CN111362350A - Hydrophobic metal net, preparation method and application in oil-water separation - Google Patents
Hydrophobic metal net, preparation method and application in oil-water separation Download PDFInfo
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- CN111362350A CN111362350A CN202010101507.1A CN202010101507A CN111362350A CN 111362350 A CN111362350 A CN 111362350A CN 202010101507 A CN202010101507 A CN 202010101507A CN 111362350 A CN111362350 A CN 111362350A
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/40—Devices for separating or removing fatty or oily substances or similar floating material
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Abstract
The invention discloses a hydrophobic metal net, a preparation method and application in oil-water separation, wherein ionic liquid is polymerized by ultraviolet light to form polyion liquid to be loaded on the metal net, the hydrophobic metal net is prepared, the contact angle to water in the air is 120-150 degrees, and the thickness of the polyion liquid layer on the surface of the hydrophobic metal net is 1-10 microns. The preparation method is rapid and efficient, and has good repeatability. The hydrophobic metal net can penetrate oil and cut water, has high separation efficiency on various oil-water mixtures, has the advantages of high temperature resistance and pollution resistance, and has great potential application value.
Description
Technical Field
The invention belongs to the technical field of functional materials and oil-water separation, and particularly relates to a polyion liquid loaded hydrophobic metal mesh, a preparation method and application in oil-water separation.
Background
Large volumes of oily waste water are often produced in oil extraction, oil tanker transport, textile industry and daily life. The oily wastewater is treated, so that not only can the water resource be protected from being polluted, but also the purified oil and water can be recycled, and the resources are saved. The membrane separation method based on the surface wettability of the solid material can effectively separate the oily wastewater, and has the advantages of high speed, high efficiency, low cost, simple and convenient operation and the like.
The separation membrane with hydrophobic surface can penetrate oil and intercept water, and has oil-water separation effect. CN107163277A, CN107837693A and CN110655676A all disclose preparation processes of hydrophobic separation membranes, but these preparation methods have many steps, use more organic substances and have high cost. The literature (Applied Surface Science 427 (2018) 253-261) reports a stainless steel net film hydrophobically modified by octadecanoic acid, aluminum particles are deposited on the Surface of the net film by electrostatic deposition before modification, the energy consumption is high, and the aluminum particles are easy to fall off in the oil-water separation process of the net film. The literature (ACS appl. mater. Interfaces 2014, 6, 13324-13329) reports a polydopamine-polyacrylic acid composite net which is modified by mercury ions and is hydrophobic, and the method uses heavy metals and has great harm to human bodies and environment. As mentioned above, the hydrophobic separation membrane in the prior art has the disadvantages of complicated preparation process, harsh preparation conditions, high cost, environmental unfriendliness, poor material stability and the like, does not have universality, and is difficult to be practically applied.
Disclosure of Invention
The invention aims to provide a hydrophobic metal net, a preparation method and application in oil-water separation, wherein the preparation method is quick and efficient and has good repeatability, the hydrophobic metal net can penetrate oil and cut water, and has the advantages of high separation efficiency on various oil-water mixtures, high temperature resistance and pollution resistance.
The specific technical scheme for realizing the purpose of the invention is as follows:
a preparation method of a hydrophobic metal net is characterized in that: the method comprises the following specific steps:
step 1: cleaning the metal mesh with acetone and deionized water in sequence, and drying for later use;
step 2: dipping the metal mesh in the step 1 in a polymerization monomer solution, fully wetting, and then carrying out ultraviolet polymerization, wherein polyion liquid formed by polymerization is loaded on the metal mesh;
and step 3: cleaning the metal mesh obtained in the step 2 with acetone and deionized water in sequence, and drying to obtain the hydrophobic metal mesh; wherein:
the ultraviolet polymerization is free radical polymerization under the irradiation of ultraviolet light with the wavelength of 365 nanometers, and the polymerization time is 1-120 minutes.
The ionic liquid monomer is composed of anions and cations, and the cations are at least one of quaternary ammonium salts, quaternary phosphonium salts, imidazolium salts and pyrrole salts; the anion is at least one of hexafluorophosphate radical, tetrafluoroborate radical and bis (trifluoromethyl sulfonyl imide) ion; the cation contains a carbon-carbon double bond, and the substituent is at least one of butyl, hexyl, octyl and long-chain substituent.
The cross-linking agent is divinylbenzene.
The photoinitiator is 2-hydroxy-2-methyl-1-phenyl-1-acetone.
The solvent is at least one of 1-butyl-3-methylimidazole hexafluorophosphate and N-N-dimethylformamide.
A hydrophobic metal net prepared by the method.
The contact angle of the hydrophobic metal net to water in air is 120-150 degrees, and the thickness of the polyion liquid layer on the surface is 1-10 microns.
The application of the hydrophobic metal net in oil-water separation is characterized in that the hydrophobic metal net can penetrate oil and intercept water to separate an oil-water mixture with the volume ratio of oil to water of 0.01-1; wherein the oil-water mixture is a mixed solution of at least one of n-hexane, toluene, corn oil, dichloromethane and dichloroethane and water.
Compared with the prior art, the invention has the following beneficial effects:
(1) the polyion liquid used in the invention has strong stability and good mechanical property, and is not easy to lose and deform in the using process.
(2) The preparation process is simple, the preparation can be carried out by a one-step method under the irradiation of ultraviolet light, the complex processes such as phase transfer, electrostatic spinning, subsequent modification and the like are not involved, and the scale is easy.
(3) The prepared hydrophobic metal net has high separation efficiency on oil-water mixtures, is suitable for n-hexane, toluene, corn oil, dichloromethane, dichloroethane and the like, is high-temperature resistant, pollution-resistant and reusable.
Drawings
FIG. 1 is a scanning electron microscope image of the surface topography of a hydrophobic metal mesh prepared in example 1 of the present invention;
FIG. 2 is a scanning electron microscope image of a cross-section of a hydrophobic metal mesh prepared in example 1 of the present invention;
FIG. 3 is a photograph showing the contact angle of the hydrophobic metal mesh prepared in example 1 of the present invention with water in the air;
FIG. 4 is a photograph of an experimental apparatus for oil-water separation of the hydrophobic metal mesh prepared in example 1 of the present invention;
FIG. 5 is a graph of separation effect data of the hydrophobic metal mesh prepared in example 1 of the present invention for separating various oil-water mixtures with a volume fraction of 30%;
fig. 6 is a graph of the separation effect data of the hydrophobic metal mesh prepared in example 1 of the present invention at 80 c for continuously separating a dichloroethane/water mixture having a volume fraction of 30%.
Detailed Description
The invention is described in detail below with reference to the figures and specific embodiments.
Example 1
Step 1: shearing a metal sintered felt with the diameter of 5 cm and the mesh opening of 100 microns, putting the metal sintered felt into a beaker, adding 10 ml of acetone for ultrasonic cleaning for 20 minutes, taking out the metal sintered felt, repeatedly washing the metal sintered felt with deionized water, then putting the metal sintered felt into the beaker, adding 10 ml of deionized water for ultrasonic cleaning for 20 minutes, taking out the metal sintered felt, putting the metal sintered felt into an oven, and drying the metal sintered felt at 60 ℃ for later use;
step 2: adding 2.82g of ionic liquid monomer 1-vinyl-3-octyl imidazole hexafluorophosphate, 0.26g of cross-linking agent divinylbenzene and 0.15g of photoinitiator 2-hydroxy-2-methyl-1-phenyl-1-acetone into a beaker, adding 1.38g of solvent 1-butyl-3-methylimidazole hexafluorophosphate, and ultrasonically dissolving for 20 minutes to obtain a uniformly mixed polymerization monomer solution;
and step 3: soaking the dried metal sintered felt for later use in the polymerized monomer solution prepared in the step 2, and carrying out ultrasonic treatment for 20 minutes to completely wet the metal sintered felt;
and 4, step 4: taking out the completely wetted metal sintered felt, horizontally placing the metal sintered felt on a glass plate, and polymerizing the metal sintered felt for 60 minutes under 365-nanometer ultraviolet light;
and 5: after polymerization is finished, the metal sintered felt is respectively ultrasonically cleaned for 20 minutes by using 10 ml of acetone and 10 ml of deionized water, and then the metal sintered felt is placed into an oven and dried at 60 ℃ to obtain the hydrophobic metal mesh loaded with the polyion liquid.
Referring to fig. 1, a scanning electron microscope image of the surface topography of the hydrophobic metal mesh shows that the polyion liquid is loaded on the surface of the metal mesh.
Referring to fig. 2, a scanning electron microscope image of a cross section of the hydrophobic metal mesh shows that the thickness of the polyion liquid layer on the surface of the hydrophobic metal mesh is 4 μm.
Referring to fig. 3, when a 5 microliter drop of water is dropped on the surface of the hydrophobic metal mesh, the drop of water is spherical, and the contact angle of the hydrophobic metal mesh to water in air is 142 °, which has hydrophobic properties.
Example 2
Referring to fig. 4, the hydrophobic metal net 2 prepared as above is fixed in an oil-water separation device, and a dichloroethane/water mixture in a volume ratio of 3:7 is added, so that dichloroethane 3 can penetrate through the hydrophobic metal net 2 and flow into a beaker, and water 1 is trapped above the hydrophobic metal net.
Referring to fig. 5, the hydrophobic metal mesh prepared by the method has an excellent separation effect on an oil-water mixture of n-hexane, toluene, corn oil, dichloromethane and dichloroethane, and the separation efficiency is more than 99.55%.
Referring to fig. 6, the hydrophobic metal mesh prepared above was continuously separated from dichloroethane/water mixture at 80 ℃ for 100 times, the water content in dichloroethane was less than 1200 mg/kg, and the separation efficiency was more than 99.84%.
Claims (9)
1. The preparation method of the hydrophobic metal net is characterized by comprising the following specific steps of:
step 1: cleaning the metal mesh with acetone and deionized water in sequence, and drying for later use;
step 2: dipping the metal mesh in the step 1 in a polymerization monomer solution, fully wetting, and then carrying out ultraviolet polymerization, wherein polyion liquid formed by polymerization is loaded on the metal mesh;
and step 3: cleaning the metal mesh obtained in the step 2 with acetone and deionized water in sequence, and drying to obtain the hydrophobic metal mesh; wherein:
step 1, the metal net is a two-dimensional or three-dimensional metal woven net or a metal sintered felt at least containing one of iron, chromium, nickel, copper and aluminum elements, and the mesh is 20 to 200 microns;
step 2, the polymerization monomer solution comprises an ionic liquid monomer, a cross-linking agent, a photoinitiator and a solvent; wherein the molar ratio of the ionic liquid monomer to the cross-linking agent is 1:0.05-2, the dosage of the photoinitiator is 1-10wt% of the total mass of the ionic liquid monomer and the cross-linking agent, and the mass of the solvent is 0.1-10 times of the total mass of the ionic liquid monomer and the cross-linking agent;
the ultraviolet polymerization is free radical polymerization under the irradiation of ultraviolet light with the wavelength of 365 nanometers, and the polymerization time is 1-120 minutes.
2. The method according to claim 1, wherein the ionic liquid monomer is composed of an anion and a cation, and the cation is at least one of quaternary ammonium salts, quaternary phosphonium salts, imidazolium salts and pyrrole salts; the anion is at least one of hexafluorophosphate radical, tetrafluoroborate radical and bis (trifluoromethyl sulfonyl imide) ion; the cation contains a carbon-carbon double bond, and the substituent is at least one of butyl, hexyl, octyl and long-chain substituent.
3. The method of claim 1, wherein the crosslinking agent is divinylbenzene.
4. The method according to claim 1, wherein the photoinitiator is 2-hydroxy-2-methyl-1-phenyl-1-propanone.
5. The method according to claim 1, wherein the solvent is at least one of 1-butyl-3-methylimidazolium hexafluorophosphate and N-N-dimethylformamide.
6. A hydrophobic metal mesh made by the method of claim 1.
7. The hydrophobic metal net according to claim 6, wherein the contact angle to water in air is 120-150 °, and the thickness of the polyionic liquid layer on the surface is 1-10 μm.
8. Use of the hydrophobic metal mesh of claim 6 in oil-water separation.
9. The use according to claim 7, wherein the hydrophobic metal mesh is capable of oil and water penetration and separation of oil-water mixture with oil-water volume ratio of 0.01-1; wherein the oil-water mixture is a mixed solution of at least one of n-hexane, toluene, corn oil, dichloromethane and dichloroethane and water.
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Cited By (2)
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CN114904495A (en) * | 2022-04-29 | 2022-08-16 | 东南大学 | Adsorption film for adsorbing and removing mycotoxin in liquid, adsorption method and application thereof |
CN115286771A (en) * | 2022-07-05 | 2022-11-04 | 青岛科技大学 | Preparation method and application of switchable oil-water separation intelligent material polyion liquid |
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CN114904495A (en) * | 2022-04-29 | 2022-08-16 | 东南大学 | Adsorption film for adsorbing and removing mycotoxin in liquid, adsorption method and application thereof |
CN114904495B (en) * | 2022-04-29 | 2024-02-20 | 东南大学 | Adsorption film for removing mycotoxin in liquid by adsorption, adsorption method and application thereof |
CN115286771A (en) * | 2022-07-05 | 2022-11-04 | 青岛科技大学 | Preparation method and application of switchable oil-water separation intelligent material polyion liquid |
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