An automatic oil-water separation device

Abstract

Embodiments of the present application provide an oil-water automatic separation device, which comprises a vertical separation tank, the side of the separation tank is provided with an oil phase outlet and a mixed liquid inlet below the oil phase outlet, and the bottom of the separation tank is provided with a water phase outlet; the oil phase outlet is connected to a reaction kettle through a pipeline; the water phase outlet is connected to a wastewater tank through a U-shaped separation bend and a cross pipe in sequence; a balance pipe port is arranged on the top of the reaction kettle, the top of the separation tank, the top of the cross pipe and the top of the wastewater tank, and a gas phase balance pipeline is connected between the four balance pipe ports; the height of the cross pipe is lower than that of the oil phase outlet. The oil-water automatic separation device provided by the embodiments of the present application can at least realize automatic separation of oil phase and water phase, is not only suitable for normal pressure scenes, but also can stably operate under micro-pressure or vacuum conditions, thereby widening the application scenes.

Description

Technical Field

[0001] This application relates to the field of chemical production technology, and in particular to an automatic oil-water separation device. Background Technology

[0002] In the fine synthesis of electronic chemicals, such as the preparation of tetrahydroxybenzophenone, the water produced as a reaction byproduct needs to be removed promptly by azeotropic distillation. The distillate, after condensation, forms a mixture of solvent and water. This mixture is then separated by an oil-water separator, with the solvent recycled back into the reaction system and the aqueous phase discharged. Traditional oil-water separators typically have the following drawbacks: 1. Risk of metal contamination: Existing separators are usually made of stainless steel or carbon steel, which easily introduces metal impurities into the system. In electronic chemical production, the introduction of metal ions can severely affect the electrical properties of the product, leading to product defects; 2. Separation during synthesis requires manual operation; 3. Insufficient safety: Electronic chemical production often involves flammable organic solvents. In the existing device design, the location of the mixed liquid inlet may cause droplets to fall and generate static electricity through friction, posing a risk of combustion and explosion; 4. Only suitable for atmospheric pressure environments. Utility Model Content

[0003] In view of the above-mentioned problems in the prior art, the embodiments of this application propose an automatic oil-water separation device. This automatic oil-water separation device can at least achieve automatic separation of oil phase and water phase. It is not only suitable for normal pressure scenarios, but can also operate stably under micro-pressure or vacuum conditions, thus broadening the application scenarios.

[0004] According to one aspect of this application, an automatic oil-water separation device is provided, including a vertical separation tank. The side of the separation tank is provided with an oil phase outlet and a mixed liquid inlet located below the oil phase outlet. The bottom of the separation tank is provided with a water phase outlet. The oil phase outlet is connected to a reaction vessel through a pipeline. The water phase outlet is connected to a wastewater tank in sequence through a U-shaped separating bend and a horizontal pipe. The top of the reaction vessel, the top of the separation tank, the top of the horizontal pipe, and the top of the wastewater tank are all provided with balance pipe ports. A gas phase balance pipe is connected between the four balance pipe ports. The height of the horizontal pipe is lower than that of the oil phase outlet.

[0005] In some embodiments, the vertical height h3 between the highest point of the right branch of the U-shaped liquid separator and the lowest point of the U-shaped liquid separator satisfies the following condition: ρ1*h3=ρ1*h1+ρ2*h2; where ρ1>ρ2, ρ1 represents the density of the aqueous phase, ρ2 represents the density of the oil phase, h1 represents the vertical height between the upper liquid surface of the aqueous phase in the separator and the lowest point of the U-shaped liquid separator, and h2 represents the vertical height between the upper and lower liquid surfaces of the oil phase in the separator.

[0006] In some embodiments, the height of the mixture inlet is located at the interface between the oil phase and the water phase.

[0007] In some embodiments, the vertical height between the mixture inlet and the oil phase outlet is h4, and the vertical height between the mixture inlet and the lowest point of the U-shaped separator bend is h5, where h4 equals h5.

[0008] In some embodiments, the inner wall of the separation tank is provided with a polymer coating.

[0009] In some embodiments, the polymer coating is Halar. ® Coating or Teflon coating.

[0010] In some embodiments, the top of the separator is also provided with an inert gas inlet.

[0011] In some embodiments, the top of the separator is also provided with a gas sampling port, which is connected to an oxygen content analyzer.

[0012] In some embodiments, the side of the separator is also provided with an upper viewing mirror and a lower viewing mirror; the upper viewing mirror is used to observe the top surface of the oil phase, and the lower viewing mirror is used to observe the interface between the oil phase and the water phase.

[0013] In some embodiments, valves for controlling the on / off state are provided at the mixture inlet, the oil phase outlet, and the horizontal pipe.

[0014] The beneficial technical effects of this utility model are as follows: 1. It can achieve continuous feeding and automatic separation of oil and water phases, saving labor costs; 2. During the separation process, the oil phase flows into the reactor from the oil phase outlet, and the water phase flows into the wastewater tank from the water phase outlet through the U-shaped separating bend and the horizontal pipe, achieving a highly efficient separation effect and achieving excellent results where the water phase contains almost no oil phase and the oil phase contains almost no water phase; 3. It can maintain the interface between the oil and water phases at a preset position; 4. It can solve the problem of metal contamination in the production of electronic chemicals, enabling products to meet the most stringent electronic grade standards; 5. Safety is improved, and the device can be used for the two-phase separation of flammable and explosive media; 6. It has wide adaptability, as the device is not only suitable for atmospheric pressure scenarios but can also operate stably under micro-pressure or vacuum conditions, broadening its application scenarios. Attached Figure Description

[0015] To more clearly illustrate the technical solutions in the embodiments of this application or the prior art, the drawings used in the embodiments will be briefly described below. Obviously, the drawings described below are only some embodiments of this application. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort. It is worth noting that, according to industry standard practice, the components are not drawn to scale and are only used for illustrative purposes. In fact, for clarity of discussion, the dimensions of the components can be arbitrarily increased or decreased.

[0016] Figure 1This is a schematic diagram of an automatic oil-water separation device according to an embodiment of this application.

[0017] Figure 2 This is a schematic diagram of an automatic oil-water separation device according to an embodiment of this application.

[0018] Figure 3 This is a schematic diagram of an automatic oil-water separation device according to another embodiment of this application.

[0019] Figure 4 This is a schematic diagram of an automatic oil-water separation device according to yet another embodiment of this application.

[0020] Figure 5 This is a schematic diagram of an automatic oil-water separation device according to yet another embodiment of this application. Detailed Implementation

[0021] The technical solutions of the embodiments of this application will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only a part of the embodiments of this application, and not all of the embodiments. All other embodiments obtained by those skilled in the art based on the embodiments of this application are within the scope of protection of this application.

[0022] The following disclosure provides numerous different embodiments or examples for implementing various features of the provided subject matter. Specific examples of devices and arrangements will be described below to simplify the present invention. These are merely examples and are not intended to limit the present invention. Reference numerals and / or letters may be repeated in various examples of the present invention. Such repetition is for brevity and clarity only and does not in itself indicate a relationship between the various embodiments and / or configurations discussed.

[0023] Furthermore, unless otherwise specified, the embodiments and features described in this application can be combined with each other. This application will now be described in detail with reference to the accompanying drawings and embodiments. It should be understood that the specific structures shown in the figures are merely illustrative and are not intended to limit the scope of this application. Other structures not described in the figures may be provided according to actual needs when describing specific figures, and are not intended to limit the scope of this application.

[0024] Figure 1 This is a schematic diagram of an automatic oil-water separator according to an embodiment of this application. (Reference) Figure 1As shown, according to some embodiments of this application, an automatic oil-water separation device is provided. The automatic oil-water separation device includes a vertical separation tank 10. The side of the separation tank 10 is provided with an oil phase outlet 13 and a mixed liquid inlet 14 located below the oil phase outlet 13. The bottom of the separation tank 10 is provided with a water phase outlet 15. The oil phase outlet 13 is connected to a reaction vessel 11 through a pipe. The water phase outlet 15 is connected to a wastewater tank 12 in sequence through a U-shaped liquid bend 16 and a horizontal pipe 17. The top of the reaction vessel 11, the top of the separation tank 10, the top of the horizontal pipe 17, and the top of the wastewater tank 12 are all provided with balance pipe ports 18. A gas phase balance pipe 19 is connected between the four balance pipe ports 18. The height of the horizontal pipe 17 is lower than that of the oil phase outlet 13. It should be understood that the device of this application is used to separate oil-water mixtures in which the density of the oil phase is less than that of the water phase. The left branch 161 of the U-shaped separating bend 16 of the device is shorter than the right branch 162, and the top of the right branch 162 connects to the horizontal pipe 17, which in turn connects to the wastewater tank 12. The automatic oil-water separation device of this application achieves automatic separation through the liquid level difference generated by the different densities of two immiscible liquids (water phase and oil phase). The device of this application can at least achieve continuous feeding and automatic separation of the oil and water phases, saving labor costs. The automatic oil-water separation device of this application connects the oil phase outlet to the reactor via a pipeline, and the water phase outlet is connected to the wastewater tank sequentially via the U-shaped separating bend and the horizontal pipe. The entire device can be sealed, and gas phase balance is achieved through gas phase balance pipelines connecting the components (reactor, separation tank, wastewater tank). The entire device can be vacuumed, allowing for stable operation under micro-pressure or vacuum conditions, thus broadening its application scenarios. The position of the mixed liquid inlet of the automatic oil-water separation device of this application is lower than that of the oil phase outlet, which can prevent the mixed liquid from dripping directly onto the liquid surface or tank wall during feeding, causing static electricity to be generated by friction, thereby improving the safety of the device.

[0025] Figure 2 This is a schematic diagram of an automatic oil-water separator according to an embodiment of this application. (Reference) Figure 2As shown, in some embodiments, the vertical height h3 between the highest point of the right branch 162 of the U-shaped liquid-distributing bend 16 and the lowest point of the U-shaped liquid-distributing bend 16 satisfies the following condition: ρ1*h3=ρ1*h1+ρ2*h2; where ρ1>ρ2, ρ1 represents the density of the aqueous phase, ρ2 represents the density of the oil phase, h1 represents the vertical height between the upper liquid surface L1 of the aqueous phase in the separator 10 and the lowest point of the U-shaped liquid-distributing bend 16, and h2 represents the vertical height between the upper and lower liquid surfaces of the oil phase in the separator 10. It should be understood that L1 is the upper liquid surface of the aqueous phase, the lower liquid surface of the oil phase, and the interface between the oil phase and the aqueous phase, and L2 is the upper liquid surface of the oil phase. In other words, h2 also represents the vertical height between the upper liquid level L2 of the oil phase in the separator 10 and the interface L1 between the oil and water phases, and h6 represents the vertical height between the highest point of the right branch 162 of the U-shaped liquid separator 16 and the interface L1 between the oil and water phases, satisfying the following condition: ρ1*h6=ρ2*h2. This application, through the design of the U-shaped liquid separator and the height parameters, forms a liquid seal and pressure balance system, enabling the interface between the oil and water phases to automatically stabilize within a preset height range, achieving continuous, automatic, and precise separation of the light and heavy phases.

[0026] Figure 3 This is a schematic diagram of an automatic oil-water separator according to another embodiment of this application. (Reference) Figure 3 As shown, in some embodiments, the height of the mixture inlet 14 is further located at the interface L1 between the oil phase and the water phase, so that the interface between the oil phase and the water phase is more stable in a fixed position, ensuring the separation effect.

[0027] Continue to refer to Figure 3As shown, the diameter of the separator 10 can be d, and the height can be h0, where h0 / d = 3~4 (d can be 200~400mm). This achieves a balance between separation effect and manufacturing cost and space occupation. The device of this application is small in scale, low in manufacturing cost, and can achieve excellent separation effect. The height of the separator 10, the diameter of the separator 10, and the diameter of the U-shaped liquid-liquid bend 16 are related to the properties of the two substances to be separated (the difficulty of separation), the feed flow rate, and specific separation requirements (e.g., the solvent content in the water is less than 0.05%, and the water content in the solvent is less than 0.01%). The greater the separation difficulty, the larger the feed flow rate, and the higher the separation requirements, the longer the separation time is required, and the higher the required height, and the thicker the separator 10 and the U-shaped liquid-liquid bend 16 need to be. Therefore, if the vertical space on site is limited, the separation time can be increased by thickening the separator 10 and the U-shaped liquid-liquid bend 16. If the horizontal space on site is limited, the height can be increased to increase the separation time. For mixtures with small density differences, a higher h0 / d (greater than 3) is needed to prolong the residence time and promote phase separation; for negative pressure or volatile media, a higher h0 / d value (3.5~4.0) can reduce gas phase entrainment.

[0028] Figure 4 This is a schematic diagram of an automatic oil-water separator according to yet another embodiment of this application. (See reference) Figure 4 As shown, in some embodiments, the vertical height between the mixture inlet 14 and the oil phase outlet 13 is h4, and the vertical height between the mixture inlet 14 and the lowest point of the U-shaped distribution bend 16 is h5, where h4 equals h5. It should be understood that other height parameters, such as the vertical height h3 between the highest point of the right branch 162 of the U-shaped distribution bend 16 and the lowest point of the U-shaped distribution bend 16, still satisfy the requirements. Figure 2 The parameter relationships in the embodiments. When the water, a byproduct of the preparation of tetrahydroxybenzophenone, is removed by azeotropic distillation, the automatic oil-water separation device of the embodiments of this application can be used to separate the mixture of distillate (solvent and water), which can achieve continuous, automatic and precise separation of solvent and water. Since h4 equals h5, the separation path of solvent from water is consistent with the separation path of water from solvent, and the interface between solvent and water is more stably maintained at a fixed height.

[0029] Continue to refer to Figure 1 As shown, in some embodiments, a polymer coating is provided on the inner wall 101 of the separation tank 10. The polymer coating may be Halarium. ® Non-stick coatings such as coatings or Teflon coatings that are resistant to strong acids and alkalis and organic solvents. It should be understood that the entire inner wall 101 is coated with a polymer coating, for example, Halarium can be applied by spraying. ®The coating is applied to the stainless steel shell of the separator 10. While the shell of the separator 10 is made of stainless steel to ensure structural strength, its inner wall is coated with a polymer coating that completely isolates the material from contact with the metal shell, fundamentally eliminating the risk of metal ion contamination from electronic chemicals. Specifically, Halar... ® The coating has excellent resistance to high temperature, strong acids and alkalis, and organic solvents. Its smooth and non-adhesive surface can completely isolate the material from contact with the metal casing, solving the problem of metal contamination in the production of electronic chemicals, ensuring the ultra-high purity of electronic chemicals, and enabling the product to meet the most stringent electronic grade standards.

[0030] Continue to refer to Figure 1 Valves are installed at the mixed liquid inlet 14, the oil phase outlet 13, and the horizontal pipe 17 to control the on / off state of the liquid separation process.

[0031] Figure 5 This is a schematic diagram of an automatic oil-water separator according to yet another embodiment of this application. (See reference) Figure 5 As shown, in some embodiments, the top of the separator 10 is also provided with an inert gas inlet 20. The inert gas inlet 20 can be controlled to open and close by a valve, and the inert gas can be nitrogen. Nitrogen or other inert gases can be introduced before operation to replace the air in the automatic oil-water separator, reducing the oxygen content to below a safe level, eliminating the conditions for combustion and explosion within the automatic oil-water separator, thus improving safety and making the automatic oil-water separator particularly suitable for handling flammable solvents. In some embodiments, the top of the separator 10 is also provided with a gas sampling port 21, which is connected to an oxygen content analyzer. A valve is provided at the gas sampling port 21 to control its opening and closing. The oxygen content analyzer can accurately analyze the oxygen content within the automatic oil-water separator. The design of the inert gas inlet 20, the gas sampling port 21, and the oxygen content analyzer can reduce the oxygen content within the automatic oil-water separator to a safe level before the mixed liquid is introduced.

[0032] In some embodiments, the side of the separator 10 is also provided with an upper viewing mirror 22 and a lower viewing mirror 23; the upper viewing mirror 22 is used to observe the top surface of the oil phase, and the lower viewing mirror 23 is used to observe the interface L1 between the oil phase and the water phase (see...). Figure 2 The top surface of the oil phase is also the upper liquid surface L2 of the oil phase (see...). Figure 2 The separation process within the automatic oil-water separator can be monitored in real time through the sight glass.

[0033] Before first use, open valve V1 and close valves V2, V3, V4, and V5. Inject water into the inlet of valve V1 until the water interface seals the mixture inlet 14. Open valve V4 to introduce nitrogen into the automatic oil-water separator to create an inert gas environment. Open valve V5 and, after the oxygen content is detected by an oxygen content analyzer and reduced to below the safe oxygen content limit, close valves V4 and V5 to proceed to the next step, ensuring operational safety. Next, inject the mixture to be separated (water and oil phase solvent) into the mixture inlet 14. The solvent and water are immiscible. Because of its low density, it floats on the surface of the water. When the solvent level reaches the height of the oil phase outlet 13, valves V2 and V3 are opened. The solvent flows out from the oil phase outlet 13 through valve V2 and back to the reactor 11. Water flows out from the water phase outlet 15 through the U-shaped separating bend 16, the horizontal pipe 17 and valve V3 and enters the wastewater tank 12. The mixture to be separated is continuously injected from the mixed liquid inlet 14 to achieve automatic separation. The interface between the oil phase and the water phase is observed to be stable at the same height as the mixed liquid inlet 14 when viewed through the lower sight glass 23. The solvent level is observed to be stable at the same height as the oil phase outlet 13 when viewed through the upper sight glass 22.

[0034] The automatic oil-water separation device provided in this application can be used in the production of electronic chemicals, meeting the high requirements of electronic chemical production. It can achieve automatic, efficient, and precise oil-water separation, and effectively prevent metal contamination and ensure operational safety. In addition, the inert gas inlet and the gas sampling port connected to the oxygen content analyzer designed in this application can control the oxygen content within the device, avoiding the risk of combustion and explosion.

[0035] The above description is merely a preferred embodiment of this application and is not intended to limit this application. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of this application should be included within the protection scope of this application.

Claims

1. An automatic oil-water separation device, characterized in that, The system includes a vertical separation tank, with an oil phase outlet on the side and a mixed liquid inlet located below the oil phase outlet, and an aqueous phase outlet at the bottom of the separation tank. The oil phase outlet is connected to the reactor via a pipeline; The aqueous phase outlet is connected to the wastewater tank via a U-shaped separating bend and a horizontal pipe in sequence; The top of the reactor, the top of the separator, the top of the horizontal pipe, and the top of the wastewater tank are all provided with balance ports, and a gas phase balance pipe is connected between the four balance ports. The height of the horizontal pipe is lower than that of the oil phase outlet.

2. The automatic oil-water separator according to claim 1, characterized in that, The vertical height h3 between the highest point of the right branch of the U-shaped liquid distribution bend and the lowest point of the U-shaped liquid distribution bend satisfies the following condition: ρ1*h3=ρ1*h1+ρ2*h2. Wherein, ρ1>ρ2, ρ1 represents the density of the aqueous phase, ρ2 represents the density of the oil phase, h1 represents the vertical height between the upper liquid level of the aqueous phase in the separator and the lowest point of the U-shaped liquid distribution bend, and h2 represents the vertical height between the upper and lower liquid levels of the oil phase in the separator.

3. The automatic oil-water separator according to claim 2, characterized in that, The height of the mixture inlet is located at the interface between the oil phase and the water phase.

4. The automatic oil-water separator according to claim 3, characterized in that, The vertical height between the mixture inlet and the oil phase outlet is h4, and the vertical height between the mixture inlet and the lowest point of the U-shaped liquid distribution bend is h5, where h4 equals h5.

5. The automatic oil-water separator according to claim 1, characterized in that, The inner wall of the separation tank is coated with a polymer coating.

6. The automatic oil-water separation device according to claim 5, characterized in that, The polymer coating is Halar. ® Coating or Teflon coating.

7. The automatic oil-water separator according to claim 1, characterized in that, The top of the separator is also equipped with an inert gas inlet.

8. The automatic oil-water separator according to claim 7, characterized in that, The top of the separation tank is also equipped with a gas sampling port, which is connected to an oxygen content analyzer.

9. The automatic oil-water separator according to claim 1, characterized in that, The side of the separation tank is also equipped with an upper viewing mirror and a lower viewing mirror; The upper viewing mirror is used to observe the top surface of the oil phase, and the lower viewing mirror is used to observe the interface between the oil phase and the water phase.

10. The automatic oil-water separator according to claim 1, characterized in that, Valves for controlling the on / off state are installed at the inlet of the mixture, the outlet of the oil phase, and on the horizontal pipe.

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