CN110237727B - Preparation method of super-hydrophobic separation membrane - Google Patents

Preparation method of super-hydrophobic separation membrane Download PDF

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CN110237727B
CN110237727B CN201910532315.3A CN201910532315A CN110237727B CN 110237727 B CN110237727 B CN 110237727B CN 201910532315 A CN201910532315 A CN 201910532315A CN 110237727 B CN110237727 B CN 110237727B
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刘华蓉
崔晓玲
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University of Science and Technology of China USTC
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D17/00—Separation of liquids, not provided for elsewhere, e.g. by thermal diffusion
    • B01D17/02—Separation of non-miscible liquids
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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    • B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
    • B01D67/0002—Organic membrane manufacture
    • B01D67/0006—Organic membrane manufacture by chemical reactions
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    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
    • B01D69/02—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor characterised by their properties
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
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Abstract

The invention provides a preparation method of a super-hydrophobic separation membrane, which comprises the following steps: dispersing the intercommunicated porous polymer microspheres in a solution to obtain a dispersion liquid; and filtering and depositing the dispersion liquid by adopting a matrix, and drying to obtain the super-hydrophobic separation membrane. The fluorine-free super-hydrophobic separation membrane is prepared by the intercommunicated porous polymer microspheres, the preparation method of the super-hydrophobic separation membrane is simple, rapid and efficient, and the prepared super-hydrophobic separation membrane has high-efficiency oil-water separation capacity, high oil flux, good stability and recoverability under the corrosion condition, and has important significance for novel oil-water separation membranes capable of realizing large-scale production and application.

Description

Preparation method of super-hydrophobic separation membrane
Technical Field
The invention relates to the technical field of oil-water separation membrane materials, in particular to a preparation method of a super-hydrophobic separation membrane.
Background
With the advance of industrialization, serious environmental damage and economic loss caused by the increasing oil pollution of water sources and frequent oil leakage accidents in the past decades have become huge challenges worldwide. To eliminate the effects of oil contamination, oil-water separation using superhydrophobic separation membranes is generally considered the most efficient, effective and feasible method of separation.
The super-hydrophobic material is a material with a water contact angle of more than 150 degrees and a rolling contact angle of less than 8 degrees, has wide application prospect in the fields of oil-water separation, self-cleaning and energy related, and has attracted great interest in academia and industry. Polymers with hydrophobic-lipophilic properties are useful as low surface energy materials for oil-water separation. Among them, fluoropolymers are very effective in building superhydrophobic surfaces; but even with the lowest surface energy-CF2-(6mJ×m-2) The constructed smooth surface can only reach the maximum contact angle of 119 degrees, and the super-hydrophobicity is difficult to realize. Roughness is essential for superhydrophobic surfaces, and particle modification is a common method of forming a rough surface by spreading additional particles on a substrate. Recently reported particle modification methods mainly include plasma enhanced chemical vapor deposition, physical vapor deposition, aerosol deposition, dip coating, spin coating, spray coating, magnetron sputtering, hot pressing and dipping. However, these processes have considerable disadvantages, such as complex preparation, high costs, poor mechanical properties and resistance to corrosive environments, and even slight mechanical damage can permanently lose the functionality of these materials; in addition, large-scale application is difficult to achieve.
The Chinese patent with the application number of 201710035678.7 discloses a preparation method of a super-hydrophobic magnesium alloy coating, which comprises the steps of firstly grinding a magnesium alloy by abrasive paper or a grinding wheel, removing surface grease and an oxide layer after acid cleaning, then carrying out subfluorination treatment on the surface, then electrodepositing a chloroaluminum ion solution on the surface subjected to hatching treatment to form an aluminum layer, and finally carrying out lifting and pulling on SiO in a lifting manner2And Polydimethylsiloxane (PDMS) composite solution is coated on the surface after electrodeposition to prepare the super-hydrophobic coating. However, the method needs multi-step operation to realize the super-hydrophobic effect, has complex process and needs subfluorination treatment, and causes harm to the environment.
Therefore, a method which is simple and easy to operate and can realize large-scale production of the oil-water separation membrane is developed, and the separation membrane has high oil-water separation capacity, good stability and recoverability under a corrosive condition, and has important significance for developing and applying a novel oil-water separation membrane.
Disclosure of Invention
The invention aims to provide a preparation method of a super-hydrophobic separation membrane, and the super-hydrophobic separation membrane provided by the application has high-efficiency oil-water separation capacity, good stability and recyclability under a corrosive condition.
In view of the above, the present application provides a method for preparing a superhydrophobic separation membrane, comprising the steps of:
dispersing the intercommunicated porous polymer microspheres in a solution to obtain a dispersion liquid;
and filtering and depositing the dispersion liquid by adopting a matrix, and drying to obtain the super-hydrophobic separation membrane.
Preferably, the solution is toluene, acetone, alcohols or an alcohol-water mixed solution.
Preferably, when the solution is an alcohol-water mixed solution, the alcohol in the alcohol-water mixed solution is selected from ethanol, methanol or isopropanol, and the volume ratio of the alcohol to the water in the alcohol-water mixed solution is (1-5): (1-5).
Preferably, the substrate is a stainless steel mesh, filter paper or filter membrane.
Preferably, the substrate is a stainless steel mesh, and the intercommunicated porous polymer microspheresThe area ratio of the mass to the stainless steel mesh is 0.01-5 mg/cm2The mesh number of the stainless steel mesh is 300-2000 meshes.
Preferably, the particle size of the intercommunicated porous polymer microspheres is 1-400 μm.
Preferably, the preparation method of the intercommunicated porous polymer microspheres specifically comprises the following steps:
mixing an oil-soluble monomer, a cross-linking agent and an emulsifier to obtain an oil phase;
mixing the oil phase and water to obtain a double emulsion;
and initiating the double emulsion to react to obtain the intercommunicated porous polymer microspheres.
Preferably, the oil-soluble monomer has the formula CH2＝CR1R2Wherein R is1Is hydrogen or methyl, R2Is aryl, a derivative thereof or COOR3，R3Is alkyl or a derivative thereof;
the cross-linking agent has a general formula of R4(CR5＝CH2)nWherein R is4Is aryl, alkyl, ether-containing or ester-containing radical, R5Is hydrogen or methyl, n is an integer of 2 to 4;
the structural formula of the emulsifier is shown in the specification
Figure BDA0002100141690000031
Figure BDA0002100141690000032
Wherein X is NH4 +、Na+、K+Or amine salt, R is aliphatic alkyl or aryl, a is an integer of 6-14, b is 1 or 2, and c is an integer of 3-14.
Preferably, the method of initiating the reaction is radiation initiation or free radical initiation.
The application provides a preparation method of a super-hydrophobic separation membrane, which comprises the steps of dispersing intercommunicated porous polymer microspheres in a solution, filtering and depositing, and drying to obtain the super-hydrophobic separation membrane; according to the method, the communicated porous polymer microspheres are used for preparing the super-hydrophobic separation membrane, the communicated porous polymer microspheres have lipophilicity and hydrophobicity, so that the surface of the separation membrane has low surface energy, and the porous structure of the particles increases the roughness of the surface of the separation membrane, so that the separation membrane has super-hydrophobicity; furthermore, the intercommunicated porous polymer microspheres are difficult to infiltrate into an acidic aqueous solution, an alkaline aqueous solution or pure water, so that the separation membrane has high-efficiency oil-water separation capacity under corrosive conditions.
Drawings
FIG. 1 is a scanning electron micrograph of porous microspheres S1-P (St-DVB);
FIG. 2 is a scanning electron microscope photograph and a water contact angle photograph of the superhydrophobic separation membrane S2;
FIG. 3 is a scanning electron micrograph of porous microspheres S3-P (MMA-St-DVB);
FIG. 4 is a scanning electron microscope photograph and a water contact angle photograph of the superhydrophobic separation membrane S4;
FIG. 5 is a scanning electron micrograph of porous microspheres S5-P (BA-St-DVB);
FIG. 6 is a scanning electron microscope photograph and a water contact angle photograph of the superhydrophobic separation membrane S6;
FIG. 7 is a scanning electron micrograph of porous microspheres S7-P (EHA-St-DVB);
FIG. 8 is a scanning electron microscope photograph and a water contact angle photograph of the superhydrophobic separation membrane S8;
FIG. 9 is a scanning electron micrograph of porous microspheres S9-P (SMA-St-DVB);
FIG. 10 is a scanning electron microscope photograph and a water contact angle photograph of the superhydrophobic separation membrane S10;
fig. 11 is a graph of separation efficiency, flux and contact angle for different cycle numbers of the superhydrophobic separation membrane S10 prepared in example 5.
Detailed Description
For a further understanding of the invention, reference will now be made to the preferred embodiments of the invention by way of example, and it is to be understood that the description is intended to further illustrate features and advantages of the invention, and not to limit the scope of the claims.
In view of the requirements of the prior art on the separation membrane, the application provides a preparation method of a super-hydrophobic separation membrane, which utilizes intercommunicated porous polymer microspheres to prepare the separation membrane, so that the obtained separation membrane has high oil-water separation capacity, good stability and recyclability under corrosive conditions. Specifically, the embodiment of the invention discloses a preparation method of a super-hydrophobic separation membrane, which comprises the following steps:
dispersing the intercommunicated porous polymer microspheres in a solution to obtain a dispersion liquid;
and filtering and depositing the dispersion liquid by adopting a matrix, and drying to obtain the super-hydrophobic separation membrane.
In the process of preparing the super-hydrophobic separation membrane, the intercommunicated porous polymer microspheres are dispersed in a solution to obtain a dispersion liquid; in the present application, the intercommunicated porous polymer microspheres are well known to those skilled in the art, and have a particle size of 1-400 μm, and in a specific embodiment, the intercommunicated porous polymer microspheres have a particle size of 5-10 μm. Specifically, the preparation method of the intercommunicated porous polymer microspheres comprises the following steps:
mixing an oil-soluble monomer, a cross-linking agent and an emulsifier to obtain an oil phase;
mixing the oil phase and water to obtain a double emulsion;
and initiating the double emulsion to react to obtain the intercommunicated porous polymer microspheres.
In the above process, the oil-soluble monomer has the general formula CH2＝CR1R2Wherein R is1Is hydrogen or methyl, R2Is aryl, a derivative thereof or COOR3，R3Is alkyl or a derivative thereof; more specifically, the oil-soluble monomer is selected from one or more of styrene, 4-methyl styrene, 4-ethyl styrene, chlorostyrene, chloromethyl styrene, and (meth) acrylates, and in specific embodiments, the oil-soluble monomer is selected from one or two of styrene, methyl methacrylate, n-butyl acrylate, ethylhexyl acrylate, and octadecyl methacrylate.
The cross-linking agent has a general formula of R4(CR5＝CH2)nWherein R is4Is aryl, alkyl, ether-containing or ester-containing radical, R5Is hydrogen or methyl, n is an integer of 2 to 4; more specifically, the cross-linking agent is selected from one or more of ethylene glycol dimethacrylate, octanediol acrylate, pentaerythritol diacrylate, pentaerythritol triacrylate, pentaerythritol tetraacrylate, and divinylbenzene, and in particular embodiments, the cross-linking agent is selected from divinylbenzene. The structural formula of the emulsifier is shown in the specification
Figure BDA0002100141690000051
Wherein X is NH4 +、Na+、K+Or amine salt, R is saturated or unsaturated aliphatic alkyl or aryl, a is an integer of 6-14, b is 1 or 2, and c is an integer of 3-14. In a particular embodiment, the emulsifier selected is 12-acryloxy-9-octadecenoic acid.
After the oil phase is obtained, it is then mixed with water to obtain a double emulsion consisting of a number of large droplets containing many small droplets inside. The mass ratio of the oil phase to the water phase is 1: (5-10). And finally, initiating polymerization by the double emulsion to obtain the intercommunicated porous polymer microspheres. The method for initiating the reaction is radiation initiation or free radical initiation; in a specific embodiment, the method for initiating the reaction is gamma-ray radiation initiation, more specifically, a cobalt 60 radiation source is selected, and the absorption dose rate of the cobalt 60 radiation source is 10-200 Gy.min-1The absorbed dose is 30-200 KGy, and the irradiation temperature is room temperature.
After the intercommunicated porous polymer microspheres are obtained according to the method, the intercommunicated porous polymer microspheres are dispersed in a solution to obtain a dispersion liquid; the solution is selected from toluene, acetone, alcohols or alcohol-water mixed solution; in a specific embodiment, the solution is selected from a mixed solution of ethanol and water. The volume ratio of the ethanol to the water is (1-5): (1-5), in a specific embodiment, the volume ratio of the ethanol to the water is 1: 1.
After the dispersion liquid is obtained, the dispersion liquid is filtered and deposited by using a matrix, and the super-hydrophobic separation membrane is obtained after drying. In thatIn this process, the substrate is a substrate well known to those skilled in the art, and in particular embodiments, the substrate is selected from a stainless steel mesh, a filter paper, or a filter membrane. More particularly, the substrate is selected from a stainless steel mesh; the mass of the intercommunicated porous polymer microspheres to the area ratio of the stainless steel mesh is 0.01-5 mg/cm2The mesh number of the stainless steel mesh is 300-2000 meshes. The ratio of the mass of the intercommunicated polymer microspheres to the area of the stainless steel mesh directly influences the thickness of the separation membrane, and the increase of the thickness can increase the contact angle and enhance the super-hydrophobicity; but the area ratio exceeds 1mg/cm2Excessive accumulation of microspheres can be caused, so that the microspheres are easy to fall off, and the stability of the membrane is affected.
The fluorine-free super-hydrophobic separation membrane is prepared by the intercommunicated porous polymer microspheres, the preparation method of the super-hydrophobic separation membrane is simple, rapid and efficient, and the prepared super-hydrophobic separation membrane has high-efficiency oil-water separation capacity, high oil flux, good stability and recoverability under the corrosion condition, and has important significance for novel oil-water separation membranes capable of realizing large-scale production and application.
For further understanding of the present invention, the following examples are provided to illustrate the preparation method of the superhydrophobic separation membrane of the present invention, and the scope of the present invention is not limited by the following examples.
In the examples, a constant speed mechanical stirrer of model D2010W, manufactured by Shanghai Spire Instrument Co., Ltd, was used for stirring;
detecting the shapes and sizes of the porous polymer microspheres and the super-hydrophobic oil-water separation membrane by using a Hitachi high-new SU8200 field emission scanning electron microscope;
the surface water contact angle of the film was measured by a contact angle meter SL200B (shanghai barron information corporation); the test conditions were room temperature (24. + -. 2 ℃ C.), a relative humidity of 75%, and the contact angles at 5 different positions were randomly measured for each sample, and the average value was taken, and the sample film was vacuum-dried at 60 ℃ for 6 hours before the test.
Example 1
(1) Adding 2g of styrene, 1g of divinylbenzene and 0.75g of 12-acryloyloxy-9-octadecenoic acid into a 100ml beaker, using a syringe to take a certain amount of ammonia water to adjust the pH to 8, and uniformly mixing to obtain a light yellow viscous opaque liquid which is an oil phase;
(2) dropwise adding 15.0g of distilled water into the oil phase for three times under the stirring condition of 500r/min to prepare double emulsion;
the double emulsion was transferred to a 20ml beaker and placed in a 1.30X 10 beaker15Bq60In Co-Co source, radiation polymerization reaction is initiated by gamma ray, and the dosage rate and absorbed dose are respectively 96.5 Gy.min-1And 139.0 kGy; washing the product with distilled water for 2 times, then washing with ethanol, and drying to obtain porous polymer microsphere S1, as shown in FIG. 1, the average diameter of the prepared porous polymer microsphere is 5.1 μm;
(3) firstly, placing a stainless steel net in ethanol and deionized water, respectively cleaning by ultrasonic waves, and then airing; ultrasonically dispersing 5mg of porous polymer microspheres by using 100mL of ethanol-water mixed solution with the volume ratio of 1:1, and then filtering and depositing on a contact area of 12cm2On a 304 stainless steel mesh, a superhydrophobic separation membrane S2 was prepared and the water contact angle was measured to be 151 °, as shown in fig. 2.
Example 2
Example 1 was repeated with the difference that: "2 g of styrene" was replaced with "1 g of styrene, 1g of methyl methacrylate"; "15.0 g of distilled water" was replaced with "16.5 g of distilled water"; replacing 500r/min with 300r/min to obtain porous polymer microsphere S3; as shown in FIG. 3, the average diameter of the prepared porous polymer microspheres was 5.6. mu.m.
The deposition preparation was also filtered, a superhydrophobic separation membrane S4 was prepared, and the water contact angle was measured to be 152 ° as shown in fig. 4.
Example 3
Example 1 was repeated with the difference that: "2 g of styrene" was replaced by "1 g of styrene, 1g of n-butyl acrylate"; "15.0 g of distilled water" was replaced with "18 g of distilled water"; replacing 500r/min with 300r/min to obtain porous polymer microsphere S5; as shown in FIG. 5, the average diameter of the prepared porous polymer microspheres was 8.3. mu.m.
The deposition preparation was also filtered, and a superhydrophobic separation membrane S6 was prepared and the water contact angle was measured to be 155 ° as shown in fig. 6.
Example 4
Example 1 was repeated with the difference that: "2 g of styrene" was replaced with "1 g of styrene, 1g of ethylhexyl acrylate"; "15.0 g of distilled water" was replaced with "19.5 g of distilled water"; the porous polymer microspheres S7 were finally obtained by replacing "500 r/min" with "300 r/min", and the average diameter of the prepared porous polymer microspheres was 7.4 μm, as shown in FIG. 7.
The deposition preparation was also filtered, and a superhydrophobic separation membrane S8 was prepared and the water contact angle was measured to be 152 ° as shown in fig. 8.
Example 5
Example 1 was repeated with the difference that: "2 g of styrene" was replaced with "1 g of styrene, 1g of stearyl methacrylate"; "15.0 g of distilled water" was replaced with "21.0 g of distilled water"; the porous polymer microspheres S9 were finally obtained by replacing "500 r/min" with "300 r/min", and the average diameter of the prepared porous polymer microspheres was 8.6 μm, as shown in FIG. 9.
The deposition preparation was also filtered, a superhydrophobic separation membrane S10 was prepared, and the water contact angle was measured to be 152 ° as shown in fig. 10.
Example 6
The superhydrophobic separation membrane S10 prepared in example 5 was fixed between two cylindrical glass devices of an oil-water separation apparatus, and an oil-water mixture (about 100mL of an oil solvent and 100mL of water mixed) was poured into the fixed apparatus to perform an oil-water separation experiment; the oil-water separation circulation experiment is carried out on the super-hydrophobic separation membrane S10, and the separation effect is good. Fig. 11 is a data graph of separation efficiency, flux and contact angle of a superhydrophobic separation membrane at cycle number, the bar graph in fig. 11(a) is the separation efficiency at different cycle number, and the curve is the flux at different cycle number; as can be seen from fig. 11(a), the membrane oil-water separation efficiency can reach 99.5%, and the membrane has excellent separation stability and stable permeation flux. As can be seen from fig. 11(b), there was substantially no change in contact angle during cycling.
The above description of the embodiments is only intended to facilitate the understanding of the method of the invention and its core idea. It should be noted that, for those skilled in the art, it is possible to make various improvements and modifications to the present invention without departing from the principle of the present invention, and those improvements and modifications also fall within the scope of the claims of the present invention.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.

Claims (4)

1. A preparation method of a super-hydrophobic separation membrane comprises the following steps:
dispersing the intercommunicated porous polymer microspheres in a solution to obtain a dispersion liquid;
filtering and depositing the dispersion liquid by adopting a matrix, and drying to obtain a super-hydrophobic separation membrane;
the solution is toluene, acetone, alcohol or alcohol-water mixed solution;
the substrate is a stainless steel mesh, and the mass of the intercommunicated porous polymer microspheres to the area ratio of the stainless steel mesh is 0.01-5 mg/cm2The mesh number of the stainless steel mesh is 300-2000 meshes;
the particle size of the intercommunicated porous polymer microspheres is 1-400 mu m;
when the solution is an alcohol-water mixed solution, alcohol in the alcohol-water mixed solution is selected from ethanol, methanol or isopropanol, and the volume ratio of the alcohol to the water in the alcohol-water mixed solution is (1-5): (1-5).
2. The method according to claim 1, wherein the method for preparing the intercommunicated porous polymer microspheres specifically comprises:
mixing an oil-soluble monomer, a cross-linking agent and an emulsifier to obtain an oil phase;
mixing the oil phase and water to obtain a double emulsion;
and initiating the double emulsion to react to obtain the intercommunicated porous polymer microspheres.
3. The method according to claim 2, wherein the oil-soluble monomer has a formula of CH2＝CR1R2Wherein R is1Is hydrogen or methyl, R2Is aryl, a derivative thereof or COOR3，R3Is alkyl or a derivative thereof;
the cross-linking agent has a general formula of R4(CR5＝CH2)nWherein R is4Is aryl, alkyl, ether-containing or ester-containing radical, R5Is hydrogen or methyl, n is an integer of 2 to 4;
the structural formula of the emulsifier is shown in the specification
Figure FDA0002914756850000011
Figure FDA0002914756850000012
Wherein X is NH4 +、Na+、K+Or amine salt, R is aliphatic alkyl or aryl, a is an integer of 6-14, b is 1 or 2, and c is an integer of 3-14.
4. The method of claim 2, wherein the method of initiating the reaction is radiation initiation or radical initiation.
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