CN111717968A - Preparation method of demulsification electrode for oil-containing sewage electric field - Google Patents
Preparation method of demulsification electrode for oil-containing sewage electric field Download PDFInfo
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Abstract
The invention relates to a preparation method of an electric field demulsification electrode for oily sewage, which comprises the steps of soaking a metal substrate in water, and removing solid impurities on the surface of the metal substrate under the ultrasonic condition; soaking the metal substrate subjected to ultrasonic treatment in an acid solution to remove oil stains on the surface of the metal, and drying for later use; soaking the dried metal substrate in sulfuric acid to form a metal oxide film on the metal surface; washing to remove sulfuric acid on the surface of the metal substrate, and drying for later use; and coating a layer of hydrophobic organic porous film on the surface of the metal substrate to obtain the oily sewage electric field demulsification electrode. The electrode prepared by the invention reduces the production cost, effectively relieves the phenomena of dissolution and passivation compared with the traditional electrode, and prolongs the service life of the electrode.
Description
Technical Field
The invention belongs to the technical field of oily sewage treatment, and particularly relates to a preparation method of an oily sewage electric field demulsification electrode.
Background
Oil pollutants in water are common pollutant types in industrial sewage, and the oily sewage is generated in various industries such as petroleum exploitation, petroleum refining, food processing, mechanical manufacturing and the like. At present, the oily sewage treatment technology comprises oil removal, coagulating sedimentation, air flotation, filtration and other technologies. For oily sewage with relatively large oil drop particle size and low emulsification degree, physical technologies such as oil separation, air floatation, filtration and the like are adopted, and oil pollutants in water are effectively removed by depending on oil-water density difference and the like, however, for high-emulsification oily sewage (such as chemical flooding produced water and the like), the oil drop particle size in the water is small, the oil drop property is stable, and the oil-water separation difficulty is higher.
For a plurality of oily sewage treatment technologies, effective oil removal of highly emulsified oily sewage needs to be realized, and firstly, efficient demulsification is needed, the stable state of an oil-water emulsion is broken, and oil-water separation can be effectively realized through physical oil removal processes such as air floatation and the like. The method is characterized in that the oily sewage is treated by adopting a coagulating sedimentation technology, chemical demulsifiers such as PAC (polyaluminium chloride) are added into the water, and the purpose of chemical demulsification is achieved by compressing the action mechanisms such as the double electric layer structure of dispersed-phase oil drops in the sewage. However, in the process, a coagulant such as PAC (generally 150mg/L or more) needs to be added into the sewage, a large amount of sludge is generated after the reaction, the sludge is a hazardous waste, the treatment and disposal cost is high, and the generation of a large amount of sludge brings heavy maintenance work to daily operation of sewage treatment. Compared with a chemical demulsification technology, the electric field demulsification technology has the advantages of no chemical agent addition, less oil sludge generation amount, compact and efficient equipment and the like in recent years, and is gradually paid attention by researchers. However, the conventional electric field demulsification technology is mainly used for demulsification and dehydration of W/O type emulsion (for example, electric field demulsification and dehydration in crude oil), while relatively few electric field demulsification (for example, oil-containing sewage) of O/W type emulsion is studied. At present, metal electrode materials such as iron and aluminum are directly adopted, the problems of electrode dissolution, passivation and the like are easily caused, and the demulsification efficiency of the electrode is difficult to maintain effectively for a long time. The electric field demulsification treatment of the high-emulsification oily sewage requires more efficient and stable electrode materials. For the electric field demulsification technology of oily sewage, one of the important problems to be solved is to ensure the high efficiency and stability of the electrode material in the sewage treatment process to realize the engineering application of the electric field demulsification technology.
A related application disclosed in the prior art, for example, a patent with Chinese patent publication No. CN88200107U (published in 26.7.9.1989), discloses a novel high-voltage electrostatic emulsion breaker electrode, in which metallic copper is used as an electrode substrate, polyvinylidene fluoride or polyvinyl fluoride with the thickness of 0.5-4mm is coated on the outer layer of the substrate, and water-in-oil (W/O) emulsion (such as crude oil) is subjected to electric field emulsion breaking under the condition of an electric field with the voltage of 2-20 KV. The electrode is used for electric field demulsification of W/O type emulsion such as crude oil, belongs to a high-voltage electrode due to the fact that the surface of the electrode is coated with a compact insulating high-molecular organic matter coating, can generate a breakdown phenomenon when the water content in the emulsion is higher, and cannot be used for electric field demulsification of oily sewage.
Chinese patent application No. 201911169514.9 (published 3/31/2020) discloses a method for preparing a titanium-based titanium suboxide electrode, which comprises preparing a titanium dioxide layer on a titanium substrate by using a metal titanium plate as a substrate and performing direct current sputtering, and reducing the titanium dioxide layer to a titanium suboxide layer to obtain the titanium suboxide electrode. The electrode prepared by the method is mainly used for removing organic matters in wastewater through electrocatalytic oxidation, expensive materials such as metal titanium and the like are needed for preparing the electrode, and requirements on preparation materials, equipment, operating conditions and the like are relatively high.
Chinese patent application No. 201910373223.5 (published in 2019, 8/6) discloses a concentric double-electrode discharge plasma O/W emulsion breaking device, which is characterized in that an isolation medium made of quartz material is sleeved around a metal electrode, a high-voltage electric field is applied to the metal electrode, and electrons are enriched outside the isolation medium, thereby generating an emulsion breaking electric field. Due to the shielding effect of the quartz material on the electrode electric field, the electric field intensity generated outside the isolation medium is relatively weak, so that the requirement on the field intensity of the oil-containing sewage electric field demulsification is difficult to meet on one hand, and on the other hand, the electric energy waste is also caused.
In addition, part of researchers directly adopt metals such as iron, aluminum and the like as demulsification electrodes, and relevant process research of electric field demulsification is carried out, so that the demulsification effectiveness of the low-voltage electric field on the high-emulsification oily sewage is proved. However, the problem of electrode dissolution, passivation and the like is easily caused by directly adopting metal electrode materials such as iron, aluminum and the like, and the demulsification efficiency of the electrode is difficult to maintain effectively for a long time, so that the problem cannot be solved effectively all the time.
The present invention has been made in view of the above circumstances.
Disclosure of Invention
Compared with the traditional metal electrode, the electrode prepared by the invention effectively relieves the phenomena of dissolution and passivation, ensures the demulsification effect of the electric field and prolongs the service life of the electrode.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of an oil-containing sewage electric field demulsification electrode comprises the following steps:
(1) surface ultrasonic impurity removal: soaking the metal substrate in water, and removing solid impurities on the surface of the metal substrate under the ultrasonic condition;
(2) surface pickling for oil removal: soaking the metal substrate subjected to ultrasonic treatment in an acid solution to remove oil stains on the surface of the metal, and drying for later use;
(3) oxidation by strong acid: soaking the dried metal substrate in sulfuric acid to form a metal oxide film on the metal surface;
(4) cleaning and drying: washing to remove sulfuric acid on the surface of the metal substrate, and drying for later use;
(5) coating a hydrophobic film: and (4) coating a layer of hydrophobic organic porous film on the surface of the metal substrate for standby in the step (4) to obtain the oily sewage electric field demulsification electrode.
Further, the metal substrate in the step (1) is iron or aluminum.
Further, the thickness of the metal substrate is 1.0-2.0 mm.
Further, the ultrasonic frequency in the step (1) is 28-40KHz, and the ultrasonic treatment time is 15-30 min.
Further, the acidic solution in the step (2) is prepared by dissolving sulfuric acid or hydrochloric acid in water.
Further, the mass percentage concentration of the acidic solution is 0.5-3%.
Further, the temperature of the acidic solution is 20-40 ℃.
Further, the soaking time of the metal substrate subjected to ultrasonic treatment in the step (2) in the acid solution is 10-20 min.
Further, the mass percentage concentration of the sulfuric acid in the step (3) is 72-98%.
Further, the time for soaking the metal substrate in sulfuric acid is 30-45 min.
Further, in the step (4), deionized water is adopted to wash the sulfuric acid on the surface of the metal substrate, and the washing time is less than 2 min.
The metal oxide is formed on the surface of the metal substrate, and the metal oxide improves the passivation resistance of the substrate.
Further, the pH of the residual moisture on the surface of the metal substrate after rinsing is more than 6.0.
Further, the material of the hydrophobic organic porous film in the step (5) is polytetrafluoroethylene, polypropylene or polyethylene.
Further, the thickness of the hydrophobic organic porous film is 0.5-1.0 mm.
The hydrophobic organic porous film only allows water molecules and inorganic salt ions to pass through due to small micropore diameter of the surface, and oil drops with relatively large particle size gather and move to the surface of the film under the action of an external electric field between electrodes to promote the oil drops to coalesce on the surface of the film, but cannot pass through micropores on the film due to large particle size. The film can prevent oil drops from directly accumulating on the surface of a metal polar plate to form an oil stain passivation film layer on one hand, and can effectively promote the oil drop coalescence effect on the other hand due to the hydrophobic property of the film. Furthermore, the surface of the hydrophobic organic porous membrane has a microporous structure, and the pore diameter is 0.1-0.5 μm.
Compared with the prior art, the invention has the beneficial effects that:
(1) the electrode in the invention adopts traditional materials such as iron, aluminum metal, polytetrafluoroethylene and the like as raw materials, the materials are easy to obtain and low in price, and the production cost of the electrode is reduced, so that the investment and operation cost of the electric field demulsification technology is reduced;
(2) compared with the traditional metal electrode, the electrode prepared by the invention effectively relieves the phenomena of dissolution and passivation, ensures the demulsification effect of an electric field and prolongs the service life of the electrode;
(3) the electrode prepared by the invention can be suitable for various electric field forms such as direct current, pulse direct current and the like, can be applied to demulsification of various high-emulsification oily sewage such as oilfield produced water, oil refining sewage, food processing oily sewage, mechanical processing oily sewage and the like, has obviously improved pretreatment capability compared with the efficiency of the traditional physical oil-water separation process, and has wide popularization and application prospects.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a schematic flow chart of the preparation method of the demulsification electrode for the oily sewage electric field.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention will be described in detail below. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the examples given herein without any inventive step, are within the scope of the present invention.
FIG. 1 is a schematic flow chart of the method for preparing the demulsification electrode for the electric field of oily sewage.
Example 1
The preparation method of the demulsification electrode for the oil-containing sewage electric field comprises the following steps:
(1) surface ultrasonic impurity removal: soaking a metal substrate in water, wherein the metal substrate is an iron plate, the thickness of the metal substrate is 1.0mm, and under the ultrasonic condition, removing solid impurities on the surface of the metal substrate, wherein the ultrasonic frequency is 28KHz, and the ultrasonic treatment time is 30 min;
(2) surface pickling for oil removal: soaking the metal substrate subjected to ultrasonic treatment in an acid solution for 10min, wherein the acid solution is obtained by dissolving sulfuric acid in water, the mass percentage concentration of the acid solution is 0.5%, the temperature of the acid solution is 20 ℃, removing oil stains on the surface of the metal, and drying the metal substrate in an oven for later use;
(3) oxidation by strong acid: soaking the dried metal substrate in sulfuric acid for 30min, wherein the mass percentage concentration of the sulfuric acid is 72%, and forming a metal oxide film on the metal surface through chemical oxidation;
(4) cleaning and drying: washing the sulfuric acid on the surface of the metal substrate by using deionized water, wherein the washing time is less than 2min, and drying the washed residual water on the surface of the metal substrate in an oven with the pH value of more than 6.0 for later use;
(5) coating a hydrophobic film: and (3) coating a layer of hydrophobic organic porous film on the surface of the metal substrate prepared in the step (4) by adopting a blanching process, wherein the hydrophobic organic porous film is made of polytetrafluoroethylene, the thickness of the hydrophobic organic porous film is 0.5mm, the surface of the hydrophobic organic porous film has a microporous structure, and the pore diameter is 0.1 mu m, so that the oily sewage electric field demulsification electrode is obtained.
Example 2
The preparation method of the demulsification electrode for the oil-containing sewage electric field comprises the following steps:
(1) surface ultrasonic impurity removal: soaking a metal substrate in water, wherein the metal substrate is an aluminum plate, the thickness of the metal substrate is 1.5mm, and under the ultrasonic condition, removing solid impurities on the surface of the metal substrate, the ultrasonic frequency is 34KHz, and the ultrasonic treatment time is 22 min;
(2) surface pickling for oil removal: soaking the metal substrate subjected to ultrasonic treatment in an acid solution for 15min, wherein the acid solution is obtained by dissolving sulfuric acid in water, the mass percentage concentration of the acid solution is 1.75%, the temperature of the acid solution is 30 ℃, removing oil stains on the surface of the metal, and drying the metal substrate in an oven for later use;
(3) oxidation by strong acid: soaking the dried metal substrate in sulfuric acid for 37.5min, wherein the mass percentage concentration of the sulfuric acid is 85%, and forming a metal oxide film on the metal surface through chemical oxidation;
(4) cleaning and drying: washing the sulfuric acid on the surface of the metal substrate by using deionized water, wherein the washing time is less than 2min, and drying the washed residual water on the surface of the metal substrate in an oven with the pH value of more than 6.0 for later use;
(5) coating a hydrophobic film: and (3) coating a layer of hydrophobic organic porous film on the surface of the metal substrate prepared in the step (4) by adopting a blanching process, wherein the hydrophobic organic porous film is made of polypropylene, the thickness of the hydrophobic organic porous film is 0.75mm, the surface of the hydrophobic organic porous film has a microporous structure, and the pore diameter is 0.3 mu m, so that the oily sewage electric field demulsification electrode is obtained.
Example 3
The preparation method of the demulsification electrode for the oil-containing sewage electric field comprises the following steps:
(1) surface ultrasonic impurity removal: soaking a metal substrate in water, wherein the metal substrate is an iron plate, the thickness of the metal substrate is 2.0mm, removing solid impurities on the surface of the metal substrate under the ultrasonic condition, the ultrasonic frequency is 40KHz, and the ultrasonic treatment time is 15 min;
(2) surface pickling for oil removal: soaking the metal substrate subjected to ultrasonic treatment in an acidic solution for 20min, wherein the acidic solution is obtained by dissolving sulfuric acid in water, the mass percentage concentration of the acidic solution is 3%, the temperature of the acidic solution is 40 ℃, removing oil stains on the surface of the metal, and drying the metal substrate in an oven for later use;
(3) oxidation by strong acid: soaking the dried metal substrate in sulfuric acid for 45min, wherein the mass percentage concentration of the sulfuric acid is 98%, and forming a metal oxide film on the metal surface through chemical oxidation;
(4) cleaning and drying: washing the sulfuric acid on the surface of the metal substrate by using deionized water, wherein the washing time is less than 2min, and drying the washed residual water on the surface of the metal substrate in an oven with the pH value of more than 6.0 for later use;
(5) coating a hydrophobic film: and (3) coating a layer of hydrophobic organic porous film on the surface of the metal substrate prepared in the step (4) by adopting a hot ironing process, wherein the hydrophobic organic porous film is made of polyethylene, the thickness of the hydrophobic organic porous film is 1.0mm, the surface of the hydrophobic organic porous film has a microporous structure, and the pore diameter is 0.5 mu m, so as to obtain the oily sewage electric field demulsification electrode.
Test example 1
Preparing oilfield produced water: weighing 2.0ml of kerosene, 800.2 g of Tween and 5.0g of NaCl in a beaker, fixing the volume to 1.0L by using deionized water, rapidly shearing for 10min at the speed of 10000rpm by using a T50 high-speed shearing machine to prepare the oilfield produced water with the oil concentration of about 700-plus-one 1000mg/L, and detecting the particle size distribution range of oil drops in the produced water by using a Mastersizer2000 laser particle sizer as shown in Table 1.
TABLE 1 oilfield produced Water oil droplet size distribution
| Serial number | Particle size (. mu.m) | Volume ratio (V%) |
| 1 | 0～2 | 27.37 |
| 2 | 2～20 | 70.57 |
| 3 | 20～200 | 2.06 |
| 4 | 200～2000 | 0 |
The electrodes prepared in examples 1-3 were used to perform electric field demulsification on the oilfield produced water prepared as described above. Adding 1.0L of produced water into an electric field demulsification reactor, wherein the size of a polar plate is 16cm multiplied by 6.5cm, the number of the polar plates is 2 (the number of cathode plates and the number of anode plates are respectively 1), and the distance between the polar plates is 1.5 cm. Setting power supply parameters as voltage 5.0V, frequency 10000Hz and total duty ratio 50%, starting the power supply, reacting for 15min, taking liquid surface supernatant, and measuring the oil drop particle size.
After demulsification by the electric field, the oil droplet size distribution is shown in table 2.
TABLE 2 oil droplet size distribution after demulsification by electric field
As can be seen from tables 1 and 2, after the electrode prepared by the invention is used for demulsification, the proportion of oil drops with the particle size of more than 20 microns in raw water is obviously improved, the particle size of the oil drops in the water is obviously improved, and the electrode has a good demulsification effect on oil drops which are highly emulsified in the water.
The above description is only for the specific embodiments of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art can easily conceive of the changes or substitutions within the technical scope of the present invention, and all the changes or substitutions should be covered within the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the appended claims.
Claims (10)
1. A preparation method of an oil-containing sewage electric field demulsification electrode is characterized by comprising the following steps:
(1) surface ultrasonic impurity removal: soaking the metal substrate in water, and removing solid impurities on the surface of the metal substrate under the ultrasonic condition;
(2) surface pickling for oil removal: soaking the metal substrate subjected to ultrasonic treatment in an acid solution to remove oil stains on the surface of the metal, and drying for later use;
(3) oxidation by strong acid: soaking the dried metal substrate in sulfuric acid to form a metal oxide film on the metal surface;
(4) cleaning and drying: washing to remove sulfuric acid on the surface of the metal substrate, and drying for later use;
(5) coating a hydrophobic film: and (4) coating a layer of hydrophobic organic porous film on the surface of the metal substrate for standby in the step (4) to obtain the oily sewage electric field demulsification electrode.
2. The method for preparing the electric field demulsification electrode for the oily wastewater as claimed in claim 1, wherein the metal substrate in the step (1) is iron or aluminum, and preferably, the thickness of the metal substrate is 1.0-2.0 mm.
3. The method for preparing the electric field demulsification electrode for the oily sewage as claimed in claim 1, wherein the acidic solution in the step (2) is prepared by dissolving sulfuric acid or hydrochloric acid in water, and preferably, the concentration of the acidic solution is 0.5-3% by mass.
4. The method for preparing the electric field demulsification electrode for the oily sewage as claimed in claim 1, wherein the temperature of the acidic solution in the step (2) is 20-40 ℃.
5. The method for preparing the demulsification electrode for the electric field of the oily sewage as claimed in claim 3, wherein the soaking time of the metal substrate subjected to the ultrasonic treatment in the step (2) in the acidic solution is 10-20 min.
6. The method for preparing the electric field demulsification electrode for the oily sewage according to any one of claims 1 to 5, wherein the mass percentage concentration of the sulfuric acid in the step (3) is 72 to 98 percent, and the time for soaking the metal substrate in the sulfuric acid is preferably 30 to 45 min.
7. The method for preparing the electric field demulsification electrode for the oily sewage according to any one of claims 1 to 5, wherein the deionized water is used for washing the sulfuric acid on the surface of the metal substrate in the step (4), the washing time is less than 2min, and preferably, the pH of the residual moisture on the surface of the metal substrate after washing is more than 6.0.
8. The method for preparing an oil-containing sewage electric field demulsification electrode as claimed in any one of claims 1 to 5, wherein the hydrophobic organic porous membrane in the step (5) is made of polytetrafluoroethylene, polypropylene or polyethylene.
9. The method for preparing the demulsifying electrode for the electric field of the oily sewage as claimed in claim 8, wherein the thickness of the hydrophobic organic porous film is 0.5-1.0 mm.
10. The method for preparing the demulsifying electrode for the electric field of the oily sewage as claimed in claim 8, wherein the surface of the hydrophobic organic porous membrane has a microporous structure, and the pore diameter is 0.1-0.5 μm.
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