CN111450712A - Preparation method of oil-water separation type copper-based net film material - Google Patents
Preparation method of oil-water separation type copper-based net film material Download PDFInfo
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Abstract
The invention relates to a preparation method of an oil-water separation type copper-based net film material, and belongs to the technical field of oil-water separation materials. The technical proposal of the invention further improves the separation efficiency of the material on the basis of the coating modification of the material, since for surfactant stabilized water-in-oil emulsions, when the water-in-oil emulsion comes into contact with the film, the micro-nano multilevel structure formed on the surface of the film and the oil-water interface surfactant have complex interaction, thereby destroying the stability of the original emulsion and endowing the film with the capability of demulsification, after the demulsification, oil drops are firstly captured by the rough structure on the surface of the film, then the oil drops infiltrate the film and spread rapidly, the thin layer is formed on the surface of the film to prevent water from permeating, so that oil-water separation is realized, and the technical scheme of the invention adopts the crystallization treatment of the molecular sieve coating, the number of times of the coating and enveloping for recycling can be further improved, the recycling service life of the material is further improved, and the separation efficiency of the existing separation mesh material is effectively improved.
Description
Technical Field
The invention relates to a preparation method of an oil-water separation type copper-based net film material, and belongs to the technical field of oil-water separation materials.
Background
Water is a life source and is the most basic element for the stability and development of the whole human society, the life of human beings is an important resource on the earth without water and oil, and the phenomenon of oil content in water and the problem of water content in oil can influence the normal use of water and oil. Leakage in offshore oil transportation can cause marine environmental pollution. The quality of oil is also reduced by doping water in the finished oil, and the use efficiency of the oil is influenced. The oil-water separation problem has been long studied make internal disorder or usurp, and gravity method, centrifugal method and adsorption method are all traditional oil-water separation method, but these methods all have defects. How to overcome the defects of the traditional separation method and research make internal disorder or usurp a new oil-water separation technology becomes a problem to be solved at present.
Oil-water separation has a long history of research and development. Currently, the traditional methods for oil-water separation which have been researched mainly include: physical, chemical, physicochemical, and biological methods. The four methods can be respectively subdivided into a plurality of different methods, such as a gravity method, a centrifugal method, a coagulation method, an adsorption method, a biological filter method and the like, which are widely applied in real life, and the methods can be combined to achieve higher oil-water separation efficiency in practical application.
The treatment method of the oily wastewater mainly comprises gravity separation, centrifugal separation, electric separation, adsorption separation, air flotation separation, heating oil-water separation and the like. These separation methods have problems of low separation efficiency, large energy consumption, secondary pollution, high treatment cost, and the like. Therefore, continuous exploration is needed in the field of oil-water separation, a novel oil-water separation technology with low cost and low energy consumption is developed, the oil-water separation efficiency is improved, and the pollution to the environment in the separation process is reduced.
The water content of the aqueous oil is below 30%, and the water content of the aqueous oil after treatment can be lower than 0.5% by the electric dehydration treatment method which is invented in the beginning of the 20 th century for the part of the aqueous oil. However, with the continuous development of tertiary oil recovery technology and the exploitation of heavy oil reservoirs, the emulsification of water-containing oil becomes more complex and has strong stability, and the method is difficult to process, and at present, the method mainly comprises technical methods such as ultrasonic wave, heating, microwave, rotational flow, electric pulse, chemical methods (such as adding demulsifier), magnetic treatment and the like. These methods have the problems of large energy consumption, easy secondary pollution and the like.
The treatment method of the oily wastewater mainly comprises gravity separation, centrifugal separation, electric separation, adsorption separation, air flotation separation, heating oil-water separation and the like. These separation methods have problems of low separation efficiency, large energy consumption, secondary pollution, high treatment cost, and the like.
With the continuous deepening of make internal disorder or usurp research on the surface wettability of materials, methods for preparing surfaces with special wettability such as super-hydrophilicity, super-hydrophobicity, super-oleophylicity and super-oleophylicity are mastered at present. According to the special wettability surfaces, the combination of the special wettability of an aqueous phase and the special wettability of an oil phase can further obtain a super-hydrophobic/super-oleophilic surface, a super-oleophobic/super-hydrophilic surface, a double super-hydrophobic surface and a double super-hydrophilic surface. Wherein, the super-hydrophobic/super-oleophilic surface and the super-oleophobic/super-hydrophilic surface have completely opposite wetting phenomena for water and oil, so the method can be applied to the field of oil-water separation.
The oil-water separation process comprises the separation of oil-containing wastewater and water-containing oil. The oily wastewater has wide source and large content. A large amount of oily wastewater is generated in the industries of petroleum industry, manufacturing industry, transportation, food and restaurant and the like. The oil-containing waste water source of the petroleum industry mainly comprises the processes of exploration and development, crude oil pipeline transportation, oil tanker leakage, discharge, accident occurrence and the like; the process of the spillover and blowout in the process of exploiting the seabed oil field. Oil pollutants can cause great harm to marine life, human health, water resources, atmosphere and the like. Therefore, the pollutants are required to be separated so as to achieve the purposes of recycling and standard emission, and the method has great significance for protecting the environment, saving resources and the like.
The membrane separation is a simple and efficient oil-water separation technology. At present, the oil-water separation membrane is mainly constructed by carrying out hydrophilic and hydrophobic modification on the surface of a substrate, wherein the substrate comprises polymers, stainless steel, filter cloth and the like. But has the defects of small water flux, quick attenuation, small treatment capacity, poor pollution resistance and the like. Therefore, development of a novel high-efficiency oil-water separation technology and a high-efficiency and low-cost water system pollution treatment method by make internal disorder or usurp is urgent. In addition, the oil industry also needs a new oil-water separation process to increase oil recovery.
Disclosure of Invention
The technical problems to be solved by the invention are as follows: aiming at the problems of low separation efficiency, high energy consumption, large occupied area and possibility of causing secondary pollution in the traditional method, the preparation method of the oil-water separation type copper-based net film material is provided.
In order to solve the technical problem of the preparation method of the oil-water separation type copper-based mesh film material, the invention adopts the following technical scheme:
(1) taking a copper mesh, washing the copper mesh for 3-5 times by using hydrochloric acid, washing and drying to obtain a surface treatment copper mesh material, respectively weighing 45-50 parts by weight of deionized water, 3-5 parts by weight of sulfuric acid with the mass fraction of 5% and 1% by weight of copper sulfate into a beaker, stirring and mixing to obtain an electrodeposition solution, taking the surface treatment copper mesh material as a cathode and the copper plate as an anode, placing the electrode in a numerical control double-pulse electroplating device, and carrying out electroplating treatment, washing and drying to obtain a deposition copper mesh;
(2) placing the deposited copper mesh in an ethanol solution, soaking, drying in vacuum to obtain a modified deposited copper mesh, respectively weighing 45-50 parts by weight of deionized water, 15-20 parts by weight of 10% hydrochloric acid and 15-20 parts by weight of the modified deposited copper mesh in a beaker, standing, washing to be neutral, soaking in a stearic acid ethanol solution, taking out and drying to obtain a coated modified copper mesh material;
(3) adding sodium aluminate into a sodium hydroxide solution with the mass fraction of 5% according to the mass ratio of 1:10, stirring, mixing and standing to obtain a sodium aluminate composite modified solution, adding silica sol into deionized water according to the mass ratio of 1:8, and stirring and mixing to obtain a silica sol composite solution;
(4) dropwise adding the sodium aluminate composite modified solution into the silica sol composite solution according to the volume ratio of 1:9, stirring and mixing at room temperature for 3-5 h to obtain a coating modified solution, aging the coating modified solution at room temperature, adding the coating modified copper mesh material into the coating modified solution, standing, performing crystallization treatment, collecting a crystallized and coated copper mesh, and performing vacuum drying to obtain the oil-water separation type copper-based mesh material.
The copper mesh is 120-180 meshes.
The hydrochloric acid washing adopts 1 percent by mass of hydrochloric acid.
The distance between the anode and the cathode is 3-5 cm.
The electroplating treatment is carried out for 200-300 s under the condition that the control voltage is 4V.
The solid content of the silica sol is 15%.
The crystallization treatment is performed for 10-12 hours at 100-110 ℃.
The vacuum drying is carried out for 2-3 h at 120-125 ℃.
The concentration of the ethanol solution is 0.025 mol/L.
Compared with other methods, the method has the beneficial technical effects that:
(1) the technical scheme of the invention effectively reacts by composite etching and deposition treatment of copper chloride and hydrochloric acid, a branch-shaped micro-nano structure is formed on the surface of a copper-based material in an overall reaction state, meanwhile, the technical scheme of the invention adopts a low surface energy material for coating modification, and further, an effective component has a super-hydrophobic oleophilic surface structure with the characteristic of a bionics super-hydrophobic surface, when an oil-water mixture is treated, because the surface tension between oil and water generally has a larger difference, the bionic interface oil-water separation material can selectively only infiltrate an oil phase or a water phase and repel the other phase by utilizing different infiltration performances of the surface of the bionic interface oil-water separation material on the liquid, thereby effectively improving the oil-water separation efficiency, simultaneously, stearic acid is adopted for coating modification, and compact coating modification films form a close-packed structure at different angles, the water drops quickly fall off on the surface of the water drop, because the water drops can not penetrate into gaps between the compact membranes of the material and stay on the composite surface formed by the petal sections and air, the water drops slide off when being inclined slightly, the oil drops quickly disperse on the surface of the water drops and can penetrate into the gaps between the compact membranes, because nonpolar acting force exists between the oil drops and oil molecules, the oil drops can penetrate into the gaps between the membrane materials in a short time by virtue of the mutual acting force, and the separation performance of the oil-water separation net material prepared in the technical scheme of the invention is further improved;
(2) the technical proposal of the invention further improves the separation efficiency of the material on the basis of the coating modification of the material, since for surfactant stabilized water-in-oil emulsions, when the water-in-oil emulsion comes into contact with the film, the micro-nano multilevel structure formed on the surface of the film and the oil-water interface surfactant have complex interaction, thereby destroying the stability of the original emulsion and endowing the film with the capability of demulsification, after the demulsification, oil drops are firstly captured by the rough structure on the surface of the film, then the oil drops infiltrate the film and spread rapidly, the thin layer is formed on the surface of the film to prevent water from permeating, so that oil-water separation is realized, and the technical scheme of the invention adopts the crystallization treatment of the molecular sieve coating, the number of times of the coating and enveloping for recycling can be further improved, the recycling service life of the material is further improved, and the separation efficiency of the existing separation mesh material is effectively improved.
Detailed Description
Taking a 120-180-mesh copper net, washing the copper net with 1% by mass hydrochloric acid for 3-5 times, washing the copper net with absolute ethyl alcohol for 3-5 times, rinsing the copper net with deionized water until a washing solution is neutral, drying the washed copper net at 45-50 ℃ for 1-2 hours to obtain a surface-treated copper net material, weighing 45-50 parts by weight of deionized water, 3-5 parts by weight of 5% by mass sulfuric acid and 1% by mass of copper sulfate into a beaker, stirring and mixing the materials to obtain an electrodeposition solution, taking the surface-treated copper net material as a cathode, taking a copper plate as an anode, controlling the distance between the anode and the cathode to be 3-5 cm, placing the electrode into a numerical control double-pulse electroplating device, controlling the voltage to be 4V, electroplating for 200-300 s, washing the surface-treated copper net with deionized water until the washing solution is neutral, drying the surface-treated copper net at 55-65 ℃ for 10-20 min to obtain a deposited copper net, placing the deposited copper net into a 0.025 mol/L ethanol solution, soaking the modified copper net in a modified composite sodium aluminate solution for 10-15 min, drying the modified copper net with a modified silica sol with a weight ratio of 20-10 h, adding the sodium hydroxide solution to 10-10 h, stirring the modified sodium aluminate solution, drying the modified silica-10 h, mixing the sodium aluminate-10-2-10-2-10-1-10-0-10-2-10-0-2-1-2-10-1-2-1-10-2-1-2-0-2-10-4-2.
Example 1
Washing a 120-mesh copper net with 1 mass percent hydrochloric acid for 3 times, washing with absolute ethyl alcohol for 3 times, finally leaching with deionized water until the washing liquid is neutral, drying at 45 ℃ for 1h to obtain a surface-treated copper net material, weighing 45 parts by weight of deionized water, 3 parts by weight of 5 mass percent sulfuric acid and 1 mass percent copper sulfate respectively into a beaker, stirring and mixing to obtain an electrodeposition liquid, taking the surface-treated copper net material as a cathode, taking a copper plate as an anode, controlling the distance between the anode and the cathode to be 3cm, placing the electrode into a numerical control double-pulse electroplating device, controlling the voltage to be 4V, after electroplating for 200s, washing the copper net with deionized water until the washing liquid is neutral, drying at 55 ℃ for 10min to obtain a deposited copper net, placing the deposited copper net into a 0.025 mol/L sodium aluminate solution, soaking for 10min, vacuum drying to obtain a modified deposited copper net, weighing 45 parts by weight of deionized water, 15 parts by mass percent of 10 percent hydrochloric acid and 15 parts by weight of the modified copper net in a calcined copper net, placing the sodium aluminate in a 0.025 mol/L ethanol solution, soaking for 10min, drying, adding the modified silicon-coated copper net material into a modified copper net, stirring, drying at room temperature, mixing to obtain a modified silicon-coated composite solution, drying solution, adding a modified copper-coated composite modified silicon-coated solution, drying solution, stirring solution, drying solution with a modified silicon-coated copper net material, stirring solution with a modified silicon-coated by weight ratio of 10% modified copper net solution of 10% modified copper net, stirring solution of 10h, stirring at room temperature of 10, stirring, and a modified silicon-coated solution, stirring ratio of 10h, stirring solution, drying at room temperature of 10h, drying, and a room temperature ratio of a modified silicon-coated copper net-coated copper net-coated.
Example 2
Washing a 150-mesh copper net with 1 mass percent hydrochloric acid for 4 times, washing with absolute ethyl alcohol for 4 times, finally leaching with deionized water until the washing liquid is neutral, drying at 47 ℃ for 1.5 hours to obtain a surface-treated copper net material, weighing 47 parts by weight of deionized water, 4 parts by weight of 5 mass percent sulfuric acid and 1 mass percent copper sulfate in a beaker respectively, stirring and mixing to obtain an electrodeposition liquid, washing the surface-treated copper net material as a cathode, a copper plate as an anode, controlling the distance between the anode and the cathode to be 4cm, placing the electrode in a numerical control double-pulse electroplating device, controlling the voltage to be 4V, after electroplating for 250s, washing the copper net with deionized water until the washing liquid is neutral, drying at 60 ℃ for 15 minutes to obtain a deposited copper net, placing the deposited copper net in 0.025 mol/L mol/ethanol solution, soaking for 13 minutes, drying in vacuum to obtain a deposited copper net, weighing 47 parts by weight of deionized water, 17 parts by mass percent 10 percent hydrochloric acid and 17 parts by weight of modified copper net, placing the deposited copper net in the beaker, placing the sodium aluminate in the sodium aluminate, after soaking for 13 minutes, drying, placing the sodium aluminate in a modified silicon hydroxide composite solution, mixing, drying at room temperature, mixing and drying, obtaining a modified silicon-coated composite modified copper net material, placing the sodium aluminate solution, placing the sodium aluminate after the sodium aluminate, placing the sodium aluminate, after the sodium aluminate, placing the sodium hydroxide solution, the sodium aluminate, after the sodium aluminate, after the sodium aluminate, the sodium silicate is mixed solution with the sodium silicate, the sodium silicate.
Example 3
Washing a 180-mesh copper net with 1 mass percent hydrochloric acid for 5 times, washing with absolute ethyl alcohol for 5 times, leaching with deionized water until the washing liquid is neutral, drying at 50 ℃ for 2 hours to obtain a surface-treated copper net material, weighing 50 parts by weight of deionized water, 5 parts by weight of 5 mass percent sulfuric acid and 1 mass percent copper sulfate respectively into a beaker, stirring and mixing to obtain an electrodeposition liquid, using the surface-treated copper net material as a cathode, using a copper plate as an anode, controlling the distance between the anode and the cathode to be 5cm, placing the electrode into a numerical control double-pulse electroplating device, controlling the voltage to be 4V, after electroplating for 300s, washing with deionized water until the washing liquid is neutral, drying at 65 ℃ for 20 minutes to obtain a deposited copper net, placing the deposited copper net into a 0.025 mol/L sodium aluminate solution, soaking for 15 minutes, drying in vacuum to obtain a modified deposited copper net, weighing 50 parts by weight of deionized water, 20 parts by weight of 10 mass percent hydrochloric acid and 20 parts of the modified deposited copper net, placing the copper net into the beaker, placing the sodium aluminate in a 0.025 mol/L sodium aluminate solution, placing the modified copper net in a modified silicon-coated composite solution, stirring and drying, mixing, adding the modified copper net material, after the solution, stirring, drying at room temperature, mixing, drying, adding the modified copper net material, and drying, the modified copper net material, the modified silicon-coated with a modified copper net material, and drying solution at a ratio of 10 mass percent aqueous solution of 10, stirring, obtaining a modified copper net, mixing, and drying at room temperature, and drying, obtaining a modified copper net, mixing, and drying, obtaining a modified copper-coated by weight ratio of 10 percent modified copper-coated copper net, and drying solution, and drying, and mixing, obtaining a modified copper-coated composite solution, and drying solution, and a modified copper-coated copper-.
The oil-water separation type copper-based mesh membrane material and the common oil-water separation membrane prepared by the invention are subjected to performance detection, and specific detection results are shown in the following table 1.
The test method comprises the following steps:
performance testing
Oil-water separation experiment
Oil-water separation experiments were conducted using examples 1-3 and comparative example described above. Before the oil-water separation experiment, oil and water are stirred and mixed at a high speed (the volume ratio of oil to water is 50/50), the rotating speed is 3000rpm/s, and the stirring time is 30 min.
Flux assay
The experiment was carried out by mixing 175m L oil and 175m L water, and then carrying out an oil-water separation experiment in which the water rapidly passed through a stainless steel mesh, wherein the crude oil and water mixture was separated by passing completely through the water phase for 15s and the gasoline and water mixture was separated by passing completely through the water phase for 13 s.
Determination of oil content and separation efficiency
And (3) measuring the oil content in the separated water phase by using an infrared oil meter, wherein the measuring method comprises the following steps: pouring a certain volume of water sample into a separating funnel, adding hydrochloric acid for acidification until the pH value is less than or equal to 2, washing a sampling bottle by using 20ml of carbon tetrachloride, transferring the sampling bottle into the separating funnel, adding about 20g of sodium chloride, fully oscillating for 2min, and frequently opening a piston for exhausting. After standing for stratification, the extract was poured into a volumetric flask through a glass sand core funnel in which anhydrous sodium sulfate having a thickness of about 10mm had been placed. The extraction was repeated once with 20ml of carbon tetrachloride. And (3) taking a proper amount of carbon tetrachloride to wash the glass sand core funnel, and enabling the washing liquid to flow into the volumetric flask together. Adding carbon tetrachloride to dilute to the constant volume of the marked line, and shaking up. The Oil content was measured with an infrared Oil tester (Oil 460, produced by Wako instruments & technologies, Beijing).
TABLE 1 characterization of oil-water separation type copper-based mesh material
As can be seen from Table 1, the oil-water separation type copper-based mesh membrane prepared by the method disclosed by the invention is high in flux, high in oil-water separation efficiency and flux retention rate, and can be repeatedly used.
Claims (9)
1. The preparation method of the oil-water separation type copper-based net film material is characterized by comprising the following specific preparation steps:
(1) taking a copper mesh, washing the copper mesh for 3-5 times by using hydrochloric acid, washing and drying to obtain a surface treatment copper mesh material, respectively weighing 45-50 parts by weight of deionized water, 3-5 parts by weight of sulfuric acid with the mass fraction of 5% and 1% by weight of copper sulfate into a beaker, stirring and mixing to obtain an electrodeposition solution, taking the surface treatment copper mesh material as a cathode and the copper plate as an anode, placing the electrode in a numerical control double-pulse electroplating device, and carrying out electroplating treatment, washing and drying to obtain a deposition copper mesh;
(2) placing the deposited copper mesh in an ethanol solution, soaking, drying in vacuum to obtain a modified deposited copper mesh, respectively weighing 45-50 parts by weight of deionized water, 15-20 parts by weight of 10% hydrochloric acid and 15-20 parts by weight of the modified deposited copper mesh in a beaker, standing, washing to be neutral, soaking in a stearic acid ethanol solution, taking out and drying to obtain a coated modified copper mesh material;
(3) adding sodium aluminate into a sodium hydroxide solution with the mass fraction of 5% according to the mass ratio of 1:10, stirring, mixing and standing to obtain a sodium aluminate composite modified solution, adding silica sol into deionized water according to the mass ratio of 1:8, and stirring and mixing to obtain a silica sol composite solution;
(4) dropwise adding the sodium aluminate composite modified solution into the silica sol composite solution according to the volume ratio of 1:9, stirring and mixing at room temperature for 3-5 h to obtain a coating modified solution, aging the coating modified solution at room temperature, adding the coating modified copper mesh material into the coating modified solution, standing, performing crystallization treatment, collecting a crystallized and coated copper mesh, and performing vacuum drying to obtain the oil-water separation type copper-based mesh material.
2. The method for preparing an oil-water separation type copper-based mesh film material according to claim 1, wherein the method comprises the following steps: the copper mesh is 120-180 meshes.
3. The method for preparing an oil-water separation type copper-based mesh film material according to claim 1, wherein the method comprises the following steps: the hydrochloric acid washing adopts 1 percent by mass of hydrochloric acid.
4. The method for preparing an oil-water separation type copper-based mesh film material according to claim 1, wherein the method comprises the following steps: the distance between the anode and the cathode is 3-5 cm.
5. The method for preparing an oil-water separation type copper-based mesh film material according to claim 1, wherein the method comprises the following steps: the electroplating treatment is carried out for 200-300 s under the condition that the control voltage is 4V.
6. The method for preparing an oil-water separation type copper-based mesh film material according to claim 1, wherein the method comprises the following steps: the solid content of the silica sol is 15%.
7. The method for preparing an oil-water separation type copper-based mesh film material according to claim 1, wherein the method comprises the following steps: the crystallization treatment is performed for 10-12 hours at 100-110 ℃.
8. The method for preparing an oil-water separation type copper-based mesh film material according to claim 1, wherein the method comprises the following steps: the vacuum drying is carried out for 2-3 h at 120-125 ℃.
9. The method for preparing an oil-water separation type copper-based mesh film material according to claim 1, wherein the concentration of the ethanol solution is 0.025 mol/L.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112386952A (en) * | 2020-10-10 | 2021-02-23 | 重庆工商大学 | Emulsified oil liquid purification device based on super-hydrophobic/super-lipophilic screen net film |
| CN113522046A (en) * | 2021-08-27 | 2021-10-22 | 东北电力大学 | Metal microfiltration membrane and preparation method and application thereof |
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2020
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112386952A (en) * | 2020-10-10 | 2021-02-23 | 重庆工商大学 | Emulsified oil liquid purification device based on super-hydrophobic/super-lipophilic screen net film |
| CN113522046A (en) * | 2021-08-27 | 2021-10-22 | 东北电力大学 | Metal microfiltration membrane and preparation method and application thereof |
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