li et al (j. mater. chem.2012, 22, 9774-9781) modified with nanocrystalline coated fibers and octadecyl mercaptan to make superhydrophobic textiles. The hydrophobic/lipophilic filter membranes are widely applied in practical application due to low cost and good usability, but still have the problems of poor separation selectivity, low separation efficiency and the like.
The technology disclosed in this patent relates to the use of fluorided silica (F-SiO)2) The nano particles and Polydimethylsiloxane (PDMS) are used for modifying polyethylene terephthalate (PET) mesh fabric, and the F-SiO is prepared by two-step impregnation2Nanoparticles and PDMS modified PET (F-SiO)2/PDMS @ PET) mesh. The fabric has super-hydrophobic performance and can realize more than 95% of oil-water separation on various organic liquids.
Disclosure of Invention
In order to achieve the above object, the present invention provides a F-SiO2Nano particles and PDMS modified PET mesh fabric, F-SiO produced by the method2the/PDMS @ PET mesh fabric has super-hydrophobic performance and has the function of realizing oil-water separation of various organic liquids.
To achieve the aboveThe preparation idea of the invention is as follows: firstly, introducing low-energy high-viscosity silicone resin Polydimethylsiloxane (PDMS) to the surface of a polyethylene terephthalate (PET) mesh fabric to ensure that the PET and the PDMS have strong bonding strength and the flexibility of the PET mesh fabric is kept, and in addition, the introduction of the PDMS is used as an adhesive to fix fluorinated silicon oxide (F-SiO)2) Nanoparticles; second using F-SiO2The nano particles are used for secondary modification to generate micro roughness, so that a large number of bubbles are captured to enhance the hydrophobicity of the nano particles; finally, the PET mesh fabric has a specific mesh fabric aperture (cavity), and the micro-nano structure generated by the two reactions and the cavity have a synergistic effect, so that the F-SiO2the/PDMS @ PET mesh fabric obtains higher super-hydrophobic performance. The above-mentioned F-SiO2The fluorine-containing group in the nano particles is a precondition for ensuring the hydrophobicity of the nano particles.
The purpose of the invention is realized by the following technical scheme that the F-SiO2The preparation method of the nano-particle and PDMS modified PET mesh fabric comprises the following steps:
(1) Hydrophobic F-SiO2Preparation of nanoparticles
Adding 3g of silicon dioxide nano particles into a mixed solution containing 4ml of ammonia water and 16ml of deionized water, and then carrying out ultrasonic treatment for 10 min; then, 0.6ml Perfluorodecyltriethoxysilane (PFDTES) was added to 80ml ethanol and magnetically stirred at room temperature for 60 min; then, dropwise adding the silicon dioxide suspension into the fluorosilane mixed solution, and continuously stirring at the temperature of 30-50 ℃ to ensure that the hydrolytic condensation reaction is complete; after the reaction is finished, cooling the mixture to room temperature, centrifuging the reaction product for 5-10min at the centrifugal speed of 8000-15000 r/min, washing with absolute ethyl alcohol, and centrifuging twice; then, the product obtained by centrifugation is dried for 12-24h in a vacuum environment at 50-80 ℃, and finally hydrophobic SiO is obtained2Nanoparticles, labelled F-SiO2Nanoparticles;
(2) Preparation of hydrophobic PDMS @ PET mesh fabric
Placing the PET mesh fabric in deionized water and absolute ethyl alcohol for 15min, and respectively drying for 10min for later use; weighing 0.3g of PDMS and 0.03g of curing agent according to the mass ratio of 10: 1, adding 15ml of Tetrahydrofuran (THF), magnetically stirring for 5min, performing ultrasonic treatment for 20-30min, and dissolving to obtain solutions a and b respectively; then, mixing the two solutions to obtain a mixed PDMS solution; afterwards, putting the PET mesh fabric into the mixed PDMS solution and carrying out ultrasonic treatment for 30min, and then pre-curing the PET mesh fabric in an oven at 70-90 ℃ for 5-15min to obtain hydrophobic PDMS @ PET mesh fabric;
(3) Super-hydrophobic F-SiO2Preparation of/PDMS @ PET mesh fabric
0.1g F-SiO at room temperature2Weighing the nano particles into 15ml of THF, ultrasonically dispersing for 30min, and immersing the hydrophobic PDMS @ PET mesh fabric into the F-SiO-containing solution2THF solution for 10-20 min; drying in an oven at 70-90 deg.C for 5 min; taking out the mesh fabric, and immersing again in the solution containing F-SiO2THF solution for 10-20min, and placing in oven at 70-90 deg.C for 1 hr; finally, preparing the super-hydrophobic F-SiO2a/PDMS @ PET mesh.
As an improvement, the average particle diameter of the silica nanoparticles is 20nm, and the purity is 99.0%.
As an improvement, the purity of the 1H, 1H, 2H, 2H-perfluorodecyl triethoxysilane (PFDTES) is 96%.
As a modification, the PET mesh fabric is purchased with the specifications of 60 meshes, 120 meshes, 200 meshes, 250 meshes, 300 meshes and 400 meshes.
The gain effect of the invention is as follows:
1. The invention relates to F-SiO2Nanoparticles and PDMS modified PET mesh fabric, the super-hydrophobic F-SiO2The two-step impregnation involved in the preparation method of the PDMS @ PET mesh fabric does not greatly change the existing chemical fiber production process flow, greatly reduces the fixed investment and is beneficial to improving the product competitiveness.
2. The invention relates to F-SiO2nanoparticles and PDMS modified PET mesh fabric, the super-hydrophobic F-SiO2The preparation method of the PDMS (polydimethylsiloxane) PET mesh fabric adopts step-by-step production, which is beneficial to quality monitoring of each link, and meanwhile, the intermediate product (PDMS @ PET mesh fabric) of the production link can be sold or combined with other nano particles, which is beneficial to enterprisesThe industry carries out production adjustment in time according to market demands.
3. The invention relates to F-SiO2Nanoparticles and PDMS modified PET mesh fabric, the super-hydrophobic F-SiO2The preparation method of the PDMS @ PET mesh fabric adopts an oven drying and curing process, and utilizes the procedures and equipment in the weaving process, so that the energy consumption is reduced, and the energy conservation and the environmental protection are facilitated.
4. The invention relates to F-SiO2Nanoparticles and PDMS modified PET mesh fabric, the super-hydrophobic F-SiO2The preparation method of the/PDMS @ PET mesh fabric adopts an oven 80 ℃ curing process, combines corresponding waste gas treatment equipment, and produces hot air through the reaction of burning organic gases (ethanol and tetrahydrofuran) and feeds the hot air back to the oven, so that the energy consumption is reduced, and the energy conservation and environmental protection are facilitated.
Drawings
FIG. 1 preparation of superhydrophobic F-SiO2Schematic diagram of basic steps of/PDMS @ PET mesh.
FIG. 2(a) unmodified silica and (b) modified F-SiO2The wetting properties of the nanoparticles were compared.
Fig. 3 sem image of PET mesh, (a) d 0.25 mm; (b) d is 0.12 mm; (c) d is 0.075 mm; (d) d is 0.058 mm; (e) d is 0.048 mm; (f) d is 0.038 mm. (g) Super-hydrophobic F-SiO2High magnification images of/PDMS @ PET mesh (d 0.038mm) and (h) unmodified PET mesh (d 0.12 mm).
Fig. 4 SEM images and elemental composition of the PET mesh surface, (a, b) unmodified PET mesh; (c, d) superhydrophobic F-SiO2a/PDMS @ PET mesh.
FIG. 5(a) super hydrophobic F-SiO2XPS survey of/PDMS @ PET mesh, PDMS @ PET mesh and unmodified PET mesh. (b-d) high resolution spectra of each element.
FIG. 6(a) super hydrophobic F-SiO2static Water Contact Angle (CA) of the/PDMS @ PET mesh. (b) Super-hydrophobic F-SiO2Water immersion photo of/PDMS @ PET mesh. (c, d) superhydrophobic F-SiO2Water droplets on PDMS @ PET mesh and unmodified PET mesh. (e) Super-hydrophobic F-SiO2Perpdms @ PET meshThe fabric floats on the water surface.
FIG. 7 shows the hole diameter at six different hole diameters (a) of 0.25 mm; (b)0.12 mm; (c)0.075 mm; (d)0.058 mm; (e)0.048 mm; (f)0.038mm super-hydrophobic F-SiO2Water Contact Angle (CA) of PDMS @ PET mesh.
FIG. 8 shows that different oil-water mixtures have super-hydrophobic F-SiO with different pore diameters2Separation efficiency of PDMS @ PET mesh. In the figure, trichomethane: trichloromethane: n-Decane: n-decane; kerosene: kerosene; normal octane: n-octane; n-Hexane: n-hexane.
FIG. 9 shows superhydrophobic F-SiO of kerosene-water and chloroform-water mixtures (a) and (b) with different pore diameters2Separation efficiency on PDMS @ PET mesh. kerosene: kerosene; trichomethane: trichloromethane
FIG. 10 oil of different surface energies in superhydrophobic F-SiO with pore size of 0.048mm2Separation efficiency on PDMS @ PET mesh.
Detailed Description
The invention provides F-SiO2Nanoparticles and PDMS modified PET mesh fabric, the super-hydrophobic F-SiO2The general steps of the preparation method of the/PDMS @ PET mesh fabric are shown in figure 1 and comprise the following 3 key process steps.
Step 1 is hydrophobic F-SiO2Preparation of nanoparticles
Adding 3g of silicon dioxide nano particles into a mixed solution containing 4ml of ammonia water and 16ml of deionized water, and then carrying out ultrasonic treatment for 10 min; then, 0.6ml Perfluorodecyltriethoxysilane (PFDTES) was added to 80ml ethanol and magnetically stirred at room temperature for 60 min; then, dropwise adding the silicon dioxide suspension into the fluorosilane mixed solution, and continuously stirring at 40 ℃ to completely carry out the hydrolytic condensation reaction; after the reaction is finished, cooling the mixture to room temperature, centrifuging the reaction product for 5min at the centrifugal speed of 10000 r/min, washing with absolute ethyl alcohol, and centrifuging twice; then, the product obtained by centrifugation is dried for 12 hours in a vacuum environment at 60 ℃ to finally obtain hydrophobic SiO2nanoparticles, labelled F-SiO2Nanoparticles. FIG. 2 shows the result of the untreated silicaThe rice grains have high surface energy and become wet by water droplets, thereby generating hydrophilicity. Modified F-SiO2The nano particles can well keep the spherical shape of water drops and have stronger hydrophobicity. The results show that the addition of fluorine-containing groups reduces SiO2The surface energy of the nanoparticles. PET mesh fabrics with different pore diameters (0.25-0.038 mm) are selected as base materials, and the surface of the base materials is subjected to super-hydrophobic modification. It should be noted that the diameter refers to the inscribed circle of the various PET mesh fabrics, as shown by the yellow lines in fig. 3 a. In addition, the local high resolution images depict the micro-topography before and after the superhydrophobic modification, as shown in fig. 3g and h. It can be seen that agglomerated particles with micro-nano roughness appear on the surface of the treated PET mesh fabric compared to the untreated PET mesh fabric due to the addition of the nanoparticles. The roughness helps to capture a large number of bubbles, so that the PET mesh fabric obtains higher super-hydrophobic performance. Macroscopically, the change of the roughness can not cause the change of the structural shape of the mesh fabric, thereby ensuring that the application range of the mesh fabric is not limited.
Step 2 is the preparation of a hydrophobic PDMS @ PET mesh
Placing the PET mesh fabric in deionized water and absolute ethyl alcohol for 15min, and respectively drying for 10min for later use; weighing 0.3g of PDMS and 0.03g of curing agent according to the mass ratio of 10: 1, adding 15ml of Tetrahydrofuran (THF), magnetically stirring for 5min, performing ultrasonic treatment for 25min, and dissolving to obtain solutions a and b respectively; then, mixing the two solutions to obtain a mixed PDMS solution; thereafter, the PET mesh was put into the mixed PDMS solution and sonicated for 30min, and then the PET mesh was pre-cured in an oven at 80 ℃ for 10min to obtain a hydrophobic PDMS @ PET mesh.
Step 3 is super-hydrophobic F-SiO2Preparation of/PDMS @ PET mesh fabric
0.1g F-SiO at room temperature2Weighing the nanoparticles into 15ml Tetrahydrofuran (THF), ultrasonically dispersing for 30min, and placing the hydrophobic PDMS @ PET mesh fabric into F-SiO2Soaking in tetrahydrofuran solution for 15 min; drying in an oven at 80 ℃ for 5 minutes; taking out the mesh fabric, and putting in F-SiO again2Placing in tetrahydrofuran solution for 15min in an oven at 80 deg.C for 1 hr; finally, the superhydrophobic material is preparedF-SiO2a/PDMS @ PET mesh. Furthermore, the EDS spectra in fig. 4 show that the superhydrophobic F-SiO is comparable to the uncoated PET mesh fabric2The fluorine content of the/PDMS @ PET mesh was significantly increased. The experimental results also show that the only source of fluorine is the PFDTES molecule, so that the modified fluorine-containing group was successfully grafted to SiO2The surface of the nanoparticles. Similarly, silicon element which is mainly derived from SiO is also detected on the surface of the super-hydrophobic PET mesh fabric2A molecule. To further determine whether the low surface energy groups successfully modified the PET mesh fabric, the xps spectrum and the high resolution spectra of various elements of the PET mesh fabric are depicted as shown in fig. 5. Super-hydrophobic F-SiO2The high resolution C1s spectrum of the/PDMS @ PET web had four peaks at 284.0ev (corresponding to C-C/C-H bonds), 282.4ev (corresponding to C-Si bonds), 292.2ev (corresponding to C-F bonds) and 289ev (corresponding to C ═ O bonds), where the C-F bonds are due to PFDTES molecules and the C ═ O bonds are derived from the PET web. Furthermore, in the case of superhydrophobic F-SiO2The absorption peaks at 689.3ev and 684.9ev, corresponding to-CF, respectively, were also found in the high resolution F1s spectrum of the/PDMS @ PET mesh fabric2-and-CF3Chemical bond. In FIG. 6d, the high resolution Si2P spectrum shows three peaks for Si-C (100.8eV), Si-O-Si (103.4eV), and Si-OH (104.5eV), further indicating that PFDTES molecules have been grafted to the surface of the silica nanoparticles during the fluorination modification. Furthermore, the chemical bonds of Si-O-Si (288.5ev) and Si-OH (290ev) indicate PFDTES to SiO2Chemical reactions between the nanoparticles occur. Based on the above analysis, PFDTES molecules and F-SiO were demonstrated2the nanoparticles have successfully undergone a polycondensation reaction.
Water non-wettability Performance test
The non-wettability is an important factor for generating the oil-water separation function. As shown in FIG. 6a, the Contact Angle (CA) of water reached 153.3 ° (for a mesh with a pore size of 0.048 mm), indicating that F-SiO was prepared2the/PDMS @ PET mesh has great super-hydrophobicity. In addition, the prepared mesh not only shows super-hydrophobicity, but also has extremely low adhesion to water drops. Dropping on super-hydrophobic F-SiO2Water drops on the/PDMS @ PET mesh fabric roll off from the surface easily. This superhydrophobic state can be well explained by the cassie-baxter wetting model, in which air bubbles are trapped in valleys of coarse structure, greatly reducing the contact area of the solid surface with water droplets. When the super-hydrophobic F-SiO2When the/PDMS @ PET mesh was immersed in deionized water, the submerged portion became a mirror surface, as shown in FIG. 6 b. Due to the air pockets on the surface of the prepared mesh, the contact interface below the liquid surface is mainly a water-air interface, not a water-solid interface. Furthermore, by comparing the superhydrophobic F-SiO2The hydrophobicity of the/PDMS @ PET mesh (see fig. 6c) and the unmodified PET mesh (see fig. 6d) clearly observe that the unmodified PET mesh cannot reach a superhydrophobic state and droplets form hemispheres. Another interesting phenomenon is that the super-hydrophobic F-SiO2When the/PDMS @ PET mesh fabric is placed in deionized water, the buoyancy of the mesh fabric is greatly increased, so that the mesh fabric floats on the water surface. Accordingly, the water droplets may still remain spherical on the mesh surface, as shown in fig. 6 e. Furthermore F-SiO2The mesh pore size and non-wetting properties of the/PDMS @ PET mesh are influenced by each other as shown in FIG. 7. Apparently, F-SiO with six different pore diameters2the/PDMS @ PET can obtain excellent super-hydrophobic performance. Wherein, the apparent water CA on the surface of the mesh fabric is increased along with the continuous reduction of the pore diameter of the mesh fabric. This is mainly due to the fact that water droplets will be embedded into the superhydrophobic F-SiO2in the/PDMS @ PET mesh fabric, water drops can be stably supported in the mesh with a smaller water CA value, and conversely, the super-hydrophobic mesh with a smaller pore size is closer to a plane, so that super-hydrophobic F-SiO is caused2The water CA value of the/PDMS @ PET mesh was higher.
Oil-water separation efficiency test
Prepared super-hydrophobic F-SiO2the/PDMS @ PET mesh fabric can be used for separating oil-water mixtures of different types. It is worth mentioning that after being placed at room temperature for 30 days, the super-hydrophobicity and super-lipophilicity of the composite material are not obviously changed, and the composite material shows excellent stability. Due to super-hydrophobic F-SiO2the/PDMS @ PET mesh fabric has excellent super-hydrophobicity and super-lipophilicity and can be used as a selective filter membrane to realize oil-water separation. First, we will superhydrophobic F-SiO2PerPDMS @ PET netThe woven fabric was placed in a separating device, and then 60 ml of an oil-water mixture (10 ml of water and 50 ml of oil) was poured into a funnel using a glass rod. In the separation process, oil drops slowly pass through the super-hydrophobic F-SiO under the action of gravity2the/PDMS @ PET mesh was then collected. At the same time, water is also collected in the top container due to the superhydrophobicity. Subsequently, the separation efficiency was calculated by observing the volume change of the oil before and after collection:
Wherein V0is the volume of oil before separation, VcIs the volume of oil separated. In the initial stage, F-SiO is super-hydrophobic2the/PDMS @ PET mesh fabric has a somewhat low calculated separation efficiency for oil droplet adsorption and wetting of the collection container surface. Then, the oil is in the super-hydrophobic F-SiO2The adsorption on the PDMS @ PET mesh fabric reaches a saturated state, and the separation efficiency is improved to a stable level. In order to discuss the relationship between the oil-water separation efficiency and the mesh size, 6 types of super-hydrophobic F-SiO with different apertures are prepared2a/PDMS @ PET mesh of 0.25mm, 0.12mm, 0.075mm, 0.058mm, 0.048mm and 0.038mm, respectively. Oil-water separation experiments were subsequently performed. In order to ensure the objectivity and the accuracy of an experimental result, the same super-hydrophobic F-SiO is used2Experiments were performed on 5 different sets of oil-water mixtures on a/PDMS @ PET mesh fabric and the separation efficiency was calculated as shown in figure 8. The result shows that 6 groups of super-hydrophobic F-SiO with different pore diameters2The separation efficiency of the PDMS @ PET mesh fabric to the oil-water mixture is over 90 percent, and the maximum separation efficiency can reach 98 percent. Among them, as the mesh size of PET becomes smaller, the separation efficiency is generally improved, and different oil-water mixtures show the same tendency, as shown in fig. 9. However, we can clearly see that the superhydrophobic F-SiO with a pore size of 0.038mm2the/PDMS @ PET mesh showed a lower separation efficiency than the mesh with a pore size of 0.048 mm. This is in contrast to the superhydrophobic F-SiO2The trend of the water CA in the/PDMS @ PET mesh was reversed. Thus, it can be concluded that the superhydrophobic F-SiO2Mesh size of PDMS @ PET meshThe oil-water separation capability is influenced to a certain extent. Another phenomenon is that different types of oil in the oil-water mixture also result in different values of separation efficiency. This phenomenon is due to the oil and the superhydrophobic F-SiO2The degree of surface energy matching of the/PDMS @ PET mesh. Oils of different surface energies, i.e. chloroform (1.489 g/cm), were tested as a function of the type of oil3) N-decane (0.73 g/cm)3) Kerosene (0.8 g/cm)3) Octane (0.703 g/cm)3) And n-hexane (0.66 g/cm)3) Super-hydrophobic F-SiO with same aperture2Separation efficiency on a/PDMS @ PET mesh as shown in FIG. 10. The results show that the super-hydrophobic F-SiO2The separation efficiency of the PDMS @ PET mesh fabric to 5 oil-water mixtures is over 95 percent, and the separation efficiency to kerosene is the highest and is 98 percent.
Claims (1)
1. F-SiO2The nano-particle and PDMS modified PET mesh fabric is characterized in that the preparation method of the modified PET mesh fabric comprises the following steps:
(1) Hydrophobic F-SiO2Preparation of nanoparticles
Adding 3g of silicon dioxide nano particles into a mixed solution containing 4ml of ammonia water and 16ml of deionized water, and then carrying out ultrasonic treatment for 10 min; then, 0.6ml Perfluorodecyltriethoxysilane (PFDTES) was added to 80ml ethanol and magnetically stirred at room temperature for 60 min; then, dropwise adding the silicon dioxide suspension into the fluorosilane mixed solution, and continuously stirring at the temperature of 30-50 ℃ to ensure that the hydrolytic condensation reaction is complete; after the reaction is finished, cooling the mixture to room temperature, centrifuging the reaction product for 5-10min at the centrifugal speed of 8000-15000 r/min, washing with absolute ethyl alcohol, and centrifuging twice; then, the product obtained by centrifugation is dried for 12-24h in a vacuum environment at 50-80 ℃, and finally hydrophobic SiO is obtained2Nanoparticles, labelled F-SiO2Nanoparticles;
(2) Preparation of hydrophobic PDMS @ PET mesh fabric
placing the PET mesh fabric in deionized water and absolute ethyl alcohol for 15min, and respectively drying for 10min for later use; weighing 0.3g of PDMS and 0.03g of curing agent according to the mass ratio of 10: 1, adding 15ml of Tetrahydrofuran (THF), magnetically stirring for 5min, performing ultrasonic treatment for 20-30min, and dissolving to obtain solutions a and b respectively; then, mixing the two solutions to obtain a mixed PDMS solution; afterwards, putting the PET mesh fabric into the mixed PDMS solution and carrying out ultrasonic treatment for 30min, and then pre-curing the PET mesh fabric in an oven at 70-90 ℃ for 5-15min to obtain hydrophobic PDMS @ PET mesh fabric;
(3) Super-hydrophobic F-SiO2Preparation of/PDMS @ PET mesh fabric
0.1g F-SiO2Weighing the nano particles into 15ml of THF, ultrasonically dispersing for 30min, and immersing the hydrophobic PDMS @ PET mesh fabric into the F-SiO-containing solution2THF solution for 10-20 min; drying in an oven at 70-90 deg.C for 5 min; taking out the mesh fabric, and immersing again in the solution containing F-SiO2THF solution for 10-20min, and placing in oven at 70-90 deg.C for 1 hr; finally, preparing the super-hydrophobic F-SiO2a/PDMS @ PET mesh.
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| CN118374226A (en) * | 2024-06-24 | 2024-07-23 | 中国科学院西北生态环境资源研究院 | Preparation method of modified organosilicon super-hydrophobic material, preparation method of super-hydrophobic aggregate and self-adaptive cement-based material |
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