CN114369278B - Method for preparing super-hydrophobic porous material based on double-emulsion template - Google Patents
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Abstract
The invention discloses a method for preparing a super-hydrophobic porous material based on a double-emulsion template, which comprises the following steps of (1) dispersing a siloxane coupling agent, a hydrophilic emulsifier and an initiator in deionized water to obtain an emulsion template A; (2) Adding the emulsion template A into a high internal phase emulsion template B consisting of styrene, a cross-linking agent A, a cross-linking agent B and a lipophilic emulsifier, and stirring and emulsifying for 5-60min to obtain a double-emulsion template prepolymerization system; (3) And (3) reacting the double-emulsion template prepolymer system at 40-80 ℃ for 4-16h to obtain the super-hydrophobic porous material. The cross-linking agent A and the cross-linking agent B are respectively selected from one of divinylbenzene, triallyl isocyanurate, N-methylene bisacrylamide, trimethylolpropane triacrylate, ethylene glycol dimethacrylate and dipentaerythritol pentaacrylate. The porous material prepared by the invention can continuously separate an oil-water immiscible mixture and an oil-water emulsion with stable surfactant in a suction filtration mode.
Description
Technical Field
The invention relates to the technical field of material preparation, in particular to a method for preparing a super-hydrophobic porous material based on a double-emulsion template.
Background
Oil leakage incidents and the discharge of a large amount of industrial oily wastewater are increasing worldwide, and the leakage of canned and transported chemicals has already made a great threat to marine ecosystems and water quality safety. Therefore, the removal of organic pollutants from water has become an important and timely problem limiting environmental pollution. The traditional treatment methods, such as skimmer collection, addition of chemical dispersants, use of filter media and various adsorption materials, generally consume time and energy, and have the problems of low separation efficiency, secondary pollution and the like. The super-hydrophobic/super-oleophylic three-dimensional porous material developed based on the bionic strategy draws wide attention in the field of oil-water separation. The organic matter causing oil pollution includes not only light oil floating on the water surface, deposited heavy oil, but also emulsified oil droplets stabilized by a surfactant. The separation of oil and water emulsions presents significant challenges compared to immiscible oil and water mixtures. This is because the micro-sized emulsion droplets under the action of the surfactant have high stability and a complicated structure, and it is difficult to achieve effective aggregation. This makes developing simple, efficient, low-cost oil pollution treatment strategies faced with a number of challenges and challenges.
At present, various innovative super-wettability materials have been designed for efficient oil-water separation. Among these materials, three-dimensional porous materials such as melamine sponge, cellulose sponge, polyurethane sponge, metal foam, etc. are applied to oil-water separation after surface modification. Although the super-wetting foam is exquisite in design, the pore size of the base material cannot effectively intercept water drops in the micro-nano emulsion through the size sieving effect. A simple strategy for preparing the super-wetting three-dimensional porous material to directly realize oil-water emulsion separation still has great challenges. On the other hand, the surface modification process of the porous matrix material is complicated or the equipment is expensive, and even fluoride is used to reduce the surface energy, thereby causing secondary environmental pollution.
Disclosure of Invention
The invention aims to provide a novel method for preparing a super-hydrophobic porous material aiming at the problems of the existing porous material for oil-water emulsion separation, namely the super-hydrophobic porous material is prepared based on a double-emulsion template method.
The invention provides a method for preparing a super-hydrophobic porous material based on a double-emulsion template, which comprises the following steps:
(1) Dispersing a siloxane coupling agent, a hydrophilic emulsifier and an initiator in deionized water to obtain an emulsion template A.
(2) Adding the emulsion template A into a high internal phase emulsion template B consisting of styrene, a cross-linking agent A, a cross-linking agent B and a lipophilic emulsifier, and stirring and emulsifying for 5-60min to obtain a double-emulsion template prepolymerization system.
(3) Reacting the double-emulsion template prepolymer at 40-80 ℃ for 4-16h, cleaning the product with absolute ethyl alcohol, and then blowing and drying at 20-100 ℃ for 8-16h to obtain the super-hydrophobic porous material.
Wherein the siloxane coupling agent is one of vinyl triethoxysilane, gamma-aminopropyl triethoxysilane, gamma-glycidoxypropyl trimethoxysilane, gamma-methacryloxypropyl trimethoxysilane and vinyl tri (beta-methoxyethoxy) silane.
The hydrophilic emulsifier is one of sodium dodecyl sulfonate, hexadecyl trimethyl ammonium bromide, tween80, tween20, alkyl glucoside and alkylphenol polyoxyethylene polyoxypropylene ether APEP-105.
The initiator is one of sodium persulfate, ammonium persulfate, potassium persulfate, cumene hydroperoxide, azodiisobutyl amidine hydrochloride, a sodium persulfate/sodium bisulfite composite system and an ammonium persulfate/sodium bisulfite composite system.
The cross-linking agent A and the cross-linking agent B are different substances and are respectively selected from one of divinylbenzene, triallyl isocyanurate, N-methylene bisacrylamide, trimethylolpropane triacrylate, ethylene glycol dimethacrylate, dipentaerythritol pentaacrylate and urethane acrylate EBECRYL 284.
The lipophilic emulsifier is one of glycol fatty acid ester, MOA-3, MOA-5, oleate, span80, span60, polyoxyethylene sorbitol hexastearate and glyceryl monostearate.
Preferably, the proportion of the raw material components is as follows:
1-10 parts of siloxane coupling agent, 0.1-2 parts of hydrophilic emulsifier, 1-10 parts of initiator, 1000-3000 parts of deionized water, 10-50 parts of styrene, 10-50 parts of cross-linking agent A, 1-10 parts of cross-linking agent B and 1-20 parts of lipophilic emulsifier.
Compared with the prior art, the invention has the advantages that:
(1) According to the invention, a porous material is prepared by polymerizing a high internal phase emulsion template B consisting of styrene, a crosslinking agent A, a crosslinking agent B and a lipophilic emulsifier, a micro-nano structure and low surface energy modification are built in situ on a porous material skeleton by polymerizing an emulsion template A consisting of water, a hydrophilic emulsifier and a siloxane coupling agent, and the preparation of the super-hydrophobic porous material is realized by one step through a double-emulsion template method.
(2) The super-hydrophobic porous material is prepared in one step by a double-emulsion template method, so that the process is simple and the cost is low; and water is used as a dispersion medium, and toxic and harmful solvents are not used, so that the method accords with the trend of green, environment-friendly and sustainable development, and is expected to realize the macro preparation and marketization popularization of the material.
(3) The porous material prepared by the invention has excellent hydrophobic/oleophylic performance and reasonable pore size, can continuously separate an oil-water immiscible mixture and continuously separate an oil-water emulsion with stable surfactant in a suction filtration mode, and is expected to realize the application of the material in treating large-area water pollution.
Additional advantages, objects, and features of the invention will be set forth in part in the description which follows and in part will become apparent to those having ordinary skill in the art upon examination of the following or may be learned from practice of the invention.
Drawings
FIG. 1, SEM pictures of the products obtained in comparative example 1 and example 1.
FIG. 2 static water/oil contact Angle measurements of the products obtained in comparative example 1 and example 1.
Fig. 3, macroscopic hydrophobic/oleophilic properties of the porous material of example 1.
The super-hydrophobic porous material of fig. 4 and example 1 absorbs floating oil (light oil) on water and heavy oil deposited underwater.
The superhydrophobic porous material of fig. 5 and example 1 achieves continuous separation of oil-water immiscible mixture by suction filtration.
FIG. 6 shows that the super-hydrophobic porous material of example 1 realizes continuous separation of oil-water emulsion by suction filtration.
Detailed Description
The preferred embodiments of the present invention will be described in conjunction with the accompanying drawings, and it should be understood that they are presented herein only to illustrate and explain the present invention and not to limit the present invention.
Example 1
A method for preparing a super-hydrophobic porous material based on a double-emulsion template comprises the following steps: (1) Dispersing 2 parts by weight of gamma-aminopropyltriethoxysilane, 0.4 part by weight of sodium dodecyl sulfate and 2 parts by weight of initiator sodium persulfate in 2000 parts by weight of deionized water to obtain an emulsion template A containing a siloxane coupling agent, a hydrophilic emulsifier and an initiator. (2) 2004.4 weight portions of the emulsion template A are added into a high internal phase emulsion template B consisting of 30 weight portions of styrene, 15 weight portions of cross linker A divinyl benzene, 5 weight portions of cross linker B ethylene glycol dimethacrylate and 10 weight portions of lipophilic emulsifier Span80, and mechanically stirred and emulsified for 10min at 200r/min, so as to obtain a double emulsion template prepolymerization system consisting of the emulsion template A and the high internal phase emulsion template B. (3) And (3) reacting the double-emulsion template prepolymer system obtained in the step (2) at 65 ℃ for 8h, cleaning the product with absolute ethyl alcohol, and then drying by blowing at 50 ℃ for 12h to obtain the super-hydrophobic porous material.
Example 2
A method for preparing a super-hydrophobic porous material based on a double-emulsion template comprises the following steps: (1) Dispersing 10 parts by weight of gamma-aminopropyltriethoxysilane, 1 part by weight of hexadecyl trimethyl ammonium bromide and 2 parts by weight of initiator ammonium persulfate in 1000 parts by weight of deionized water to obtain an emulsion template A containing a siloxane coupling agent, a hydrophilic emulsifier and an initiator. (2) Adding 1013 parts by weight of the emulsion template A into a high internal phase emulsion template B consisting of 30 parts by weight of styrene, 10 parts by weight of cross-linking agent AN, N-methylene bisacrylamide, 10 parts by weight of cross-linking agent B trimethylolpropane triacrylate and 15 parts by weight of lipophilic emulsifier MOA-3, and mechanically stirring and emulsifying at 800r/min for 20min to obtain a double emulsion template prepolymerization system consisting of the emulsion template A and the high internal phase emulsion template B. (3) And (3) reacting the double-emulsion template prepolymer system obtained in the step (2) at 65 ℃ for 16h, cleaning the product with absolute ethyl alcohol, and then blowing and drying the product at 80 ℃ for 8h to obtain the super-hydrophobic porous material.
Example 3
A method for preparing a super-hydrophobic porous material based on a double-emulsion template comprises the following steps: (1) 1 part by weight of gamma-glycidoxypropyltrimethoxysilane, 0.2 part by weight of alkyl glucoside and 1 part by weight of initiator cumene hydroperoxide are dispersed in 2000 parts by weight of deionized water to obtain an emulsion template A containing a siloxane coupling agent, a hydrophilic emulsifier and an initiator. (2) Adding 2002.2 parts by weight of emulsion template A into a high internal phase emulsion template B consisting of 20 parts by weight of styrene, 20 parts by weight of cross-linking agent A ethylene glycol dimethacrylate, 10 parts by weight of cross-linking agent B dipentaerythritol pentaacrylate and 20 parts by weight of lipophilic emulsifier oleate, and mechanically stirring and emulsifying for 60min at 100r/min to obtain a double emulsion template prepolymerization system consisting of the emulsion template A and the high internal phase emulsion template B; (3) And (3) reacting the double-emulsion template prepolymer system obtained in the step (2) at 40 ℃ for 16h, cleaning the product with absolute ethyl alcohol, and then drying by blowing at 80 ℃ for 8-16h to obtain the super-hydrophobic porous material.
Example 4
A method for preparing a super-hydrophobic porous material based on a double-emulsion template comprises the following steps: (1) Dispersing 5 parts by weight of vinyltris (beta-methoxyethoxy) silane, 1 part by weight of a hydrophilic emulsifier (alkylphenol polyoxyethylene polyoxypropylene ether APEP-105) and 5 parts by weight of an initiator azobisisobutylamidine hydrochloride in 3000 parts by weight of deionized water to obtain an emulsion template A containing a siloxane coupling agent, the hydrophilic emulsifier and the initiator. (2) Adding 3011 parts by weight of the emulsion template A into a high internal phase emulsion template B consisting of 30 parts by weight of styrene, 10 parts by weight of a cross-linking agent A, urethane acrylate EBECRYL 284, 10 parts by weight of a cross-linking agent B, triallyl isocyanurate and 20 parts by weight of a lipophilic emulsifier, namely glyceryl monostearate, and mechanically stirring and emulsifying for 30min at 600r/min to obtain a double emulsion template prepolymerization system consisting of the emulsion template A and the high internal phase emulsion template B; (3) And (3) reacting the double-emulsion template prepolymer system obtained in the step (2) at 80 ℃ for 8h, cleaning the product with absolute ethyl alcohol, and then drying by blowing air at 80 ℃ for 8h to obtain the super-hydrophobic porous material.
Example 5
A method for preparing a super-hydrophobic porous material based on a double-emulsion template comprises the following steps: (1) 1 part by weight of gamma-methacryloxypropyltrimethoxysilane, 0.1 part by weight of hydrophilic emulsifier Tween80 and 2 parts by weight of initiator (sodium persulfate/sodium bisulfite composite system) are dispersed in 1000 parts by weight of deionized water to obtain an emulsion template A containing a siloxane coupling agent, the hydrophilic emulsifier and the initiator. (2) Adding 1003.1 parts by weight of emulsion template A into a high internal phase emulsion template B consisting of 19 parts by weight of styrene, 30 parts by weight of cross-linking agent A trimethylolpropane triacrylate, 1 part by weight of cross-linking agent B divinylbenzene and 5 parts by weight of lipophilic emulsifier polyoxyethylene sorbitol hexastearate, and mechanically stirring and emulsifying for 10min at 200r/min to obtain a double emulsion template prepolymerization system consisting of the emulsion template A and the high internal phase emulsion template B; (3) And (3) reacting the double-emulsion template prepolymer system obtained in the step (2) at 40 ℃ for 16h, cleaning the product with absolute ethyl alcohol, and then drying by blowing at 50 ℃ for 12h to obtain the super-hydrophobic porous material.
Comparative example 1
A preparation method of a porous material comprises the following steps: (1) 2 parts by weight of initiator sodium persulfate was dispersed in 2000 parts by weight of deionized water to obtain initiator-containing solution A. (2) Adding 2002 parts by weight of the solution A into a high internal phase emulsion template B consisting of 30 parts by weight of styrene, 15 parts by weight of cross-linking agent A divinylbenzene, 5 parts by weight of cross-linking agent B ethylene glycol dimethacrylate and 10 parts by weight of lipophilic emulsifier Span80, and mechanically stirring and emulsifying for 10min at 200r/min to obtain a prepolymerization system; (3) And (3) reacting the prepolymer system obtained in the step (2) at 65 ℃ for 8h, cleaning the product with absolute ethyl alcohol, and then drying the product by blowing air at 50 ℃ for 12h to obtain the porous material.
And (4) performance testing:
(1) Scanning Electron microscope Picture (SEM)
The morphology of the porous materials prepared in example 1 and comparative example 1 was analyzed by using a JSM-7500F scanning electron microscope, the acceleration voltage was 20.0KV, and before the sample was tested, the surface gold spraying treatment was performed. The test results are shown in FIG. 1. In the figure, a1 to a3 are porous materials of comparative example 1, and b1 to b3 are porous materials of example 1. The pore structure is a highly penetrated pore, and the pore diameter is 200nm-10 μm; the difference is that a plurality of nano-spheres are distributed on the pore framework in the embodiment 1, and the spheres are polymerized by the emulsion template A, so that the roughness is increased, and the hydrophobic property is favorably improved.
(2) Static contact Angle test (WCA/OCA)
The surface of the porous materials prepared in example 1 and comparative example 1 was subjected to Water Contact Angle (WCA) and Oil Contact Angle (OCA) tests using an OCA25 type tester of Dataphysics, germany. The results are shown in FIG. 2. In the figure, a, b are the static water/oil contact angles of the porous material of comparative example 1, c, d are the static water/oil contact angles of the porous material of example 1. It was confirmed that comparative example 1 is a hydrophobic/super oleophilic porous material and example 1 is a super hydrophobic/super oleophilic porous material. The emulsion template A is added and polymerized to form microspheres, so that the roughness is increased, and the further improvement of the hydrophobic property (WCA is increased by 8 degrees)
(3) Macroscopic hydrophobic/oleophilic Properties
Dyeing water with water-soluble pigments (methyl orange and bromophenol blue); petroleum ether was dyed with an oil-soluble pigment (oil Red O). The surface of the superhydrophobic porous material prepared in example 1 was subjected to a macro hydrophobic/oleophilic property test. The test results are shown in FIG. 3. Indicating that the oil-water separation capability is realized.
(4) The superhydrophobic porous material prepared in example 1 was subjected to a separated light oil (heavy oil)/water test. The specific test method comprises the following steps: the porous material of example 1 in a block form was used as an oil-absorbing material, and the material was held by tweezers and put into light oil (petroleum ether was stained with oil red O) on the water surface to carry out an oil-absorbing operation, as shown in FIG. 4 a. The porous material of example 1 was further used as an oil-absorbing material in a lump form, and the oil-absorbing material was placed in underwater heavy oil (chloroform was stained with oil red O) while being held by tweezers, as shown in FIG. 4 b. It can be seen that the porous material of the present invention can separate light oil and heavy oil in water.
(5) The superhydrophobic porous material prepared in example 1 was subjected to a continuous separation light oil (heavy oil)/water test by a pump. The specific test method comprises the following steps: the water inlet of the pump was connected to an oil absorbent material (porous material of example 1) which extended into a graduated cylinder filled with water, light oil and heavy oil, the liquid in the graduated cylinder, the light oil being on the water surface, the heavy oil being at the bottom of the graduated cylinder, the middle being water. The water outlet of the pump is connected with another measuring cylinder as an oil collecting device. The oil absorption material realizes continuous collection of light oil on the water surface (petroleum ether is dyed by oil red O)/heavy oil under water (trichloromethane is dyed by oil red O) by a pump (see figure 5).
(6) The superhydrophobic porous material prepared in example 1 was subjected to an oil-water emulsion separation test. The specific test method comprises the following steps: (1) preparing an oil-water emulsion: at V Water (I) ：V Toluene =1: under the condition of 50, 1g/L of Span80 surfactant is added, and the mixture is stirred for 1 hour at the speed of 600r/min, so that the stable water-in-oil emulsion is obtained. (2) oil-water emulsion separation: as shown in fig. 6a, one end of the pump is connected to the oil absorbing material (porous material of example 1) and the other end of the pump is connected to a beaker (oil collecting device). Oil absorptionThe material is continuously collected by a pump. Observing the liquid before and after separation by using an eyepiece-free inverted fluorescence digital microscope, wherein a plurality of liquid drops exist in the cream-white water-in-oil emulsion before separation as shown in figure 6 b; however, a clear oil phase was obtained after separation, and no droplets were observed in the filtrate after separation.
Although the present invention has been described with reference to a preferred embodiment, it should be understood that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (8)
1. A method for preparing a super-hydrophobic porous material based on a double-emulsion template is characterized in that the super-hydrophobic porous material is prepared by in-situ polymerization of an emulsion template A and a high internal phase emulsion template B under the action of an initiator; the emulsion template A is prepared from water, a hydrophilic emulsifier and a siloxane coupling agent; the high internal phase emulsion template B is prepared from styrene, a cross-linking agent A, a cross-linking agent B and a lipophilic emulsifier.
2. The method for preparing the superhydrophobic porous material based on the double emulsion template according to claim 1, wherein the cross-linking agent a and the cross-linking agent B are different substances, and are selected from one of divinylbenzene, triallyl isocyanurate, N-methylenebisacrylamide, trimethylolpropane triacrylate, ethylene glycol dimethacrylate, dipentaerythritol pentaacrylate, urethane acrylate EBECRYL 284.
3. The method for preparing the superhydrophobic porous material based on the double emulsion template as claimed in claim 1, wherein the steps are as follows:
(1) Dispersing a siloxane coupling agent, a hydrophilic emulsifier and an initiator in deionized water to obtain an emulsion template A;
(2) Adding the emulsion template A into a high internal phase emulsion template B consisting of styrene, a cross-linking agent A, a cross-linking agent B and a lipophilic emulsifier, and stirring and emulsifying for 5-60min to obtain a double-emulsion template prepolymerization system;
(3) Reacting the double-emulsion template prepolymer system at 40-80 ℃ for 4-16h, cleaning the product with absolute ethyl alcohol, and then drying by blowing air at 20-100 ℃ for 8-16h to obtain the super-hydrophobic porous material.
4. The method for preparing a superhydrophobic porous material based on a double emulsion template as claimed in claim 3, wherein the siloxane coupling agent is one of vinyltriethoxysilane, gamma-aminopropyltriethoxysilane, gamma-glycidoxypropyltrimethoxysilane, gamma-methacryloxypropyltrimethoxysilane, vinyltris (beta-methoxyethoxy) silane.
5. The method for preparing the superhydrophobic porous material based on the double emulsion template as claimed in claim 3, wherein the hydrophilic emulsifier is one of sodium dodecyl sulfate, cetyl trimethyl ammonium bromide, tween80, tween20, alkyl glucoside, alkylphenol polyoxyethylene polyoxypropylene ether APEP-105.
6. The method for preparing the superhydrophobic porous material based on the double emulsion template of claim 3, wherein the lipophilic emulsifier is one of glycol fatty acid ester, MOA-3, MOA-5, oleate, span80, span60, polyoxyethylene sorbitol hexastearate, glyceryl monostearate.
7. The method for preparing the superhydrophobic porous material based on the double emulsion template as claimed in claim 3, wherein the initiator is one of sodium persulfate, ammonium persulfate, potassium persulfate, cumene hydroperoxide, azobisisobutylamidine hydrochloride, a sodium persulfate/sodium bisulfite complex system, and an ammonium persulfate/sodium bisulfite complex system.
8. A superhydrophobic porous material, characterized by being prepared by the preparation method of any one of claims 1-7.
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| CN202210076717.9A CN114369278B (en) | 2022-01-24 | 2022-01-24 | Method for preparing super-hydrophobic porous material based on double-emulsion template |
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| CN202210076717.9A CN114369278B (en) | 2022-01-24 | 2022-01-24 | Method for preparing super-hydrophobic porous material based on double-emulsion template |
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| CN114369278B true CN114369278B (en) | 2023-01-31 |
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| WO2004005355A1 (en) * | 2002-07-09 | 2004-01-15 | Galip Akay | Microporous polymers |
| CN103435731A (en) * | 2013-08-30 | 2013-12-11 | 中国科学技术大学 | Preparation method of porous polymer microspheres |
| CN105664897A (en) * | 2016-02-29 | 2016-06-15 | 中国科学院兰州化学物理研究所 | Method for preparing magnetic porous microsphere adsorbing material by utilizing O/W/O double emulsion template |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2004005355A1 (en) * | 2002-07-09 | 2004-01-15 | Galip Akay | Microporous polymers |
| CN103435731A (en) * | 2013-08-30 | 2013-12-11 | 中国科学技术大学 | Preparation method of porous polymer microspheres |
| CN105664897A (en) * | 2016-02-29 | 2016-06-15 | 中国科学院兰州化学物理研究所 | Method for preparing magnetic porous microsphere adsorbing material by utilizing O/W/O double emulsion template |
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