CN113384919B - Stress-induced surface wettability continuous-transition Janus composite film and preparation method and application thereof - Google Patents

Stress-induced surface wettability continuous-transition Janus composite film and preparation method and application thereof Download PDF

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CN113384919B
CN113384919B CN202110452397.8A CN202110452397A CN113384919B CN 113384919 B CN113384919 B CN 113384919B CN 202110452397 A CN202110452397 A CN 202110452397A CN 113384919 B CN113384919 B CN 113384919B
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CN113384919A (en
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胡路阳
张善美
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Anhui University of Science and Technology
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    • B01D17/02—Separation of non-miscible liquids
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    • D01F1/02—Addition of substances to the spinning solution or to the melt
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    • D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/88—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
    • D01F6/94—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of other polycondensation products
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    • D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
    • D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
    • D04H1/42—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties characterised by the use of certain kinds of fibres insofar as this use has no preponderant influence on the consolidation of the fleece
    • D04H1/4382—Stretched reticular film fibres; Composite fibres; Mixed fibres; Ultrafine fibres; Fibres for artificial leather
    • D04H1/43825—Composite fibres
    • D—TEXTILES; PAPER
    • D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
    • D04H1/70—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres
    • D04H1/72—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged
    • D04H1/728—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged by electro-spinning
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    • 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
    • D06M15/21—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
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    • 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
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
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    • 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 a Janus composite film with stress-induced surface wettability continuous transition, which comprises the following components in percentage by weight: the elastic membrane comprises a hydrophobic porous elastic membrane and a hydrophilic layer deposited on one surface of the hydrophobic porous elastic membrane, wherein the hydrophilic layer is obtained by wetting, drying and heat treatment of a ZIF-L layer through polyvinylpyrrolidone. The invention also discloses a preparation method of the Janus composite film with the stress-induced surface wettability continuously changed. The invention also discloses application of the stress-induced surface wettability continuous transition Janus composite film in oil-water separation. The invention has the characteristics of quick response to stress and continuous regulation and control of surface wettability through stress, and can regulate and control the flux of oil-water separation by controlling the strain magnitude when being used for oil-water separation.

Description

Stress-induced surface wettability continuous-transition Janus composite film and preparation method and application thereof
Technical Field
The invention relates to the technical field of Janus porous composite films, in particular to a stress-induced surface wettability continuous transition Janus composite film and a preparation method and application thereof.
Background
Over billions of years of development and evolution, animals and plants in nature create a variety of fascinating and surprising surfaces that provide well-defined micro/nano structures that achieve a variety of wettabilities from superhydrophilic to superhydrophobic. Inspired by these functional biological surfaces, a number of biomimetic surfaces with specific wettability were prepared and applied for self-cleaning, anti-icing, liquid transport, corrosion resistance and oil-water separation. However, most surfaces inspired by nature only have single wettability, and their functionality is limited. In general, surfaces with different wettabilities can be prepared by exploiting the synergy of surface layering structure and surface chemical composition. Thus, some smart surface materials are fabricated that have a response to light, pH, heat, gas, electric field, and electrolyte.
Although the development of these smart materials has attracted extensive attention, there are still some problems with their preparation and use. For example, a photoresponsive surface made of an inorganic material requires a relatively long time to recover its hydrophobic state. The synthesis of photoresponsive monomers is a tedious and expensive task, although photoresponsive polymer surfaces avoid time-consuming wettability conversion processes. For pH sensitive surfaces, most require triggering by a droplet with a specific pH or pre-wetting by an aqueous solution with a suitable pH. Similar to pH-responsive surfaces, in order to obtain the desired wettability, the gas-responsive surface needs to be triggered beforehand by gas stimulation or using water droplets that have been pretreated with a gas. If its responsive initial wettability is restored, additional thermal treatment or gas purging is required. Unlike the above-described stimulus, electric field triggering can achieve simple, ultrafast surface wettability control. But safety issues caused by high pressure require special attention. In addition, the stability of these smart responsive surfaces is also critical for repeated cycling. Therefore, it is a challenge to obtain a stable smart surface with a simple and fast response.
Disclosure of Invention
Based on the technical problems in the background art, the invention provides a stress-induced surface wettability continuous-transition Janus composite film, and a preparation method and application thereof.
The invention provides a stress-induced surface wettability continuous transition Janus composite film, which comprises the following components in percentage by weight: the hydrophobic porous elastic film comprises a hydrophobic porous elastic film and a hydrophilic layer deposited on one surface of the hydrophobic porous elastic film, wherein the hydrophilic layer is obtained by wetting, drying and heat treatment of a ZIF-L layer through polyvinylpyrrolidone.
The Janus membrane refers to a separation membrane with different properties (such as hydrophile/hydrophobe, polarity/nonpolar, positive charge/negative charge and the like) on two sides of the membrane.
ZIF-L is a Zn-utilizing compound 2+ And 2-methylimidazole according to a certain proportion to obtain the zeolite imidazolate framework material with a microporous structure. ZIF-L is a conventional material in the chemical field。
Preferably, the raw material of the hydrophobic porous elastic membrane is a mixture of an elastic polymer and a hydrophobic substance.
Preferably, the elastomeric polymer comprises polyurethane or the like.
Preferably, the hydrophobic material comprises silicone or the like.
Preferably, the siloxane comprises: <xnotran> , , , , , , , , , , , , , ,1H,1H,2H,2H- ,1H,1H,2H,2H- ,1H,1H,2H,2H- ,1H,1H,2H,2H- ,1H,1H,2H,2H- ,1H,1H,2H,2H- . </xnotran>
Preferably, the weight ratio of elastomeric polymer to hydrophobic substance is from 18 to 25.
Preferably, the heat treatment temperature is 130-180 ℃.
Preferably, the heat treatment time is 0.5 to 2 hours.
After the heat treatment, a treatment such as cleaning may be performed.
The invention also provides a preparation method of the Janus composite film with the stress-induced surface wettability continuously-converted, which comprises the following steps: floating the hydrophobic porous elastic film on the surface of a mixed solution containing zinc ions and 2-methylimidazole, and reacting to obtain a Janus film; and then wetting the hydrophilic surface of the Janus film by using a polyvinylpyrrolidone aqueous solution, drying, and then carrying out heat treatment to obtain the stress-induced surface wettability continuous transition Janus composite film.
The zinc ion can be selected from zinc nitrate, zinc acetate, zinc sulfate, zinc chloride, etc.
Preferably, the temperature of the reaction is 25-60 ℃.
Preferably, the reaction time is 0.25 to 3 hours.
Preferably, the molar ratio of zinc ions to 2-methylimidazole is from 0.01 to 0.06.
Preferably, the concentration of 2-methylimidazole is from 0.1 to 2.5mol/L.
Preferably, the drying temperature is room temperature.
Preferably, the mass fraction of the polyvinylpyrrolidone aqueous solution is 1 to 5wt%.
Preferably, the hydrophobic porous elastic film is electrospun.
The electrostatic spinning method can be as follows: preparing a siloxane and polyurethane mixed solution, and then carrying out electrostatic spinning; the mass fraction of the polyurethane can be 18-25wt%, and the solvent can be a mixed solvent of N, N dimethylformamide and tetrahydrofuran which have the same volume; the spinning voltage can be 15-25kV, and the spinning speed can be 0.3-2ml/h.
The water may be purified water, deionized water, etc.
The invention also provides application of the stress-induced surface wettability continuous transition Janus composite film in oil-water separation.
Has the advantages that:
stress stimulation response is a simple and quick method for adjusting the surface wettability, and the macroscopic deformation of the material causes the microstructure of the material to be obviously changed under the action of an external force, so that a potential condition is provided for the regulation and control of the surface wettability. Preparing a hydrophobic porous elastic film by using polyurethane and siloxane, depositing a hydrophilic ZIF-L layer on one surface of the film, wetting the hydrophilic surface of the film by using polyvinylpyrrolidone, drying and carrying out heat treatment to obtain a Janus composite film; the prepared Janus composite film has the characteristics of quick response to stress and continuous regulation and control of surface wettability through stress, and when the Janus composite film is used for oil-water separation, the flux of the oil-water separation can be regulated and controlled through controlling the strain; the polyvinylpyrrolidone is used for wetting the hydrophilic surface, and after drying and heat treatment, the polyvinylpyrrolidone-based hydrophilic surface material has good stress response performance; in addition, the preparation method has the advantages of simple preparation process, low cost and strong controllability.
Drawings
Fig. 1 is an optical photograph of a stress-induced surface wettability continuous-transition Janus composite film prepared in example 1.
Fig. 2 is an SEM photograph of the stress-induced surface wettability continuous transition Janus composite thin film prepared in example 1.
FIG. 3 is a graph showing the relationship between surface contact angles and stretching cycles under different strains after pre-stretching the stress-induced surface wettability continuous transition Janus composite film prepared in example 1.
FIG. 4 is a graph of the flux results for neat liquids of stress induced surface wettability continuous transition Janus composite films prepared in example 1, wherein Hexane is n-Hexane, petroleumether is petroleum ether, and Dodecanoe is n-Dodecane.
FIG. 5 is a graph showing the results of separating oil and water mixtures of the stress-induced surface wettability continuous-transition Janus composite film obtained in example 1, wherein Hexane is n-Hexane, petroleumether is petroleum ether, and Dodecanoe is n-Dodecane.
Fig. 6 is an SEM photograph of the stress-induced surface wettability continuous transition Janus composite film prepared in example 2.
Fig. 7 is an SEM photograph of the stress-induced surface wettability continuous transition Janus composite film prepared in example 3.
Detailed Description
The technical solution of the present invention will be described in detail below with reference to specific examples.
Example 1
A preparation method of a Janus composite film with continuously transformed surface wettability induced by stress comprises the following steps:
dissolving 2g of polyurethane in 4mL of tetrahydrofuran and 4mL of N, N dimethylformamide, stirring for 20 hours, adding octadecyl triethoxysilane (the mass fraction of the octadecyl triethoxysilane is 4 wt%), stirring overnight, then placing into an injector with a No. 25 needle, adjusting the voltage to be 18kV, and adjusting the spinning speed to be 1mL/h, and carrying out electrostatic spinning; peeling the collected film from the collector, drying at 60 ℃ for 12 hours under vacuum to obtain a hydrophobic porous elastic film, and then cutting;
floating the cut hydrophobic porous elastic film on the surface of a mixed aqueous solution of 25mmol/L zinc nitrate and 0.2 mol/L2-methylimidazole, preserving the temperature at 40 ℃ for 1 hour, washing with water, and drying to obtain a Janus film with a ZIF-L layer deposited on one surface;
and then wetting the hydrophilic surface of the Janus film by using a polyvinylpyrrolidone aqueous solution with the mass fraction of 2wt%, drying at room temperature, and then keeping the temperature at 150 ℃ for 1h to obtain the stress-induced surface wettability continuous transition Janus composite film.
The stress-induced surface wettability of the Janus composite film prepared in example 1 was continuously changed, and the results of the examination were shown in FIGS. 1 to 5.
FIG. 1 is an optical photograph of a stress-induced surface wettability continuous transition Janus composite film prepared in example 1; fig. 2 is an SEM photograph of the stress-induced surface wettability continuous transition Janus composite film prepared in example 1.
As can be seen from fig. 1-2: the Janus film can be prepared in a large size, the hydrophilic layer formed by the ZIF-L nanosheets is deposited on the surface of the polyurethane fibers, and the holes among the polyurethane fibers are filled with the ZIF-L nanosheets.
Fig. 3 is a relationship between surface contact angles and stretching cycles under different strains after pre-stretching the stress-induced surface wettability continuous transition Janus composite film prepared in example 1.
As can be seen from fig. 3: after the film is subjected to pre-stretching treatment, the surface contact angle of the film is increased along with the increase of strain, and after 50 stretching cycles, the change of the surface contact angle along with the strain is still consistent with that of the first stretching, and is not obviously changed.
FIG. 4 is a graph of flux results for neat liquids of stress induced surface wetting continuous transition Janus composite films prepared in example 1, where Hexane is n-Hexane, petroleumether is petroleum ether, and Dodecacan is n-Dodecane.
As can be seen from fig. 4: the flux of all liquids increases with increasing strain.
FIG. 5 is a graph showing the separation efficiency of oil and water mixtures of the Janus composite film with continuous transition of stress-induced surface wettability prepared in example 1, wherein Hexane is n-Hexane, petroleumether is petroleum ether, and Dodecacan is n-Dodecane.
As can be seen from fig. 5: the separation efficiency of all oil-water mixed liquid is higher than 98 percent.
Example 2
A preparation method of a Janus composite film with stress-induced surface wettability continuous transition comprises the following steps:
dissolving 2g of polyurethane in 4mL of tetrahydrofuran and 4mL of N, N dimethylformamide, stirring for 20 hours, adding octadecyl triethoxysilane (the mass fraction of the octadecyl triethoxysilane is 4 wt%), stirring overnight, then placing into an injector with a No. 25 needle, adjusting the voltage to be 18kV, and adjusting the spinning speed to be 1mL/h, and carrying out electrostatic spinning; peeling the collected film from the collector, drying at 60 ℃ for 12h under vacuum to obtain a hydrophobic porous elastic film, and then cutting;
floating the cut hydrophobic porous elastic film on the surface of a mixed aqueous solution of 25mmol/L zinc nitrate and 0.2 mol/L2-methylimidazole, preserving the temperature at 40 ℃ for 0.5h, washing with water, and drying to obtain a Janus film with a ZIF-L layer deposited on one surface;
and then wetting the hydrophilic surface of the Janus film by using a polyvinylpyrrolidone aqueous solution with the mass fraction of 2wt%, drying at room temperature, and then keeping the temperature at 150 ℃ for 1h to obtain the stress-induced surface wettability continuous transition Janus composite film.
Fig. 6 is an SEM photograph of the stress-induced surface wettability continuous transition Janus composite film prepared in example 2.
Example 3
A preparation method of a Janus composite film with stress-induced surface wettability continuous transition comprises the following steps:
dissolving 2g of polyurethane in 4mL of tetrahydrofuran and 4mL of N, N dimethylformamide, stirring for 20 hours, adding octadecyl triethoxysilane (the mass fraction of the octadecyl triethoxysilane is 4 wt%), stirring overnight, then placing into an injector with a No. 25 needle, adjusting the voltage to be 18kV, and adjusting the spinning speed to be 1mL/h, and carrying out electrostatic spinning; peeling the collected film from the collector, drying at 60 ℃ for 12h under vacuum to obtain a hydrophobic porous elastic film, and then cutting;
floating the cut hydrophobic porous elastic film on the surface of a mixed aqueous solution of 25mmol/L zinc nitrate and 0.2 mol/L2-methylimidazole, preserving the temperature at 40 ℃ for 1.5h, washing with water, and drying to obtain a Janus film with a ZIF-L layer deposited on one surface;
and then wetting the hydrophilic surface of the Janus film by using a polyvinylpyrrolidone aqueous solution with the mass fraction of 2wt%, drying at room temperature, and then preserving heat for 1h at 150 ℃ to obtain the stress-induced surface wettability continuous transition Janus composite film.
Fig. 7 is an SEM photograph of the stress-induced surface wettability continuous transition Janus composite film prepared in example 3.
Example 4
A preparation method of a Janus composite film with continuously transformed surface wettability induced by stress comprises the following steps:
dissolving 1.75g of polyurethane in 4mL of tetrahydrofuran and 4mL of N, N-dimethylformamide, stirring for 20h, adding 1H, 2H-perfluorododecyl trimethoxy silane (the mass fraction of which is 1wt percent), stirring overnight, then putting into a syringe with a No. 25 needle, adjusting the voltage to be 25kV and the spinning speed to be 2mL/h, and carrying out electrostatic spinning; peeling the collected film from the collector, drying at 60 ℃ for 12h under vacuum to obtain a hydrophobic porous elastic film, and then cutting;
floating the cut hydrophobic porous elastic film on the surface of a mixed aqueous solution of 10mmol/L zinc nitrate and 0.1 mol/L2-methylimidazole, preserving the temperature at 60 ℃ for 0.25h, cleaning and drying to obtain a Janus film with a ZIF-L layer deposited on one surface;
and then wetting the hydrophilic surface of the Janus film by using a polyvinylpyrrolidone aqueous solution with the mass fraction of 1wt%, drying at room temperature, and then preserving heat at 180 ℃ for 0.5h to obtain the stress-induced surface wettability continuous transition Janus composite film.
Example 5
A preparation method of a Janus composite film with stress-induced surface wettability continuous transition comprises the following steps:
dissolving 2.7g of polyurethane in 4mL of tetrahydrofuran and 4mL of N, N-dimethylformamide, stirring for 20h, adding 1H, 2H-perfluorooctyltriethoxysilane (the mass fraction of which is 10wt percent), stirring overnight, then placing into an injector with a No. 25 needle head, adjusting the voltage to be 15kV, and adjusting the spinning speed to be 0.3mL/h, and carrying out electrostatic spinning; peeling the collected film from the collector, drying at 60 ℃ for 12h under vacuum to obtain a hydrophobic porous elastic film, and then cutting;
floating the cut hydrophobic porous elastic film on the surface of a mixed aqueous solution of 60mmol/L zinc nitrate and 2.5 mol/L2-methylimidazole, preserving the temperature at 25 ℃ for 3 hours, cleaning, and drying to obtain a Janus film with a ZIF-L layer deposited on one surface;
and then wetting the hydrophilic surface of the Janus film by using a polyvinylpyrrolidone aqueous solution with the mass fraction of 5wt%, drying at room temperature, and then keeping the temperature at 130 ℃ for 2h to obtain the stress-induced surface wettability continuous transition Janus composite film.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered as the technical solutions and the inventive concepts of the present invention within the technical scope of the present invention.

Claims (14)

1. A stress-induced surface wettability continuous-transition Janus composite film, comprising: the hydrophobic porous elastic film comprises a hydrophobic porous elastic film and a hydrophilic layer deposited on one surface of the hydrophobic porous elastic film, wherein the hydrophilic layer is obtained by wetting, drying and heat treatment of a ZIF-L layer by polyvinylpyrrolidone;
the raw material of the hydrophobic porous elastic film is a mixture of an elastic polymer and a hydrophobic substance;
the hydrophobic material comprises a siloxane;
the elastomeric polymer comprises polyurethane.
2. The stress-induced surface wettability continuous transition Janus composite film of claim 1, wherein the siloxane comprises: <xnotran> , , , , , , , , , , , , , ,1H,1H,2H,2H- ,1H,1H,2H,2H- ,1H,1H,2H,2H- ,1H,1H,2H,2H- ,1H,1H,2H,2H- ,1H,1H,2H,2H- . </xnotran>
3. The stress-induced surface wettability continuous transition Janus composite film according to claim 1, wherein the weight ratio of the elastic polymer to the hydrophobic substance is from 18 to 25.
4. The stress-induced surface wettability continuous transition Janus composite film as claimed in claim 1, wherein the heat treatment temperature is 130-180 ℃.
5. The stress-induced surface wettability continuous transition Janus composite film as claimed in claim 1, wherein the heat treatment time is 0.5 to 2 hours.
6. A method for preparing a Janus composite film with continuously transformed stress-induced surface wettability as defined in any one of claims 1 to 5, comprising the steps of: floating the hydrophobic porous elastic film on the surface of a mixed solution containing zinc ions and 2-methylimidazole, and reacting to obtain a Janus film; and then, wetting the hydrophilic surface of the Janus film by using a polyvinylpyrrolidone aqueous solution, drying, and then carrying out heat treatment to obtain the stress-induced surface wettability continuous transition Janus composite film.
7. The method for preparing a stress-induced surface wettability continuous-transition Janus composite film according to claim 6, wherein the reaction temperature is 25-60 ℃.
8. The method for preparing a Janus composite film with the stress-induced surface wettability for continuous transition according to claim 6, wherein the reaction time is 0.25-3h.
9. The method for preparing a Janus composite film with continuous transition of stress-induced surface wettability as claimed in claim 6, wherein the molar ratio of zinc ions to 2-methylimidazole is 0.01-0.06.
10. The method for preparing a stress-induced surface wettability continuous-transition Janus composite film according to claim 6, wherein the concentration of 2-methylimidazole is 0.1-2.5mol/L.
11. The method for preparing a Janus composite film with the stress-induced surface wettability continuously-transformed as claimed in claim 6, wherein the drying temperature is room temperature.
12. The method for preparing a stress-induced surface wettability continuous-transition Janus composite film according to claim 6, wherein the mass fraction of the polyvinylpyrrolidone aqueous solution is 1-5wt%.
13. The method for preparing a stress-induced surface wettability continuous-transition Janus composite film according to claim 6, wherein the hydrophobic porous elastic film is prepared by electrospinning.
14. Use of the stress-induced surface-wetting continuous transition Janus composite film of any one of claims 1-5 for oil-water separation.
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