CN110947206A - Nylon net-based multiphase oil-water continuous separation method - Google Patents
Nylon net-based multiphase oil-water continuous separation method Download PDFInfo
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- CN110947206A CN110947206A CN201911338397.4A CN201911338397A CN110947206A CN 110947206 A CN110947206 A CN 110947206A CN 201911338397 A CN201911338397 A CN 201911338397A CN 110947206 A CN110947206 A CN 110947206A
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- B01D17/02—Separation of non-miscible liquids
Abstract
The invention discloses a nylon net-based multiphase oil-water continuous separation method, which is characterized in that a nylon net prewetted by heavy oil is arranged on a suction filtration device, and the layer-by-layer separation of each phase is realized by utilizing negative pressure. The method is based on the environment-friendly material such as nylon net, can carry out orderly, gradual and controllable integrated separation on the multiphase oil and water by combining the guide of negative pressure, is simple, convenient and flexible, has wide applicability, and has high separation speed and separation efficiency.
Description
Technical Field
The invention belongs to the field of oil-water separation, and particularly relates to a nylon net-based multiphase oil-water continuous separation method.
Background
Since 1967, the crude oil leakage accident of super oil tanker 'tolicadansyl' is the past, the offshore oil leakage accident frequently happens, and organic compounds contained in the oil comprise benzene, toluene and other toxic substances which seriously damage the marine ecology. In addition, the industrial development and daily life of human beings bring a large amount of industrial oily wastewater and domestic sewage. These oily sewage seriously affect the human living environment, the life safety of various species and the health condition of the ecosystem. Therefore, under the condition of meeting the requirements of national economy and environmental development, in order to solve the problems, the research and the search of materials with oil-water separation function and economical efficiency are profound.
At present, crude oil on the sea surface has extremely high diffusivity, the crude oil must be treated as soon as possible after an accident to reduce the crude oil diffusion, and the petroleum and refined products thereof also have extremely high adhesion, pollute separation materials and equipment and cause the functional failure of the separation materials and the equipment. Researchers can perform oil-water separation by manufacturing interface materials with tunable wettability by imitating biological tissues, but the manufacturing involves 3D printing, photoetching and laser direct writing technologies, and the manufacturing process is complex and extremely high in cost.
Therefore, the detection of the oil-water separation method with high efficiency and low cost has important significance.
Disclosure of Invention
In order to avoid the defects of the prior art, the invention provides the nylon net-based multiphase oil-water continuous separation method, so that the high-efficiency classification and separation of the oily sewage can be realized on the basis of low-cost manufacture, large-area application and strong applicability.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
the invention relates to a nylon net-based multiphase oil-water continuous separation method, which is characterized by comprising the following steps of:
step 1, cleaning and assembling a high borosilicate solvent suction filtration device, wherein a filter cup, a hollow filter head and a liquid collection bottle are sequentially arranged from top to bottom, and a side pipe of the hollow filter head is connected with an air extraction valve through a rubber hose;
step 2, cleaning and drying the nylon net, then installing the nylon net between a filter cup and a hollow filter head of the suction filtration device, pre-wetting the nylon net by heavy oil to obtain an oil-water continuous separation device, and ensuring that the nylon net is sealed at the matching position of the filter cup and the hollow filter head;
step 3, adding the multiphase oil-water mixture to be separated into a filter cup, standing and layering, wherein the lower layer is heavy oil, the middle layer is water, and the upper layer is light oil;
step 4, opening the air extraction valve to enable two sides of the nylon net to be communicated to atmospheric pressure, enabling the lower-layer heavy oil to automatically pass through the nylon net and enter a liquid collecting bottle, and blocking water and light oil by the nylon net to collect the heavy oil;
step 5, after the heavy oil is collected, exhausting the device through an exhaust valve to enable the device space below the nylon net to generate negative pressure; stopping pumping air when the water layer starts to pass through the nylon net, and communicating two sides of the nylon net to atmospheric pressure;
after the water layer completely enters the liquid collecting bottle, the light oil is blocked by the nylon net, and water is collected;
step 6, after the water is collected, exhausting the device through the air exhaust valve again to enable the device space below the nylon net to generate negative pressure; stopping pumping air and communicating two sides of the nylon net to atmospheric pressure when the light oil layer starts to pass through the nylon net;
and after all the light oil enters the liquid collecting bottle, collecting the light oil to complete the continuous separation of the multiphase oil and water.
Further, the nylon net is made of polyamide 6, namely pure nylon fiber woven fabric, and is woven into a square-hole net structure by a twill weaving method.
Further, the aperture of the nylon net is 200-600 meshes (complying with a Taylor standard sieve).
Further, the high borosilicate solvent suction filtration device is cleaned by sequentially using acetone with the concentration of more than or equal to 95 percent and alcohol solution with the concentration of more than or equal to 99.7 percent; the nylon mesh was cleaned with distilled water and blown dry with high pressure nitrogen. And removing impurities such as surface stains, particles and the like by cleaning. The nylon mesh is sandwiched between the hollow filter head and the bowl by relatively tight clamps and ensures a seal there.
Further, the volume of the multiphase oil-water mixture added to the filter bowl should be such that the hydrostatic pressure provided by the level of the multiphase oil-water mixture in the filter bowl is less than the theoretical osmotic pressure of the selected nylon mesh after pre-wetting, otherwise the nylon mesh would not provide a barrier effect.
In the step 5 and the step 6, the air exhaust process can be stopped as long as the correspondingly blocked liquid starts to penetrate through the nylon net.
The above-described method of the present invention can be used for continuous separation of multiphase oil-water including various heavy oils (e.g., 1, 2-dichloroethane, dichloromethane, chloroform, etc.), water and light oils (e.g., n-hexane, n-octane, petroleum ether).
The principle of the invention is as follows: the method mainly utilizes the characteristics of super-hydrophilicity and super-oleophylicity of the nylon net, and has the wetting characteristics of super-oleophobicity in water and super-hydrophobicity in oil according to the similarity and intermiscibility principle. The nylon mesh pre-wetted by the water cannot be wetted again by the oil, and the oil is a non-wetting phase at the moment; on the contrary, nylon mesh pre-wetted with oil cannot be re-wetted with water, which is now the non-wetting phase. The sum of the static pressure and the negative pressure of the non-wetting phase liquid on the nylon net is larger than the theoretical osmotic pressure of the pre-wetting nylon net on the non-wetting phase at the moment by introducing the negative pressure, so that the nylon net is penetrated, and the controllable multi-layer oil-water continuous separation effect is achieved. In the invention, when the nylon net is pre-wetted by water, the nylon fibers are wrapped by a layer of water film, so that the aperture between the fibers of the nylon net is smaller, the Laplace pressure of the oil solution above the aperture is larger, namely the theoretical osmotic pressure is larger, and the liquid static pressure of the oil solvent is smaller than the theoretical osmotic pressure of the nylon net, so that the nylon net has the function of isolating the organic oil solvent. When the isolated liquid is guided by using negative pressure, the sum of the static pressure and the negative pressure of the liquid is greater than the theoretical osmotic pressure of the nylon net, the oil solvent permeates the nylon net, the wetting phase is changed into oil, the non-wetting phase is changed into water, and the nylon fiber is wrapped by a layer of oil film and has super-hydrophobic property. The wetting phase of the nylon net can be repeatedly replaced by negative pressure through the repeated operation, thereby generating repeated change of the non-wetting phase. When the introduced negative pressure P meets the formula (1), the upper layer liquid starts to permeate the nylon net:
P+Phigh≥Pintru(1)
p in the formula (1)highThe pressure, P, generated by the height of the oil solvent liquid to the nylon netintruThe theoretical osmotic pressure for a prewetted nylon mesh when subjected to such an oil solution can be obtained from equation (2) or equation (3):
γ in the formulae (2) and (3)owAnd gammawoAre the interfacial tension, theta, of both the oil solution and watero/wAnd thetaw/oThe contact angle of oil drops on the nylon net pre-wetted by water and the contact angle of water drops on the nylon net pre-wetted by oil are respectively, and d is the aperture of the nylon net.
The invention has the beneficial effects that:
1. the method is based on the environment-friendly material such as nylon net, can carry out orderly, gradual and controllable integrated separation on the multiphase oil and water by combining the guide of negative pressure, is simple, convenient and flexible, has wide applicability, and has high separation speed and separation efficiency.
2. The device related by the method of the invention has low manufacturing cost and can be applied in a large area.
Drawings
FIG. 1 is a real-shot diagram of each component of the high borosilicate solvent filtration device used in the present invention, which comprises a triangular liquid collecting bottle, a hollow filter head and a filter cup (300mL) from left to right.
FIG. 2 is a real shot of the invention after assembling the high borosilicate solvent filtration device with a nylon mesh.
FIG. 3 is a scanning electron micrograph of a 400 mesh nylon mesh used in the present invention, wherein: the magnifications of the graphs (a), (b) and (d) are 60x, 200x and 1000x, respectively, and the scales are 200 μm, 100 μm and 10 μm, respectively; FIG. (c) is a cross-sectional view taken at 89 ℃ at a magnification of 100X on a scale of 100. mu.m.
FIG. 4 is a schematic diagram of the contact angles of different liquids on a prewetted nylon mesh, and the droplets were all captured at 5 μ L, wherein the graphs (a) to (d) are respectively: a schematic view of a contact angle of water on a nylon net prewetted with light oil n-octane, a schematic view of a contact angle of water on a nylon net prewetted with heavy oil 1, 2-dichloroethane, a schematic view of a contact angle of light oil n-octane on a nylon net prewetted with water, and a schematic view of a contact angle of heavy oil 1, 2-dichloroethane on a nylon net prewetted with water.
FIG. 5 is a flow chart of the continuous separation of multiphase oil and water in the embodiment of the present invention, wherein A, B and C respectively indicate that the liquids are heavy oil, water and light oil.
FIG. 6 is a flow chart of the separation of multiphase oil-water mixtures according to the present invention, wherein M1-M5 are the following 5 multiphase oil-water mixtures: 1, 2-dichloroethane/water/n-hexane (M1); 1, 2-dichloroethane/water/n-octane (M2); chloroform/water/n-octane (M3); dichloromethane/water/n-octane (M4); dichloromethane/water/petroleum ether (M5).
FIG. 7 is a graph showing the separation efficiency of different multiphase oil-water mixtures according to the present invention, wherein M1-M5 are the following 5 multiphase oil-water mixtures: 1, 2-dichloroethane/water/n-hexane (M1); 1, 2-dichloroethane/water/n-octane (M2); chloroform/water/n-octane (M3); dichloromethane/water/n-octane (M4); dichloromethane/water/petroleum ether (M5).
Detailed Description
The following examples are given for the detailed implementation and specific operation of the present invention, but the scope of the present invention is not limited to the following examples.
The larger the mesh number, the larger the theoretical osmotic pressure of the nylon net, and can bear more oily sewage liquid. In the following examples, a 400 mesh nylon mesh was used, and scanning electron micrographs at different magnifications are shown in FIG. 3.
The nylon net has the characteristics of super-hydrophilicity and super-oleophylicity, and has the wetting characteristics of super-oleophobicity in water and super-hydrophobicity in oil according to the similarity and intermiscibility principle. FIG. 4 is a schematic representation of the contact angles of different liquids on a prewetted nylon mesh, wherein the graphs (a) - (d) are respectively: a schematic view of a contact angle of water on a nylon net prewetted with light oil n-octane, a schematic view of a contact angle of water on a nylon net prewetted with heavy oil 1, 2-dichloroethane, a schematic view of a contact angle of light oil n-octane on a nylon net prewetted with water, and a schematic view of a contact angle of heavy oil 1, 2-dichloroethane on a nylon net prewetted with water.
Example 1
The multiphase oil-water continuous separation method based on the nylon net comprises the following steps:
step 1, as shown in fig. 1 and fig. 2, cleaning a high borosilicate solvent filtration device by using acetone with the concentration of greater than or equal to 95% and alcohol solution with the concentration of greater than or equal to 99.7% in sequence, then assembling the high borosilicate solvent filtration device into a filter cup (300mL), a hollow filter head and a triangular liquid collecting bottle (500mL) from top to bottom in sequence, and connecting a side pipe of the hollow filter head with an air suction valve through a rubber hose.
And 2, cleaning the nylon net by using distilled water, drying the nylon net by using high-pressure nitrogen, cutting the nylon net to a proper size, installing the nylon net between a filter cup and a hollow filter head of a suction filtration device (fixing and sealing the nylon net by using a stainless steel iron clamp), pre-wetting the nylon net by using heavy oil 1, 2-dichloroethane to obtain an oil-water continuous separation device, and ensuring the sealing of the matching positions of the nylon net, the filter cup and the hollow filter head. The theoretical osmotic pressure of a 1, 2-dichloroethane-wetted 400 mesh nylon mesh for water according to equation (3) is 1930.4 Pa.
Step 3, preparing a multiphase oil-water mixture to be separated: 1, 2-dichloroethane is dyed orange by Sudan III, water is dyed blue by blue ink, and n-octane is dyed yellow by Sudan II for convenient observation; 50mL of 1, 2-dichloroethane, 50mL of water, and 50mL of n-octane were mixed to form a multiphase oil-water mixture.
As shown in FIG. 5a, the multiphase oil-water mixture to be separated is added into a filter cup, and is kept stand for layering, wherein the lower layer is heavy oil (A), the middle layer is water (B), and the upper layer is light oil (C).
And 4, opening the air extraction valve to enable two sides of the nylon net to be communicated to atmospheric pressure, and enabling the lower-layer heavy oil to automatically pass through the nylon net and enter the liquid collecting bottle (as shown in fig. 5 b). After waiting for a moment, the heavy oil flows out, the water and the light oil are blocked by the nylon net, the blocking time is more than 10min (as shown in figure 5 c), and the heavy oil (A) is collected;
step 5, after the heavy oil is collected, exhausting the device through an exhaust valve to enable the device space below the nylon net to generate negative pressure; when the provided negative pressure and the static pressure of the liquid level height at the moment exceed the theoretical osmotic pressure of the nylon net wetted by the 1, 2-dichloroethane, namely the water layer just starts to pass through the nylon net, stopping air suction and communicating the two sides of the nylon net to the atmospheric pressure, as shown in fig. 5 (d);
after waiting for a moment, the water layer is drained, and after all the water layer enters the liquid collecting bottle, the light oil is blocked by the nylon net for more than 10min, and as shown in fig. 5(e), water (B) is collected;
step 6, after the water is collected, exhausting the device through the air exhaust valve again to enable the device space below the nylon net to generate negative pressure; when the provided negative pressure and the static pressure of the liquid level height exceed the theoretical osmotic pressure of the nylon net wetted by water, namely the light oil layer starts to pass through the nylon net, stopping air suction and communicating the two sides of the nylon net to atmospheric pressure;
after waiting for a while, all the light oil enters the liquid collecting bottle, as shown in fig. 5(f), the light oil (C) is collected, as shown in fig. 5(g), and the continuous separation of the multiphase oil and water is completed.
In order to verify the separation effect of the method on different multiphase oil-water mixtures, a plurality of multiphase oil-water mixtures are prepared and separated according to the same method, and the flow rate and the separation efficiency are tested as follows: 1, 2-dichloroethane/water/n-hexane (M1); 1, 2-dichloroethane/water/n-octane (M2); chloroform/water/n-octane (M3); dichloromethane/water/n-octane (M4); dichloromethane/water/petroleum ether (M5).
The flow velocity v is calculated using equation (4) and the result is shown in FIG. 6:
in formula (4): v is the volume of liquid passing through the nylon mesh, S is the area used for the nylon mesh filtration function, and t is the time for the liquid to pass through the nylon mesh.
The separation efficiency R was calculated using equation (5), and the results are shown in fig. 7:
R(％)＝(1-C1)×100％ (5)
in formula (5): c1The content of oil in the separated water, namely the separation efficiency of the water; the separation efficiency of the oil can be obtained in the same way.
The detection proves that the method has higher flow rate and separation efficiency for different multiphase oil-water mixtures. Therefore, the method can realize the gradual, orderly and controllable separation of the mixed liquid of the heavy oil, the water and the light oil, and simultaneously ensure higher flow velocity and reliability.
The above description is only exemplary of the present invention and should not be taken as limiting the invention, and any modifications, equivalents, improvements, etc. made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (5)
1. A nylon net based multiphase oil-water continuous separation method is characterized by comprising the following steps:
step 1, cleaning and assembling a high borosilicate solvent suction filtration device, wherein a filter cup, a hollow filter head and a liquid collection bottle are sequentially arranged from top to bottom, and a side pipe of the hollow filter head is connected with an air extraction valve through a rubber hose;
step 2, cleaning and drying the nylon net, then installing the nylon net between a filter cup and a hollow filter head of the suction filtration device, pre-wetting the nylon net by heavy oil to obtain an oil-water continuous separation device, and ensuring that the nylon net is sealed at the matching position of the filter cup and the hollow filter head;
step 3, adding the multiphase oil-water mixture to be separated into a filter cup, standing and layering, wherein the lower layer is heavy oil, the middle layer is water, and the upper layer is light oil;
step 4, opening the air extraction valve to enable two sides of the nylon net to be communicated to atmospheric pressure, enabling the lower-layer heavy oil to automatically pass through the nylon net and enter a liquid collecting bottle, and blocking water and light oil by the nylon net to collect the heavy oil;
step 5, after the heavy oil is collected, exhausting the device through an exhaust valve to enable the device space below the nylon net to generate negative pressure; stopping pumping air and communicating the two sides of the nylon net to atmospheric pressure when the water layer starts to pass through the nylon net;
after the water layer completely enters the liquid collecting bottle, the light oil is blocked by the nylon net, and water is collected;
step 6, after the water is collected, exhausting the device through the air exhaust valve again to enable the device space below the nylon net to generate negative pressure; stopping pumping air and communicating two sides of the nylon net to atmospheric pressure when the light oil layer starts to pass through the nylon net;
and after all the light oil enters the liquid collecting bottle, collecting the light oil to complete the continuous separation of the multiphase oil and water.
2. The method of claim 1, wherein: the nylon net is composed of polyamide 6 and is woven into a square-hole net structure by a twill weaving method.
3. The method according to claim 1 or 2, characterized in that: the aperture of the nylon net is 200-600 meshes.
4. The method according to claim 1 or 2, characterized in that: the high borosilicate solvent suction filtration device is cleaned by sequentially using acetone with the concentration of more than or equal to 95 percent and alcohol solution with the concentration of more than or equal to 99.7 percent; the nylon mesh was cleaned with distilled water and blown dry with high pressure nitrogen.
5. The method of claim 1, wherein: the volume of the multiphase oil-water mixture added into the filter cup is ensured to ensure that the hydrostatic pressure provided by the liquid level height in the filter cup is less than the theoretical osmotic pressure of the selected nylon net after pre-wetting.
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| CN112156563A (en) * | 2020-09-28 | 2021-01-01 | 湖北大学 | Preparation method of nylon net with wettability gradient for water mist collection |
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