Microchannel separation method and microchannel separation device for oil-water two-phase

Abstract

The application discloses a kind of oil-water two-phase microchannel separation method and microchannel separation device.The microchannel separator device of the application includes upper cover plate, lower cover plate and micro-separator-1, micro-separator-2 sealed and installed between upper cover plate, lower cover plate in sequence.The method of the application uses a kind of microchannel separation device, using the surface properties and size confinement effect of microchannel, oil-water two-phase can be separated quickly and efficiently in microchannel, the separation process is continuous and controllable, improves the separation efficiency of oil-water system, realizes 100% separation selectivity under high feed rate, can realize the intensification and equipment miniaturization of oil-water two-phase separation process in chemical separation technology field.

Description

TECHNICAL FIELD

[0001] The present application belongs to the field of chemical separation technology, and particularly relates to a micro-channel separation method and a micro-channel separation device for oil-water two-phase. BACKGROUND

[0002] Among water pollution, oil (grease, petroleum, lipophilic organic solvents, etc.) has become one of the important pollutants, and oily wastewater has caused great threat to the ecological environment and human health. Oily wastewater exists widely, involving many fields such as life catering, agricultural production, transportation, chemical industry, manufacturing industry, petroleum industry, etc. With the continuous acceleration of urbanization and industrialization process, the problem of oil pollutants in water is increasingly prominent, and more and more attention and concern are paid. Traditional oil-water separation methods such as gravity separation method, centrifugal separation method, ultrasonic separation method, adsorption separation method and membrane separation method have the disadvantages of low efficiency or secondary pollution to the environment. The treatment of oily wastewater often requires high cost and energy consumption, which also causes great economic burden and resource waste. Therefore, it is of great significance to study the oil-water separation technology with high efficiency and low cost. SUMMARY

[0003] In view of the above problems, the present application provides a micro-channel separation method and a micro-channel separation device for oil-water two-phase. To achieve the above-mentioned purpose, the technical scheme adopted by the present application is as follows:

[0004] A micro-channel separation device for strengthening oil-water separation, the micro-separation device comprises an upper cover plate, a lower cover plate and a micro-separator-1 and a micro-separator-2 which are sealed and installed in sequence between the upper cover plate and the lower cover plate. The upper cover plate is provided with an inlet hole of oil-water raw material mixed liquid and an outlet hole of water phase (oil phase) after oil-water two-phase separation, and the lower cover plate is provided with an outlet hole of oil phase (water phase) after oil-water two-phase separation, which are both through holes; the micro-separator-1 and the micro-separator-2 are sealed and installed in sequence between the upper cover plate and the lower cover plate, and the two ends of the micro-separator-1 are respectively connected with the inlet hole of oil-water raw material mixed liquid and the outlet hole of water phase (oil phase) after oil-water two-phase separation provided on the upper cover plate; the two ends of the micro-separator-2 are respectively connected with the inlet hole of oil-water raw material mixed liquid on the separator-1 and the outlet hole of oil phase (water phase) after oil-water two-phase separation on the lower cover plate.

[0005] The high-efficiency micro-channel separation device for strengthening oil-water two-phase separation provided by the application comprises a micro-separator-1 and a micro-separator-2, wherein the micro-separator-1 is composed of one micro-separation plate or two or more micro-separation plates stacked together, the micro-separation plate is provided with an inlet hole of the oil-water raw material mixture corresponding to the upper cover plate, an outlet hole of the water phase (or the oil phase) after oil-water two-phase separation corresponding to the upper cover plate, the inlet hole and the outlet hole are through holes, and the micro-separation plate is provided with a micro-separation channel, the two ends of the micro-separation channel are connected with the inlet hole of the oil-water raw material mixture and the outlet hole of the water phase (or the oil phase) after oil-water two-phase separation, respectively.

[0006] The high-efficiency micro-channel separation device for strengthening oil-water two-phase separation provided by the application comprises a micro-separator-1 and a micro-separator-2, wherein the micro-separator-2 is composed of one micro-separation plate or two or more micro-separation plates stacked together, the micro-separation plate is provided with an inlet hole of the oil-water raw material mixture corresponding to the micro-separator-1, an outlet hole of the oil phase (or the water phase) after oil-water two-phase separation corresponding to the lower cover plate, the inlet hole is a non-through hole, the outlet hole is a through hole, and the micro-separation plate is provided with a micro-separation channel, the end of the micro-separation channel is connected with the outlet hole of the oil phase (or the water phase) after oil-water two-phase separation.

[0007] The high-efficiency micro-channel separation device for strengthening oil-water two-phase separation provided by the application comprises a micro-separator-1 and a micro-separator-2, wherein the micro-separation plate of the micro-separator-1 is provided with an oil-water raw material mixture separation cavity composed of micro-channels, the surface of the micro-channel has hydrophilic (or hydrophobic) property, and the starting end of the separation cavity is connected with the inlet hole of the oil-water raw material mixture of the micro-separator-1 and the outlet hole of the water phase (or the oil phase) after oil-water two-phase separation, respectively.

[0008] The high-efficiency micro-channel separation device for strengthening oil-water two-phase separation provided by the application comprises a micro-separator-1 and a micro-separator-2, wherein the micro-separation plate of the micro-separator-2 is provided with an oil-water raw material mixture separation cavity composed of micro-channels, the surface of the micro-channel has hydrophobic (or hydrophilic) property, the starting end of the separation cavity is connected with the inlet hole of the oil-water raw material mixture of the micro-separator-2, and the terminal end of the separation cavity is connected with the outlet hole of the oil phase (or the water phase) after oil-water two-phase separation of the micro-separator-2.

[0009] The high-efficiency micro-channel separation device for strengthening oil-water two-phase separation provided by the application comprises a micro-separator-1 and a micro-separator-2, wherein the material of the upper cover plate, the lower cover plate and the micro-separator-1 and the micro-separator-2 sealed and installed between the upper cover plate and the lower cover plate in sequence is any one of stainless steel, copper and titanium, and the sealing connection between the adjacent two modules adopts a vacuum diffusion welding mode; the sealing connection between the adjacent two modules specifically means that the remaining part of the module except the area occupied by the micro-channel and the through hole is welded and sealed.

[0010] The high-efficiency micro-channel separation device for strengthening oil-water two-phase separation provided by the application comprises a micro-separator-1 and a micro-separator-2, wherein the micro-channel is a snake-shaped channel or a spiral channel, the equivalent diameter is 50-3000 μm, the cross-sectional shape is circular or rectangular or square, and the equivalent diameter of the inlet through hole and the outlet through hole is 2-6 mm.

[0011] The present application provides a micro-channel separation method for oil-water two-phase, which uses the micro-channel separation device described above, and the oil-water raw material mixture enters the micro-separator-1 and the micro-separator-2 through the through holes on the upper cover plate, the micro-separator-1 and the micro-separator-2 in sequence, and the separation of the oil-water two-phase is carried out in the micro-separator-1 and the micro-separator-2. The oil phase (water phase) in the separation product flows out of the micro-separation device through the through holes on the micro-separator-1 and the upper cover plate, and the water phase (oil phase) flows out of the micro-separation device through the through holes on the micro-separator-2 and the lower cover plate.

[0012] In the micro-channel separation method for oil-water two-phase provided by the present application, the oil-water mixture is in the state of emulsion or oil-water stratification, and contains oil phase and water phase. The oil phase is at least one of kerosene, diesel, gasoline, dodecane, tetradecane, hexadecane, octadecane and the like long-chain alkanes, benzene, toluene, xylene, mixed benzene, carbon tetrachloride, dichloromethane, trichloromethane and the like. The water phase is at least one of water or aqueous solution of polyvinyl alcohol, gelatin, polyethylene glycol, hydrochloric acid, nitric acid, sodium hydroxide and the like. The feed amount of the oil-water mixture is 0-200 ml / min, and the separation selectivity is 100%. The oil-water two-phase involved in the present application can be applied to all kinds of oil-water systems known.

[0013] The present application adopts a micro-channel separation device, and in the continuous separation process, the oil-water two-phase can be quickly and efficiently separated in the micro-channel, and 100% separation selectivity can be achieved under high feed amount. The micro-separation device utilizes the surface properties and size confinement effect of the micro-channel, so that the separation process is more controllable, the separation efficiency of the oil-water system is effectively improved, and the energy consumption is reduced. Finally, the oil-water two-phase separation process in the field of chemical separation technology is strengthened and the equipment is miniaturized, and the separation efficiency of the system is greatly improved. BRIEF DESCRIPTION OF DRAWINGS

[0014] Figure 1 It is a schematic diagram of the upper cover plate structure of the high-efficiency micro-channel separation device for strengthening the separation of oil-water two-phase. In the figure, 1-1 is the inlet through hole of the raw material mixture, and 1-2 is the outlet through hole of the water phase (or oil phase) after separation by the micro-separator-1.

[0015] Figure 2 It is a schematic diagram of the micro-separator-1 structure of the high-efficiency micro-channel separation device for strengthening the separation of oil-water two-phase. In the figure, 2-1 is the inlet through hole of the raw material mixture, 2-2 is the outlet through hole of the water phase (or oil phase) after separation by the micro-separator-1, and 2-3 is the micro-separation plate of the micro-separator-1.

[0016] Figure 3Figure 1 is a schematic diagram of the micro-separator-2 structure of the high-efficiency micro-channel separation device for enhancing oil-water two-phase separation; in the figure, 3-1 is the raw material mixed liquid inlet hole; 3-2 is the oil phase (or water phase) outlet through hole after micro-separator-2 separation; and 3-3 is the micro-separation plate of the micro-separator-2.

[0017] Figure 4 Figure 2 is a schematic diagram of the lower cover plate structure of the high-efficiency micro-channel separation device for enhancing oil-water two-phase separation; in the figure, 4-1 is the oil phase (or water phase) outlet through hole after micro-separator-2 separation.

[0018] Figure 5 Figure 3 is a schematic diagram of the micro-separation device structure for enhancing oil-water separation. DETAILED DESCRIPTION

[0019] The preferred embodiments of the present application will be described in detail below with reference to the accompanying drawings. It should be understood that the preferred embodiments are only for the purpose of illustrating the present application, and are not intended to limit the protection scope of the present application. The present application relates to the inventive design of a micro-channel separation device for enhancing oil-water separation, which is essentially to realize the process intensification and equipment miniaturization of the oil-water two-phase separation in the field of chemical separation technology by using the surface properties and size confinement effect of the micro-channel, and to improve the separation efficiency of the system.

[0020] 1. Figure 5 Figure 1 is a schematic diagram of the micro-separation device structure for enhancing oil-water separation, which is composed of an upper cover plate (1), a lower cover plate (2), and a micro-separator-1 (3) and a micro-separator-2 (4) which are sequentially and sealingly installed between the upper cover plate and the lower cover plate. Figure 1 Figure 4 Figure 2 Figure 3

[0021] 2. In the micro-separation device for enhancing oil-water separation provided by the present application, the upper cover plate is provided with a raw material mixed liquid inlet through hole (1-1) and a water phase (or oil phase) outlet through hole (1-2) after micro-separator-1 separation. Figure 1 Figure 1

[0022] 3. In the micro-separation device for enhancing oil-water separation provided by the present application, the micro-separator-1 is composed of one or more than two pieces of micro-separation plates stacked together, and the micro-separator-1 plate is provided with a raw material mixed liquid inlet through hole (2-1) corresponding to the upper cover plate and a water phase (or oil phase) outlet through hole (2-2) corresponding to the upper cover plate after micro-separator-1 separation. Figure 2 Figure 2

[0023] ​​​​​​​​4. In the micro-separation device for enhancing oil-water separation provided by the present invention, the microreactor-2 is composed of one or more stacked micro-separation plates, and the micro-separator-2 plate is provided with an inlet hole for the raw material mixture corresponding to that on the micro-separator-1 plate. Figure 3 ,3-1), the micro separator-2 plate is provided with an outlet through hole for the oil phase (or water phase) after separation by the micro separator-2 ( Figure 3 ,3-2).

[0024] 5. In the micro-separation device for enhancing oil-water separation provided by the present invention, the lower cover plate is provided with an outlet through hole for the oil phase (or water phase) separated by micro-separator-1 and micro-separator-2, corresponding to micro-separator-2. Figure 4 ,4-1).

[0025] 6. In the micro-separation device for enhancing oil-water separation provided by the present invention, the micro-separator-1 ( Figure 2 The micro-separation plate is equipped with a separation chamber composed of parallel microchannels. Figure 2 , 2-3), the separation chamber is equipped with a raw material mixture inlet hole for micro separator-1 ( Figure 2 ,2-1) and the separation product outlet orifice of micro separator-1 ( Figure 2 ,2-2).

[0026] 7. In the micro-separation device for enhancing oil-water separation provided by the present invention, the micro-separator-2 ( Figure 3 The micro-separation plate is equipped with a separation chamber composed of parallel microchannels. Figure 3 ,3-3), the separation chamber is equipped with a raw material mixture inlet hole for micro separator-2 ( Figure 3 ,3-1) and the separation product outlet orifice of micro separator-2 ( Figure 3 ,3-2).

[0027] 8. In the micro-separation device for enhancing oil-water separation provided by the present invention, the upper cover plate ( Figure 1 Micro-splitter-1 Figure 2 Micro-splitter-2 Figure 3 ) and lower cover plate ( Figure 4 The materials are the same, and can be any of the metal materials such as stainless steel, copper, and titanium, with stainless steel being preferred. The sealing connection between the two adjacent modules adopts vacuum diffusion welding. Specifically, the sealing connection between the two adjacent modules means that the remaining parts of the module, except for the area occupied by the microchannels and through holes, are welded and sealed.

[0028] 9. In the micro-separation device for enhancing oil-water separation provided by the present invention, the microchannel is a serpentine channel or a spiral channel, preferably a serpentine channel; the equivalent diameter is 50-3000 μm, preferably 500-1000 μm; the cross-sectional shape is circular, rectangular or square, preferably rectangular; the shape of the inlet distribution cavity and the outlet collection cavity is triangular; the equivalent diameter of the inlet through hole and the outlet through hole is 2-6 mm, preferably 3-5 mm.

[0029] 10. Figure 5 This is a common overall and internal structure pattern for sealing and carrying the raw material mixture in the micro-separation device of the present invention. However, in specific implementations, it is not limited to this pattern and can be used in various ways. Figure 5 Further optimizations and improvements are made based on the basic structure.

[0030] 11. Figure 2 This is a common pattern for the overall and internal structure of the micro-separator-1 used to separate oil and water phases in this invention. However, in specific implementations, it is not limited to this pattern and can be adapted to other configurations. Figure 2 Further optimizations and improvements will be made based on the basic structure.

[0031] 12. Figure 3 This is a common pattern for the overall and internal structure of the micro-separator-2 used to separate oil and water phases in this invention. However, in specific implementations, it is not limited to this pattern and can be adapted to other configurations. Figure 3 Further optimizations and improvements will be made based on the basic structure.

[0032] Example 1:

[0033] Micro-separator-1 has a hydrophobic microchannel with a serpentine channel, an equivalent diameter of 500 μm, and a square cross-sectional shape. Micro-separator-2 has a hydrophilic microchannel with a serpentine channel, an equivalent diameter of 500 μm, and a square cross-sectional shape. Both micro-separator-1 and micro-separator-2 are made of stainless steel, with an equivalent diameter of 4 mm for the inlet and outlet through-holes. The separation system is a hexane / water mixture in an oil-water stratified state.

[0034] The hexane / water mixture is passed through the through-hole on the top cover plate ( Figure 1 ,1-1), through holes on micro separator-1 ( Figure 2 , 2-1), the feed rate is 100 ml / min, and it enters micro separator-1 and micro separator-2. Oil and water phases are separated in micro separator-1 and micro separator-2. The separated n-hexane passes sequentially through the through-hole on micro separator-1 ( Figure 2 2-2), through holes on the top cover plate ( Figure 1 (1-2) flows out, and the separated water flows through the through holes on the micro separator-2 in sequence (Figure 3 , 3-1), the through hole (4-1) on the lower cover plate. Figure 4 , 4-1) flows out.

[0035] After separation by the micro-separator, the separation selectivity is 100%.

[0036] Example 2:

[0037] The micro-channel of the micro-separator-1 has a hydrophilic surface, and is a spiral channel with an equivalent diameter of 500 μm and a square cross-sectional shape; the micro-channel of the micro-separator-2 has a hydrophobic surface, and is a spiral channel with an equivalent diameter of 500 μm and a square cross-sectional shape; the micro-separator-1 and the micro-separator-2 are both made of stainless steel, the equivalent diameter of the inlet through hole and the outlet through hole is 4 mm, and the separation system is a toluene / polyvinyl alcohol mixed solution in an emulsion state.

[0038] The toluene / 1 wt% polyvinyl alcohol aqueous solution mixed solution passes through the through hole (1-1) on the upper cover plate, Figure 1 , 2-1) on the micro-separator-1, Figure 2 , 2-1), and the feed amount is 100 ml / min, enters the micro-separator-1 and the micro-separator-2, and the oil-water two-phase separation is carried out in the micro-separator-1 and the micro-separator-2; the separated polyvinyl alcohol passes through the through hole (2-2) on the micro-separator-1, Figure 2 , 2-1) on the micro-separator-1, Figure 1 , 2-1), and the feed amount is 100 ml / min, enters the micro-separator-1 and the micro-separator-2, and the oil-water two-phase separation is carried out in the micro-separator-1 and the micro-separator-2; the separated polyvinyl alcohol passes through the through hole (2-2) on the micro-separator-1, Figure 3 , 2-1) on the micro-separator-1, Figure 4 , 4-1) flows out.

[0039] After separation by the micro-separator, the separation selectivity is 100%.

[0040] Example 3:

[0041] The micro-channel of the micro-separator-1 has a hydrophilic surface, and is a spiral channel with an equivalent diameter of 500 μm and a square cross-sectional shape; the micro-channel of the micro-separator-2 has a hydrophobic surface, and is a spiral channel with an equivalent diameter of 500 μm and a square cross-sectional shape; the micro-separator-1 and the micro-separator-2 are both made of stainless steel, the equivalent diameter of the inlet through hole and the outlet through hole is 4 mm, and the separation system is a toluene / polyvinyl alcohol mixed solution in an emulsion state.

[0042] The toluene / 1 wt% polyvinyl alcohol aqueous solution mixed solution passes through the through hole (1-1) on the upper cover plate, Figure 1 , 2-1) on the micro-separator-1, Figure 2, 2-1), the feed rate is 150 ml / min, entering micro separator-1 and micro separator-2, where oil and water phases are separated. The separated nitric acid aqueous solution passes sequentially through the through holes on micro separator-1 ( Figure 2 2-2), through holes on the top cover plate ( Figure 1 (1-2) flows out, and the separated chloroform flows through the through-holes on the micro-separator-2 in sequence ( Figure 3 3-1) Through holes on the lower cover plate ( Figure 4 ,4-1) outflow.

[0043] After separation by the micro separator, the separation selectivity is 100%.

[0044] Any aspects not covered in this invention are applicable to existing technologies.

Claims

1. A microchannel separation device for enhanced separation of oil and water phases, characterized by, The device comprises an upper cover plate, a lower cover plate, and micro-separators-1 and -2 sealed and installed in sequence between the upper cover plate and the lower cover plate; the upper cover plate is provided with an inlet hole for oil-water raw material mixture and an outlet hole for oil-water two-phase separation, and the lower cover plate is provided with an outlet hole for oil-water two-phase separation, both being through holes; the micro-separators-1 and -2 are sealed and installed in sequence between the upper cover plate and the lower cover plate, and both ends of the micro-separator-1 are respectively provided with through holes connected with the inlet hole for oil-water raw material mixture and the outlet hole for oil-water two-phase separation on the upper cover plate; both ends of the micro-separator-2 are respectively provided with through holes connected with the inlet hole for oil-water raw material mixture on the micro-separator-1 and the outlet hole for oil-water two-phase separation on the lower cover plate. The micro-separator-1 is composed of one micro-separation plate or two or more micro-separation plates stacked together, and the micro-separation plate of the micro-separator-1 is provided with the inlet hole for oil-water raw material mixture on the upper cover plate and the outlet hole for oil-water two-phase separation on the upper cover plate, both being through holes; the micro-separation plate of the micro-separator-1 is provided with a micro-channel, and both ends of the micro-channel of the micro-separator-1 are respectively connected with the inlet hole for oil-water raw material mixture and the outlet hole for oil-water two-phase separation. The micro-separator-2 is composed of one micro-separation plate or two or more micro-separation plates stacked together, and the micro-separation plate of the micro-separator-2 is provided with the inlet hole for oil-water raw material mixture on the micro-separator-1 and the outlet hole for oil-water two-phase separation on the lower cover plate, the outlet hole being a through hole; the micro-separation plate of the micro-separator-2 is provided with a micro-channel, and one end of the micro-channel of the micro-separator-2 is connected with the outlet hole for oil-water two-phase separation. The micro-channel of the micro-separator-1 is provided with hydrophilicity, the micro-channel of the micro-separator-2 is provided with hydrophobicity, the outlet hole for oil-water two-phase separation on the upper cover plate is a water phase outlet hole, and the outlet hole for oil-water two-phase separation on the lower cover plate is an oil phase outlet hole, or the micro-channel of the micro-separator-1 is provided with hydrophobicity, the micro-channel of the micro-separator-2 is provided with hydrophilicity, the outlet hole for oil-water two-phase separation on the upper cover plate is an oil phase outlet hole, and the outlet hole for oil-water two-phase separation on the lower cover plate is a water phase outlet hole.

2. The microchannel separation device for enhanced separation of oil and water according to claim 1, wherein, The micro-separation plate of the micro-separator-1 is provided with an oil-water raw material mixture separation cavity composed of a micro-channel, and the starting end of the separation cavity is connected with the inlet hole for oil-water raw material mixture and the outlet hole for oil-water two-phase separation of the micro-separator-1.

3. The microchannel separation device for enhanced separation of oil and water according to claim 1, wherein, The micro-separation plate of the micro-separator-2 is provided with an oil-water raw material mixture separation cavity composed of a micro-channel, the starting end of the separation cavity is connected with the inlet hole for oil-water raw material mixture of the micro-separator-2, and the terminal end of the separation cavity is connected with the outlet hole for oil-water two-phase separation of the micro-separator-2.

4. The microchannel separation device for enhanced separation of oil and water according to claim 1, wherein, The upper cover plate, the lower cover plate, and the micro-separators-1 and -2 sealed and installed in sequence between the upper cover plate and the lower cover plate are made of any one of stainless steel, copper, and titanium, and the sealing connection between adjacent two modules is achieved by vacuum diffusion welding.

5. The microchannel separation device for enhanced separation of oil and water phases according to any one of claims 2-4, wherein, The microchannel is a serpentine channel or a spiral channel, has an equivalent diameter of 50-3000 μm, a cross-sectional shape of one of a circle, a rectangle, and a square, and equivalent diameters of the inlet and outlet through holes of 2-6 mm.

6. A microchannel separation method of oil-water two-phase, characterized by The oil-water two-phase separation is performed using the device of claim 5, including the following steps: the oil-water raw material mixture is sequentially passed through the through holes on the upper cover plate, the micro-separator-1, and the micro-separator-2, and enters the micro-separator-1 and the micro-separator-2, and the oil-water two-phase separation is performed in the micro-separator-1 and the micro-separator-2, the oil phase in the separation product flows out of the micro-separation device through the through holes on the micro-separator-1 and the upper cover plate, and the water phase flows out of the micro-separation device through the through holes on the micro-separator-2 and the lower cover plate. Alternatively, the water phase in the separation product flows out of the micro-separation device through the through holes on the micro-separator-1 and the upper cover plate, and the oil phase flows out of the micro-separation device through the through holes on the micro-separator-2 and the lower cover plate.

7. The oil-water two-phase microchannel separation method according to claim 6, wherein, The oil-water mixture is an emulsion or an oil-water layered state, the feeding amount is 0-200 ml / min, the oil phase is one of kerosene, diesel, gasoline, dodecane, tetradecane, hexadecane, octadecane, or benzene, toluene, xylene, mixed benzene, carbon tetrachloride, dichloromethane, and trichloromethane, and the water phase is one of water or a PVA aqueous solution, a gelatin aqueous solution, a polyethylene glycol aqueous solution, a hydrochloric acid aqueous solution, a nitric acid aqueous solution, and a sodium hydroxide aqueous solution.

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