CN114369191A - Preparation method of super-hydrophobic polystyrene porous material - Google Patents
Preparation method of super-hydrophobic polystyrene porous material Download PDFInfo
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F212/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring
- C08F212/02—Monomers containing only one unsaturated aliphatic radical
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- C08F222/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a carboxyl radical and containing at least one other carboxyl radical in the molecule; Salts, anhydrides, esters, amides, imides, or nitriles thereof
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- C08J2325/02—Homopolymers or copolymers of hydrocarbons
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- C08J2435/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a carboxyl radical, and containing at least one other carboxyl radical in the molecule, or of salts, anhydrides, esters, amides, imides or nitriles thereof; Derivatives of such polymers
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Abstract
The invention discloses a preparation method of a super-hydrophobic polystyrene-based porous material, which is prepared by styrene, a cross-linking agent and a low surface energy modifier through in-situ polymerization under the action of an initiator, water and a lipophilic emulsifier. The low surface energy modifier is one of a combination of poly (dimethyl-methyl vinyl siloxane) and poly (dimethyl-methyl hydrogen siloxane), a combination of vinyl terminated poly (dimethyl siloxane) and trimethylsilyl terminated poly (dimethyl siloxane) -co-methyl hydrogen siloxane, a combination of hydroxyl terminated dimethyl siloxane and methyl triacetoxysilane, and a combination of allyl silicon terminated dimethyl siloxane and octamethyl tetrasiloxane. The porous material prepared by the invention has excellent hydrophobic property and oleophylic property, and can continuously separate an oil-water immiscible mixture and an oil-water emulsion with stable surfactant by a suction filtration mode.
Description
Technical Field
The invention relates to the technical field of porous materials, in particular to a preparation method of a super-hydrophobic polystyrene-based porous material.
Background
Frequent oil leakage accidents and the discharge of a large amount of industrial oily wastewater cause serious environmental pollution and huge economic loss. The traditional oily wastewater treatment method (chemical reagent dispersion, centrifugation, field incineration, skimmer collection) usually consumes a large amount of energy and has the problems of low separation efficiency, secondary pollution and the like. The super-hydrophobic/super-oleophylic material developed based on the bionic strategy can effectively realize oil-water separation through filtration, and becomes a research hotspot in the field of oil pollution treatment.
At present, researchers have developed a series of oil-water separation materials with special wetting functions in laboratories, such as polymer films, inorganic films, ultrathin carbon nanowires, metal filter screen films, modified sponges, metal foams, metal particles, and the like. Compared with metal matrix and carbon material matrix, the oil-water separation material using the polymer as the matrix draws more attention by the advantages of wide selectivity of the matrix, excellent corrosion resistance, diversified modification methods, adjustable comprehensive performance and the like. Meanwhile, when the wettability material with a pore structure is prepared by means of electrostatic spinning, freeze drying, 3D printing, chemical surface modification, physical coating and the like, the wettability material has defects of different degrees in the aspects of preparation cost, use scale, production period, separation flux, material stability, material service life and the like.
The high internal phase emulsion template method is to take the continuous phase of the high internal phase emulsion as a polymeric phase and the disperse phase as a pore-forming template, carry out polymerization reaction at a certain temperature, and obtain the polymer material with a porous structure after the polymerization is finished and the washing and the drying are carried out. The high internal phase emulsion template method has the advantages of capability of accurately regulating and controlling the size and distribution of the diameters of the holes and the channels, easiness in process adjustment, relatively mild reaction conditions, low requirement on equipment, low cost, short period and the like, and is favorable for macro preparation and marketization popularization and application of materials.
Disclosure of Invention
The invention aims to provide a preparation method of a super-hydrophobic polystyrene-based porous material, which has the advantages of simple process, easy process adjustment and low cost.
The preparation method of the super-hydrophobic polystyrene-based porous material provided by the invention is characterized in that styrene, a cross-linking agent and a low surface energy modifier are subjected to in-situ polymerization under the action of an initiator, water and a lipophilic emulsifier to prepare the super-hydrophobic polystyrene-based porous material.
The low surface energy modifier is a combination of two polydimethylsiloxanes. Preferably, the low surface energy modifier is one of a combination of poly (dimethyl-methylvinylsiloxane) and poly (dimethyl-methylhydrogensiloxane), a combination of vinyl-terminated poly (dimethylsiloxane) and trimethylsilyl-terminated poly (dimethylsiloxane) -copolymethyl-hydrogensiloxane, a combination of hydroxy-terminated polydimethylsiloxane and methyltriacetoxysilane, a combination of allyl-terminated polydimethylsiloxane and octamethyltetrasiloxane.
The cross-linking agent is one of divinylbenzene, triallyl isocyanurate, pentaerythritol triacrylate, trimethylolpropane triacrylate, ethylene glycol dimethacrylate and dipentaerythritol pentaacrylate.
The initiator is one of sodium persulfate, ammonium persulfate, cumene hydroperoxide, azodiisobutyl amidine hydrochloride, a sodium persulfate/sodium bisulfite composite system and an ammonium persulfate/sodium bisulfite composite system.
The lipophilic emulsifier is one of glycol fatty acid ester, MOA-3, MOA-5, oleate, Span80, Span60, polyoxyethylene sorbitol hexastearate and glyceryl monostearate.
The preparation method comprises the following steps:
(1) 1-20 parts by weight of initiator is dissolved in 1000-3000 parts by weight of deionized water to obtain an initiator solution A.
(2) Adding the initiator solution A into a mixed solution B consisting of 10-60 parts by weight of styrene, 10-50 parts by weight of cross-linking agent, 1-10 parts by weight of low surface energy modifier and 5-30 parts by weight of lipophilic emulsifier, and mechanically stirring and emulsifying for 5-60min at the speed of 200-1000r/min to obtain a prepolymerization system.
(3) And (3) reacting the prepolymer system obtained in the step (2) at the temperature of 20-80 ℃ for 4-24h, cleaning the product with absolute ethyl alcohol, and then blowing and drying at the temperature of 40-100 ℃ for 8-24h to obtain the super-hydrophobic polystyrene-based porous material.
Compared with the prior art, the invention has the advantages that:
(1) the porous material prepared by the invention has excellent hydrophobic property and oleophylic property, and can continuously separate an oil-water immiscible mixture and an oil-water emulsion with stable surfactant by a suction filtration mode. The application of the material in treating large-area water pollution is expected to be realized.
(2) The super-hydrophobic porous material is prepared by a one-step 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 conforms to the trend of green, environment-friendly and sustainable development. By adjusting factors such as the adding proportion of the components of the initiator and the monomers, the mechanical stirring speed, the emulsification time and the like, the mechanical property and the microstructure of a target product, the hydrophobic property and the oil-water emulsion separation property are controlled, so that a new experimental technical route is provided for the super-hydrophobic porous material for the oil-water emulsion separation. Hopefully realizing the macro preparation and the marketization popularization of the material.
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 is a static contact angle of comparative examples 1 to 3 with the product obtained in example 1.
FIG. 2 is a scanning electron microscope photograph of the superhydrophobic polystyrene-based porous material prepared in example 1.
Fig. 3 is a water/oil contact angle and a macroscopic hydrophobic/oleophilic property of the super-hydrophobic polystyrene-based porous material prepared in example 1.
FIG. 4 shows that the super-hydrophobic polystyrene-based porous material prepared in example 1 can separate oil and water under conditions of light oil on water, heavy oil under water and turbulent flow.
FIG. 5 is a separation efficiency test of petroleum ether for the polystyrene-based porous materials prepared in comparative examples 1 to 3 and example 1.
FIG. 6 shows that the super-hydrophobic polystyrene-based porous material prepared in example 1 can be subjected to suction filtration to realize continuous separation of immiscible oil-water mixture.
FIG. 7 shows that the super-hydrophobic polystyrene-based porous material prepared in example 1 is subjected to suction filtration to realize continuous separation of oil-water emulsion.
Detailed Description
The preferred embodiments of the present invention will be described in conjunction with the accompanying drawings, and it will be understood that they are described herein for the purpose of illustration and explanation and not limitation.
Example 1
A super-hydrophobic polystyrene-based porous material is prepared by the following steps: (1) dispersing 2 parts by weight of sodium persulfate in 2000 parts by weight of deionized water to obtain a solution A containing sodium persulfate; (2) adding 2002 parts by weight of the solution A into a mixed solution B consisting of a two-component low-surface-energy modifier consisting of 30 parts by weight of styrene, 20 parts by weight of divinyl benzene, 4 parts by weight of poly (dimethyl-methyl vinyl siloxane) and 0.4 part by weight of poly (dimethyl-methyl hydrogen siloxane) and 15 parts by weight of Span80 lipophilic emulsifier, and mechanically stirring and emulsifying at 200r/min for 10min 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 10h to obtain the super-hydrophobic polystyrene-based porous material.
Example 2:
a super-hydrophobic polystyrene-based porous material is prepared by the following steps: (1) dispersing 2 parts by weight of azobisisobutylamidine hydrochloride into 1000 parts by weight of deionized water to obtain a solution A containing the azobisisobutylamidine hydrochloride; (2) adding 1002 parts by weight of the solution A into a mixed solution B consisting of a two-component low-surface-energy modifier consisting of 30 parts by weight of styrene, 20 parts by weight of divinyl benzene, 4 parts by weight of vinyl-terminated poly (dimethyl siloxane) and 0.4 part by weight of trimethylsilyl-terminated poly (dimethyl siloxane) -co-methyl-hydrogen siloxane and 15 parts by weight of Span80 lipophilic emulsifier, and mechanically stirring and emulsifying at 600r/min for 10min to obtain a prepolymerization system; (3) and (3) reacting the prepolymer system obtained in the step (2) at 40 ℃ for 24h, cleaning the product with absolute ethyl alcohol, and then drying the product by blowing air at 80 ℃ for 24h to obtain the super-hydrophobic polystyrene-based porous material.
Example 3:
a super-hydrophobic polystyrene-based porous material is prepared by the following steps: (1) dispersing 20 parts by weight of cumene hydroperoxide in 2000 parts by weight of deionized water to obtain solution A containing the cumene hydroperoxide; (2) adding 2020 parts by weight of the solution A into a mixed solution B consisting of 20 parts by weight of styrene, 30 parts by weight of pentaerythritol triacrylate, 10 parts by weight of a two-component low surface energy modifier consisting of hydroxyl-terminated polydimethylsiloxane and 1 part by weight of methyltriacetoxysilane and 10 parts by weight of a glycol fatty acid ester lipophilic emulsifier, and mechanically stirring and emulsifying for 30min at 200r/min to obtain a prepolymerization system; (3) and (3) reacting the prepolymer system obtained in the step (2) at 80 ℃ for 8h, cleaning the product with absolute ethyl alcohol, and then drying the product by blowing air at 100 ℃ for 10h to obtain the super-hydrophobic polystyrene-based porous material.
Example 4:
super-hydrophobic polystyrene baseThe pore material is prepared by the following steps: (1) 2 parts by weight of sodium persulfate/sodium bisulfite (w)Sodium persulfate:wSodium bisulfite1:1) in 3000 parts by weight of deionized water to obtain a solution A containing a sodium persulfate/sodium bisulfite composite system; (2) adding 3002 parts by weight of the solution A into a mixed solution B consisting of 30 parts by weight of styrene, 10 parts by weight of ethylene glycol dimethacrylate, 2 parts by weight of a bicomponent low surface energy modifier consisting of allyl silicon-based end-capped polydimethylsiloxane and 0.2 part by weight of octamethyltetrasiloxane and 30 parts by weight of oleate lipophilic emulsifier, and mechanically stirring and emulsifying for 5min at 1000r/min to obtain a prepolymerization system; (3) and (3) reacting the prepolymer system obtained in the step (2) at 40 ℃ for 16h, cleaning the product with absolute ethyl alcohol, and then drying by blowing at 40 ℃ for 24h to obtain the super-hydrophobic polystyrene-based porous material.
Example 5:
a super-hydrophobic polystyrene-based porous material is prepared by the following steps: (1) dispersing 20 parts by weight of ammonium persulfate/sodium bisulfite in 2000 parts by weight of deionized water to obtain solution A containing an ammonium persulfate/sodium bisulfite composite system; (2) adding 2020 parts by weight of the solution A into a mixed solution B consisting of 30 parts by weight of styrene, 20 parts by weight of triallyl isocyanurate, 2 parts by weight of a two-component low surface energy modifier consisting of allyl silicon-based end-capped polydimethylsiloxane and 0.2 part by weight of octamethyltetrasiloxane and 15 parts by weight of a glyceryl monostearate lipophilic emulsifier, and mechanically stirring and emulsifying at 600r/min for 10min to obtain a prepolymerization system; (3) and (3) reacting the prepolymer system obtained in the step (2) at 65 ℃ for 4h, cleaning the product with absolute ethyl alcohol, and then drying the product by blowing air at 50 ℃ for 10h to obtain the super-hydrophobic polystyrene-based porous material.
Comparative example 1:
a polystyrene-based porous material without a low surface energy modifier is prepared by the following steps: (1) dispersing 2 parts by weight of sodium persulfate in 2000 parts by weight of deionized water to obtain a solution A containing sodium persulfate; (2) adding 2002 parts by weight of the solution A into a mixed solution B consisting of 30 parts by weight of styrene, 20 parts by weight of dipentaerythritol pentaacrylate and 15 parts by weight of Span80 lipophilic emulsifier, 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 10h to obtain the polystyrene-based porous material.
Comparative example 2
A single-component polystyrene-based porous material with a low surface energy modifier is prepared by the following steps: (1) dispersing 2 parts by weight of sodium persulfate in 2000 parts by weight of deionized water to obtain a solution A containing sodium persulfate; (2) adding 2002 parts by weight of the solution A into a mixed solution B consisting of 30 parts by weight of styrene, 20 parts by weight of divinyl benzene, 4.4 parts by weight of single-component low-surface-energy modifier consisting of poly (dimethyl-methylhydrogensiloxane) and 15 parts by weight of Span80 lipophilic emulsifier, 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 10h to obtain the super-hydrophobic polystyrene-based porous material.
Comparative example 3
A single-component polystyrene-based porous material with a low surface energy modifier is prepared by the following steps: (1) dispersing 2 parts by weight of sodium persulfate in 2000 parts by weight of deionized water to obtain a solution A containing sodium persulfate; (2) adding 2002 parts by weight of the solution A into a mixed solution B consisting of 30 parts by weight of styrene, 20 parts by weight of divinyl benzene, 4.4 parts by weight of poly (dimethyl-methyl vinyl siloxane) single-component low-surface-energy modifier and 15 parts by weight of Span80 lipophilic emulsifier, 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 10h to obtain the super-hydrophobic polystyrene-based porous material.
The performance test was as follows:
(1) static contact Angle test (WCA/OCA): the test was carried out by using a tester model OCA25 from Dataphysics, Germany, to measure the Water Contact Angle (WCA) and the Oil Contact Angle (OCA) of the surface of the super-hydrophobic polystyrene-based porous material prepared in example 1. The test results are shown in FIG. 1.
(2) Scanning Electron Microscopy (SEM): the morphology of the super-hydrophobic polystyrene-based porous material prepared in example 1 was analyzed by a JSM-7500F scanning electron microscope with an acceleration voltage of 20.0KV, and before the sample was tested, a surface gold-spraying treatment was performed, and the test results are shown in fig. 2.
(3) Macroscopic hydrophobic/lipophilic property test: dyeing water with a water-soluble pigment (brilliant green); petroleum ether was dyed with an oil-soluble pigment (oil Red O). The surface of the super-hydrophobic polystyrene-based porous material prepared in example 1 was subjected to a macro-hydrophobic/oleophilic property test. The test results are shown in FIG. 3.
(4) Macroscopic oil-water separation test
Petroleum ether and chloroform were dyed with an oil-soluble pigment (oil red O). As shown in fig. 4, the superhydrophobic polystyrene-based porous material prepared in example 1 was subjected to oil-water separation by simulated turbulence under agitation with light oil/water, heavy oil/water, and a, b, and c are separation diagrams under agitation with light oil/water, heavy oil/water, petroleum ether, and water, respectively.
(5) Separation efficiency test
The polystyrene-based porous materials prepared in comparative examples 1 to 3 and example 1 were used as oil absorbing materials, and oil-water immiscible liquid separation efficiency tests were conducted by a pump. The specific test method comprises the following steps: the water inlet of the pump is connected with the oil absorption material, and the water outlet of the pump is connected with a beaker (used as an oil collection device). 50g of deionized water, 50g of petroleum ether were weighed into a beaker. The oil absorbing material is continuously separated from the petroleum ether/water immiscible liquid by means of a pump. After complete separation, the mass m of water in the beaker is weighed1. Separation efficiency of oil-water immiscible liquid m 1100% of the total weight of the composition. The test results are shown in FIG. 5.
(6) The super-hydrophobic polystyrene-based 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 is connected with an oil absorption material (the porous material prepared in the embodiment 1 of the invention is used as the oil absorption material), and the water outlet of the pump is connected with a beaker and used as an oil collection device. The oil-absorbing material realizes continuous collection of light oil on the water surface (petroleum ether is dyed by oil red O) and heavy oil underwater (trichloromethane is dyed by oil red O) by a pump (see figure 6).
(7) The super-hydrophobic polystyrene-based 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: a surfactant-stabilized water-in-oil emulsion (water/petroleum ether) was prepared at VWater (W)：VOil1: under the condition of 99, 5g/L of Span80 surfactant is added, and the mixture is stirred for 3 hours at 1500r/min, so that the stable water-in-oil emulsion is obtained. (2) Oil-water emulsion separation: the water inlet of the pump is connected with an oil absorption material (the porous material prepared in the embodiment 1 of the invention is used as the oil absorption material), and the water outlet of the pump is connected with a beaker which is used as an oil collection device. The oil-absorbing material is pumped to continuously collect the oil-water emulsion as shown in figure 7 a. Observing the liquid before and after separation by using an eyepiece-free inverted fluorescence digital microscope, wherein a plurality of liquid drops are in the cream-white water-in-oil emulsion before separation as shown in figure 7 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 preparation method of a super-hydrophobic polystyrene-based porous material is characterized in that styrene, a cross-linking agent and a low surface energy modifier are subjected to in-situ polymerization under the action of an initiator, water and a lipophilic emulsifier to prepare the super-hydrophobic polystyrene-based porous material; the low surface energy modifier is a combination of two polydimethylsiloxanes.
2. The method of preparing a superhydrophobic polystyrene-based porous material of claim 1, wherein the low surface energy modifier is one of a combination of poly (dimethyl-methyl vinyl siloxane) and poly (dimethyl-methyl hydrogen siloxane), a combination of vinyl-terminated poly (dimethyl siloxane) and trimethylsilyl-terminated poly (dimethyl siloxane) -co-methyl-hydrogen siloxane, a combination of hydroxy-terminated polydimethylsiloxane and methyl triacetoxysilane, and a combination of allyl silicon-terminated polydimethylsiloxane and octamethyl tetrasiloxane.
3. The method for preparing a superhydrophobic polystyrene-based porous material according to claim 1, comprising the steps of:
(1) dissolving an initiator in deionized water to obtain an initiator solution A;
(2) adding the initiator solution A into a mixed solution B consisting of styrene, a cross-linking agent, a low-surface-energy modifier and a lipophilic emulsifier, and stirring and emulsifying for 5-60min to obtain a prepolymerization system;
(3) and (3) reacting the prepolymer system obtained in the step (2) at the temperature of 20-80 ℃ for 4-24h, cleaning the product with absolute ethyl alcohol, and then blowing and drying at the temperature of 40-100 ℃ for 8-24h to obtain the super-hydrophobic polystyrene-based porous material.
4. The method of preparing a superhydrophobic polystyrene-based porous material according to claim 3, wherein the crosslinking agent is one of divinylbenzene, triallyl isocyanurate, pentaerythritol triacrylate, trimethylolpropane triacrylate, ethylene glycol dimethacrylate, dipentaerythritol pentaacrylate.
5. The method of preparing a superhydrophobic polystyrene-based porous material according to claim 3, wherein the initiator is one of sodium persulfate, ammonium persulfate, cumene hydroperoxide, azobisisobutylamidine hydrochloride, a sodium persulfate/sodium bisulfite complex system, and an ammonium persulfate/sodium bisulfite complex system.
6. The method for preparing a superhydrophobic polystyrene-based porous material according to claim 3, wherein the lipophilic emulsifier is one of ethylene glycol fatty acid ester, MOA-3, MOA-5, oleate, Span80, Span60, polyoxyethylene sorbitol hexastearate, and glyceryl monostearate.
7. The method for preparing a superhydrophobic polystyrene-based porous material according to claim 3, wherein the raw materials are used in the following ratio:
1-20 parts of initiator, 3000 parts of deionized water, 10-60 parts of styrene, 10-50 parts of cross-linking agent, 1-10 parts of low surface energy modifier and 5-30 parts of lipophilic emulsifier.
8. A superhydrophobic polystyrene-based porous material, characterized by being prepared by the preparation method according to any one of claims 1 to 7.
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Cited By (2)
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| CN115010986A (en) * | 2022-07-11 | 2022-09-06 | 西南石油大学 | Super-hydrophobic modified melamine foam and preparation method and application thereof |
| CN116948109A (en) * | 2023-09-19 | 2023-10-27 | 西南石油大学 | Porous material for sewage treatment of photovoltaic industry chain and preparation method thereof |
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| CN116948109A (en) * | 2023-09-19 | 2023-10-27 | 西南石油大学 | Porous material for sewage treatment of photovoltaic industry chain and preparation method thereof |
| CN116948109B (en) * | 2023-09-19 | 2024-01-09 | 西南石油大学 | Porous material for sewage treatment of photovoltaic industry chain and preparation method thereof |
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