CN114042339A - Micron nickel particle loaded oil-water separation mesh membrane and preparation method and application thereof - Google Patents
Micron nickel particle loaded oil-water separation mesh membrane and preparation method and application thereof Download PDFInfo
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- CN114042339A CN114042339A CN202111471774.9A CN202111471774A CN114042339A CN 114042339 A CN114042339 A CN 114042339A CN 202111471774 A CN202111471774 A CN 202111471774A CN 114042339 A CN114042339 A CN 114042339A
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Abstract
The invention belongs to the field of surface modification of metal materials, and relates to an oil-water separation mesh membrane, and a preparation method and application thereof. The preparation method adopts a pretreated stainless steel mesh as a cathode, adopts metal ion solution containing micron nickel particles as electroplating solution, places the cathode stainless steel mesh in a magnetic field environment, and utilizes a process method combining a magnetic field induction technology and a jet flow electrodeposition technology, namely a magnetic field assisted jet flow electrodeposition technology to prepare the micron nickel particle loaded oil-water separation stainless steel mesh membrane. The oil-water separation mesh membrane provided by the invention has the advantages of simple preparation process, low cost, environmental friendliness, no need of introducing low-surface-energy organic matter modification, high oil-water separation efficiency and wide application range, and is beneficial to industrial production.
Description
Technical Field
The invention belongs to the field of surface modification of metal materials, and relates to an oil-water separation mesh membrane, and a preparation method and application thereof.
Background
Petroleum is taken as an important energy substance, namely blood of modern industry, and with the development of social economy, the demand of oil products in industrial production is greatly increased. In recent years, the water content of produced oil is higher and higher in the middle and later stages of petroleum production in China, a large amount of produced water in an oil field needs to be treated every year, and crude oil dehydration and sewage treatment are more and more difficult. In addition, various oil spilling accidents and oil pollution caused by the discharge of oily sewage to water and the ecological environment are greatly increased, and if the oil pollution is not treated in time, the oil pollution can cause great harm to the ecological environment and human life. The preparation and application research of the high-efficiency stable oil-water separation membrane has important scientific research value and practical significance in order to protect the ecological environment and prevent and treat oil pollution.
Compared with the traditional oil-water separation method (a gravity method, a centrifugal method, an in-situ combustion method and the like), the method for preparing the oil-water separation net film by adopting the electrodeposition method has the advantages of low energy consumption, high efficiency, simple process, low environmental pollution, strong universality and the like, and has attracted extensive attention of researchers. Chinese patent publication No. CN112999698A discloses a method for preparing an oil-water separation net, which comprises forming a coating with a nano-rod-shaped structure on the surface of a stainless steel net through electro-deposition of nickel and solvothermal reaction, and then forming a coating on the surface of the stainless steel net at C14H28O2And carrying out chemical modification in an ethanol solution to obtain the super-hydrophobic/super-oleophilic oil-water separation net membrane. Although the oil-water separation net film with excellent performance is successfully prepared by the method, the preparation process requires two steps of operations of electrodeposition and solvothermal reaction to construct a rough structure on a stainless steel net substrate, and low-surface-energy organic matters are required to be further introduced for surface modification, so that the preparation process is complicated, the cost is high, certain pollution is caused to the environment, and the method is not suitable for industrial large-scale production.
Therefore, the process method combining the magnetic field induction technology and the jet flow electrodeposition technology is provided, the magnetic field is applied in the jet flow electrodeposition process to induce the micron nickel particles to be adsorbed and deposited on the stainless steel mesh substrate to construct a coarse structure, the modification of low-surface-energy organic matters is not required to be subsequently introduced, the oil-water separation mesh membrane with the super-hydrophobic/super-oleophylic characteristics can be obtained in one step, and the process method is simple to operate, efficient and environment-friendly.
Disclosure of Invention
The invention discloses an oil-water separation mesh membrane loaded with micron nickel particles and a preparation method and application thereof, aiming at the problems in the prior art.
The technical scheme of the invention is as follows:
a preparation method of an oil-water separation net film loaded with micron nickel particles comprises the following steps:
step 1) pretreatment of cathode materials: cleaning the stainless steel net, and then airing for later use;
step 2) preparing an electroplating solution: adding micron nickel particles into metal ion electroplating solution, carrying out ultrasonic oscillation and stirring, and uniformly dispersing the micron nickel particles in the electroplating solution;
step 3), preparing a net film: clamping the stainless steel mesh obtained in the step (1) on a workbench of a magnetic field assisted radio-current electrodeposition device, adding the electroplating solution containing micron nickel particles obtained in the step (2) into a water bath of the device, and electrifying to obtain an oil-water separation net film;
step 4) washing the oil-water separation mesh membrane obtained in the step 3 with deionized water to remove residual electroplating solution and micron nickel particles on the surface;
and 5) placing the net film obtained in the step 4 under a ventilation condition, and naturally drying.
Preferably, in the step 1, the stainless steel net is cleaned by sequentially performing ultrasonic cleaning on the stainless steel net with acetone, ethanol and deionized water for 10min, and before the stainless steel net is cleaned, a surface oxide layer can be removed by using 1mol/L diluted hydrochloric acid.
Preferably, in the step 1, the mesh number of the stainless steel mesh is 200-400 meshes, and the size is 50 × 50 mm.
Preferably, in the step 2, the particle size of the micron nickel particles is 1-3 μm, the addition amount of the micron nickel particles in the metal ion plating solution is 1-4 g/L, and the pH of the metal ion plating solution is adjusted to 3.8-4.2 by using an alkaline solution.
Preferably, in the step 2, the ultrasonic oscillation frequency is 30-40 kHz, the stirring rotation speed is 150-200 r/min, and the oscillation stirring is 20-40 min.
Preferably, in the step 3, the magnetic field direction of the cathode region is perpendicular to the surface of the cathode metal mesh, the magnetic field strength is 50-200 mT, the temperature of the electroplating solution is controlled to be 45-55 ℃ by heating the water bath, the flow rate of the electroplating solution is 140-160L/h, the electrifying voltage is 15-20V, and the deposition time is 10-40 min.
The invention also discloses an oil-water separation mesh membrane prepared by the method.
The surface of the oil-water separation mesh membrane prepared by the method is loaded with a coarse structure formed by micron nickel particles, the pore size of the mesh membrane is 5-70 mu m, the water contact angle of the mesh membrane in the air is larger than 150 degrees, and the oil contact angle is close to 0 degree.
The invention also provides application of the oil-water separation mesh membrane in separation of oil-water mixtures and water body purification.
The invention has the beneficial effects that:
(1) the micron nickel particle-loaded oil-water separation mesh membrane is prepared in one step by adopting a magnetic field assisted jet electrodeposition process, modification of low-surface-energy organic matters is not required, and the preparation method is environment-friendly, low in cost, simple in preparation process and suitable for industrial production.
(2) The prepared oil-water separation mesh membrane has a good separation effect on diesel oil, gasoline, edible oil, carbon tetrachloride, 1, 2-dichloroethane, dichloromethane, n-hexane, petroleum ether, hexadecane and the like, is wide in application range, and can be repeatedly used.
Drawings
FIG. 1 is a scanning electron microscope image of the overall surface topography of the oil-water separation mesh film prepared in example 1
FIG. 2 is an enlarged scanning electron microscope image of the surface topography of the oil-water separation mesh membrane prepared in example 1
FIG. 3 is a surface water contact angle plot of the superhydrophobic/superhydrophilic oil-water separation mesh membrane prepared in example 1
FIG. 4 is a surface oil contact angle plot of the superhydrophobic/superhydrophilic oil-water separation mesh membrane prepared in example 1
FIG. 5 is a diagram showing an oil-water separator used for oil-water separation and the effect thereof
FIG. 6 is a scanning electron microscope image of the surface topography of the mesh film prepared in comparative example 1 without adding micron nickel particles
FIG. 7 is a surface water contact angle chart of the omentum prepared in comparative example 1
FIG. 8 is a surface oil contact angle plot of omentum prepared in comparative example 1
FIG. 9 scanning electron microscope image of the surface topography of the omentum prepared in comparative example 2 without the assistance of a magnetic field
Detailed Description
The invention is further illustrated by the following examples without limiting the scope of the invention.
Example 1:
step 1) pretreatment of cathode materials. Selecting a 300-mesh 304 stainless steel net as a cathode substrate, ultrasonically cleaning the cathode substrate with acetone, ethanol and deionized water for 10min in sequence, and airing for later use;
step 2) preparing electroplating solution. Dissolving 520g of nickel sulfate, 80g of nickel chloride, 80g of boric acid and 10g of saccharin in 1.5L of deionized water, adding deionized water until the volume of the solution is 2L, and fully stirring until the solution is completely dissolved;
and 3) dispersing micron nickel particles. Adding 4g of nickel particles with the average particle size of 2 mu m into the electroplating solution prepared in the step 2, and stirring for 30min by ultrasonic oscillation;
and 4) preparing the net film. And (2) taking the treated stainless steel mesh as a cathode, taking pure nickel as an anode, electroplating in a magnetic field environment with the surface of the cathode stainless steel mesh perpendicular to 100mT by using electroplating solution containing micron nickel particles, heating the electroplating solution to 40 ℃, enabling the flow rate of the electroplating solution to be 150L/h, adopting a direct current power supply, enabling the applied voltage to be 20V, processing for 20min, then turning off the power supply, taking out a stainless steel net membrane, washing with deionized water, and naturally airing to obtain the oil-water separation net membrane.
Fig. 1 and fig. 2 are a scanning electron microscope image and a partially enlarged scanning electron microscope image of the surface morphology of the entire oil-water separation mesh membrane prepared in this example, and it can be seen that the coarse structure of the mesh membrane surface is composed of a plurality of micron nickel particles. The wettability test is carried out on the surface of the omentum, the water contact angle of the surface of the omentum is larger than 150 degrees (figure 3), the oil contact angle is 0 degree (figure 4), and the omentum shows super-hydrophobicity/super-lipophilicity.
The super-hydrophobic/super-oleophylic net film obtained in this embodiment was subjected to oil-water separation performance test:
an oil-water separation experiment was performed using the experimental apparatus shown in fig. 5. The prepared net membrane is clamped between two quartz glass tubes through a clamp, carbon tetrachloride and deionized water are fully mixed (the volume ratio is 1: 1), the mixture is poured into an upper glass tube, the carbon tetrachloride flows into a lower beaker through meshes, and water is retained in the upper glass tube, so that oil-water separation is realized, and the separation rate is over 95 percent.
Example 2:
step 1) pretreatment of cathode materials. Selecting a 200-mesh 304 stainless steel net as a cathode substrate, ultrasonically cleaning for 10min by using acetone, ethanol and deionized water in sequence, and airing for later use;
step 2) preparing electroplating solution. Dissolving 520g of nickel sulfate, 80g of nickel chloride, 80g of boric acid and 10g of saccharin in 1.5L of deionized water, adding deionized water until the volume of the solution is 2L, and fully stirring until the solution is completely dissolved;
and 3) dispersing micron nickel particles. Adding 4g of nickel particles with the average particle size of 2 mu m into the electroplating solution prepared in the step 2, and stirring for 30min by ultrasonic oscillation;
and 4) preparing the net film. And (2) taking the treated stainless steel mesh as a cathode, taking pure nickel as an anode, electroplating in a magnetic field environment with 150mT perpendicular to the surface of the cathode stainless steel mesh by using electroplating solution containing micron nickel particles, heating the electroplating solution to 40 ℃, enabling the flow rate of the electroplating solution to be 150L/h, adopting a direct current power supply, enabling the applied voltage to be 18V, processing for 20min, then turning off the power supply, taking out a stainless steel net membrane, washing with deionized water, and naturally airing to obtain the oil-water separation net membrane.
The surface of the omentum prepared by the embodiment is subjected to wettability test, the surface water contact angle is more than 150 degrees, the oil contact angle is 0 degree, and the omentum shows super-hydrophobicity/super-lipophilicity.
The super-hydrophobic/super-oleophylic net film obtained in this embodiment was subjected to oil-water separation performance test:
an oil-water separation experiment was performed using the experimental apparatus shown in fig. 5. The prepared net membrane is clamped between two quartz glass tubes through a clamp, edible oil and deionized water are fully mixed (the volume ratio is 1: 1), the mixture is poured into an upper glass tube, the edible oil flows into a lower beaker through meshes, and water is retained in the upper glass tube, so that oil-water separation is realized, and the separation rate is over 90 percent.
Example 3:
step 1) pretreatment of cathode materials. Selecting a 400-mesh 304 stainless steel net as a cathode substrate, ultrasonically cleaning the cathode substrate with acetone, ethanol and deionized water for 10min in sequence, and airing for later use;
step 2) preparing electroplating solution. 520g of nickel sulfate, 80g of nickel chloride, 80g of boric acid and 10g of saccharin are dissolved in 1.5L of deionized water, then the deionized water is added until the volume of the solution is 2L, and the mixture is fully stirred until the solution is completely dissolved.
And 3) dispersing micron nickel particles. 4g of nickel particles with the average particle size of 2 mu m are added into the electroplating solution prepared in the step 2, and the ultrasonic oscillation stirring is carried out for 30 min.
And 4) preparing the net film. And (2) taking the treated stainless steel mesh as a cathode, taking pure nickel as an anode, electroplating in a magnetic field environment with 50mT perpendicular to the surface of the cathode stainless steel mesh by using electroplating solution containing micron nickel particles, heating the electroplating solution to 40 ℃, enabling the flow rate of the electroplating solution to be 150L/h, adopting a direct current power supply, enabling the applied voltage to be 20V, processing for 20min, then turning off the power supply, taking out a stainless steel net membrane, washing with deionized water, and naturally airing to obtain the oil-water separation net membrane.
The surface of the omentum prepared by the embodiment is subjected to wettability test, the surface water contact angle is more than 150 degrees, the oil contact angle is 0 degree, and the omentum shows super-hydrophobicity/super-lipophilicity.
The super-hydrophobic/super-oleophylic net film obtained in this embodiment was subjected to oil-water separation performance test:
an oil-water separation experiment was performed using the experimental apparatus shown in fig. 5. The prepared net membrane is clamped between two quartz glass tubes through a clamp, petroleum ether and deionized water are fully mixed (the volume ratio is 1: 1), the mixture is poured into an upper glass tube, the petroleum ether flows into a lower beaker through meshes, and water is retained in the upper glass tube, so that oil-water separation is realized, and the separation rate is more than 98%.
Comparative example 1:
this comparative example differs from example 1 in that: and (3) removing the electroplating solution, namely, not adding micron nickel particles into the electroplating solution. The rest of the experimental conditions were the same.
The prepared mesh membrane has the surface topography shown in fig. 6, and compared with the mesh membrane prepared in example 1, the mesh membrane prepared without adding micron nickel particles in the electroplating solution has a relatively smooth surface. The wettability test was performed on the surface with a water contact angle of 124 ° (fig. 7), an oil contact angle close to 0 ° (fig. 8), and the surface was not superhydrophobic. The net film is used for oil-water separation tests, and has no separation effect on oil-water mixtures.
Comparative example 2:
this comparative example differs from example 1 in that: in step 4, no magnetic field assistance is applied, i.e. electroplating is performed in a magnetic field-free environment.
The prepared mesh membrane has the surface topography shown in fig. 9: the meshes of the stainless steel mesh are all blocked by micron nickel particles. The application of the vertical magnetic field in the jet electrodeposition process can induce the micron nickel particles to deposit and adsorb on the meshes of the stainless steel net, so as to avoid the mesh blockage. The results prove that the magnetic field assisted jet electrodeposition is an effective method for preparing the oil-water separation mesh membrane loaded with the micron nickel particles.
The invention is not the best known technology.
The above embodiments are merely illustrative of the technical ideas and features of the present invention, and the purpose thereof is to enable those skilled in the art to understand the contents of the present invention and implement the present invention, and not to limit the protection scope of the present invention. All equivalent changes and modifications made according to the spirit of the present invention should be covered within the protection scope of the present invention.
Claims (9)
1. The preparation method of the oil-water separation net film loaded with the micron nickel particles is characterized by comprising the following specific steps of:
step 1) pretreatment of cathode materials: cleaning the stainless steel net, and then airing for later use;
step 2) preparing an electroplating solution: adding micron nickel particles into metal ion electroplating solution, carrying out ultrasonic oscillation and stirring, and uniformly dispersing the micron nickel particles in the electroplating solution;
step 3), preparing a net film: clamping the stainless steel mesh obtained in the step (1) on a workbench of a magnetic field assisted radio-current electrodeposition device, adding the electroplating solution containing micron nickel particles obtained in the step (2) into a water bath of the device, and electrifying to obtain an oil-water separation net film;
step 4) washing the oil-water separation mesh membrane obtained in the step 3 with deionized water to remove residual electroplating solution and micron nickel particles on the surface;
and 5) placing the net film obtained in the step 4 under a ventilation condition, and naturally drying.
2. The method for preparing a micron nickel particle-loaded oil-water separation mesh membrane according to claim 1, wherein the method comprises the following steps: in the step 1, the stainless steel net is cleaned by ultrasonic cleaning of the stainless steel net with acetone, ethanol and deionized water for 10min in sequence.
3. The method for preparing a micron nickel particle-loaded oil-water separation mesh membrane according to claim 1, wherein the method comprises the following steps: in the step 1, the mesh number of the stainless steel mesh is 200-400 meshes, and the size is 50 multiplied by 50 mm.
4. The method for preparing a micron nickel particle-loaded oil-water separation mesh membrane according to claim 1, wherein the method comprises the following steps: in the step 2, the granularity of the used micron particles is 1-3 mu m, the addition amount of the micron nickel particles in the metal ion electroplating solution is 1-4 g/L, and the PH of the used metal ion electroplating solution is adjusted to 3.8-4.2 by using an alkaline solution.
5. The method for preparing a micron nickel particle-loaded oil-water separation mesh membrane according to claim 1, wherein the method comprises the following steps: in the step 2, the ultrasonic oscillation frequency is 30-40 kHz, the stirring speed is 150-200 r/min, and the oscillation stirring is 20-40 min.
6. The method for preparing a micron nickel particle-loaded oil-water separation mesh membrane according to claim 1, wherein the method comprises the following steps: in the step 3, the magnetic field direction of the cathode region is perpendicular to the surface of the cathode stainless steel net, the magnetic field intensity is 50-200 mT, the temperature of the electroplating solution is controlled to be 45-55 ℃ by heating the water bath, the flow rate of the electroplating solution is 140-160L/h, the electrifying voltage is 15-20V, and the deposition time is 10-40 min.
7. An oil-water separation mesh membrane prepared by the method of any one of claims 1 to 6.
8. The oil-water separation mesh membrane of claim 7, wherein: the surface of the oil-water separation net film is loaded with a rough structure formed by micron nickel particles; the pore size of the oil-water separation net film is 5-70 mu m; the water contact angle of the oil-water separation net film in the air is larger than 150 degrees, and the oil contact angle is close to 0 degree.
9. Use of the oil-water separation mesh membrane of claim 7 or 8 in the treatment of oily wastewater.
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Application publication date: 20220215 |