A device and method for removing trace dispersion of grease ion impurities

Abstract

The application provides a device and method for removing grease ion impurities by micro-dispersion extraction. The device comprises a micro-dispersion assembly, an extraction separation assembly, a first fiber coalescence phase separation assembly, a second fiber coalescence water removal assembly, a water phase storage tank, and a pH sensor. In the micro-dispersion assembly, waste grease and water phase extractant form micro-scale grease droplets, so that ion impurities quickly migrate across the interface to the water phase. Subsequently, extraction is carried out through a second extraction tank, and purified oil phase with reduced ion impurity content and low water content is obtained through first fiber coalescence filler phase separation, oil-water phase separation buffer, and second fiber coalescence filler water removal. The application can alleviate the problems of low mass transfer rate, local pH unevenness, excessive emulsification, slow oil-water phase separation, and water entrainment in the oil phase in the traditional water washing or acid washing process, and is suitable for removing ion impurities from gutter oil, kitchen waste oil, hogwash oil, waste animal and plant oil, and mixed grease before preparing green aviation fuel, biodiesel, or hydrogenation raw materials.

Description

Technical Field

[0001] This invention relates to the field of oil and fat ion impurity removal technology, and in particular to an apparatus and method for removing oil and fat ion impurities by micro-dispersion extraction. Background Technology

[0002] Waste oils are an important renewable carbon resource for the production of green jet fuel, biodiesel, and hydrodeoxygenated fuels. During collection, storage, transportation, and pretreatment, waste cooking oil, kitchen waste oil, swill oil, and waste animal and vegetable oils often contain moisture, inorganic salts, metallic soaps, colloids, phospholipids, chlorinated compounds, and other ionic impurities. These impurities can lead to catalyst poisoning, bed scaling, corrosion, increased pressure drop, and product quality fluctuations during subsequent hydrotreating, deoxygenation, isomerization, or cracking processes. Therefore, developing efficient, continuous, low-energy-consumption methods with minimal oil phase loss for the removal of ionic impurities before waste oils enter the downstream processes of green jet fuel or biodiesel is of great significance.

[0003] Current waste oil pretreatment methods primarily employ processes such as water washing, acid washing, alkali washing, adsorption, sedimentation dehydration, filtration, centrifugation, or distillation. While water washing or acid washing offers advantages like simple equipment and low cost, when the ion concentration in the waste oil is low, the oil phase viscosity is high, or the ions exist in the form of metal soaps, complexes, or colloidal particles, the oil-water interface constructed by traditional stirred tank processes is limited, resulting in a long mass transfer distance and a low rate of ion migration from the oil phase to the water phase. Increasing the stirring intensity to enhance mass transfer can easily lead to the formation of a stable emulsion layer, causing difficulties in oil-water separation, water entrainment in the oil phase, oil phase loss, and an increased burden on subsequent dehydration.

[0004] Furthermore, traditional stirring or mechanical mixing processes are prone to localized pH imbalances. When local acid or alkali concentrations are too high or too low, metal complexes, saponifications, precipitates, or colloids may form near the oil-water interface, further hindering ion migration and increasing oil phase loss. For continuous green aviation kerosene production processes using waste oil as raw material, simply relying on prolonged stirring, static stratification, or gravity settling is not conducive to forming compact, stable, and scalable front-end pretreatment equipment. Summary of the Invention

[0005] The purpose of this invention is to overcome the problems of low mass transfer efficiency, easy emulsification under strong stirring, slow oil-water separation, and water inclusion in the oil phase in existing oil ion impurity removal technologies, and to provide a micro-dispersion extraction device and method for removing oil ion impurities.

[0006] To achieve the above objectives, the present invention adopts the following technical solution:

[0007] In a first aspect, the present invention provides a device for the micro-dispersion extraction and removal of oil and fat ion impurities, comprising:

[0008] Micro-dispersed components, comprising:

[0009] A water phase distribution plate has a water tank on its upper surface and a first water phase inlet hole on its side, which is connected to the water tank.

[0010] An oil phase distribution plate has its lower end face abutting against the upper end face of the water phase distribution plate. An oil groove is formed on the upper end face of the oil phase distribution plate. An oil phase feed hole is provided on the side of the oil phase distribution plate, and the oil phase feed hole is connected to the oil groove. A plurality of first vertical channels are formed on the oil phase distribution plate around the outer periphery of the oil groove, and the first vertical channels are connected to the water groove.

[0011] A droplet generating plate has its lower end face abutting against the upper end face of an oil phase distribution plate. A droplet collecting groove is formed on the upper end face of the droplet generating plate. Multiple oil-water shear grooves are formed on the droplet generating plate outside the droplet collecting groove, and these oil-water shear grooves are connected to the droplet collecting groove. A second vertical channel is formed inside the droplet generating plate corresponding to a first vertical channel, with its upper end connected to the oil-water shear groove and its lower end connected to the first vertical channel. Multiple third vertical channels are formed inside the droplet generating plate corresponding to an oil groove, with their upper ends connected to the oil-water shear groove and their lower ends connected to the oil groove. The third vertical channels are located inside the second vertical channels.

[0012] Extraction and separation components, comprising:

[0013] First extraction tank;

[0014] The second extraction vessel is coaxially disposed inside the first extraction vessel;

[0015] The lower end face of the second extraction vessel abuts against the lower end face of the first extraction vessel, and the upper end extends out of the first extraction vessel; the upper end face of the droplet generating plate abuts against the lower end face of the first extraction vessel; the droplet collecting groove communicates with the interior of the second extraction vessel;

[0016] The first extraction tank has a second aqueous phase inlet / outlet hole on one side. The second extraction tank has a first aqueous phase inlet / outlet pipe and a second aqueous phase inlet / outlet pipe respectively on the side of the second extraction tank and inside the first extraction tank along the vertical direction. The second aqueous phase inlet / outlet pipe extends out of the first extraction tank.

[0017] Preferred options also include:

[0018] A primary fiber coalescing phase separation assembly, comprising:

[0019] The first phase separation tank is provided with a first fiber coalescing packing material, which is made of oleophilic and hydrophobic fibers and hydrophilic and oleophobic fibers through weaving; the upper end of the second extraction tank extends out of the first extraction tank and is connected to one end of the first phase separation tank.

[0020] An oil-water phase separation buffer tank, one side of which is connected to the other end of the first phase separation tank;

[0021] Aqueous phase storage tank, the upper end of which is connected to the lower end of the oil-water phase buffer tank;

[0022] The aqueous phase storage tank is equipped with a first aqueous phase pipe, a second aqueous phase pipe, and a third aqueous phase pipe. One end of the first aqueous phase pipe is connected to the aqueous phase storage tank, and the other end is connected to the first aqueous phase inlet.

[0023] One end of the second water phase pipeline is connected to the water phase storage tank, and the other end is connected to the second water phase inlet / outlet.

[0024] One end of the third water phase pipeline is connected to the water phase storage tank, and the other end is connected to the second water phase inlet / outlet pipe.

[0025] Preferred options also include:

[0026] A secondary fiber coalescing dewatering assembly, comprising:

[0027] The second phase separation tank is equipped with a second fiber coalescing packing material, which is made of hydrophilic fibers through weaving.

[0028] One end of the second phase separation tank is connected to the upper end of the oil-water phase separation buffer tank;

[0029] The second phase separation tank is provided with a water phase outlet at the lower end and an oil phase outlet at the upper end.

[0030] Preferably, the aqueous phase storage tank is also equipped with a pH sensor for monitoring the pH value of the aqueous phase in the aqueous phase storage tank;

[0031] It also includes: aqueous phase replenishment tank and acid / alkali solution storage tank;

[0032] The aqueous phase replenishment tank and the acid / alkali solution storage tank are respectively connected to the aqueous phase storage tank.

[0033] Preferably, the aqueous storage tank is also equipped with a liquid level sensor.

[0034] Preferably, the width of the oil-water shear groove is 0.05~5 mm;

[0035] The apertures of the first, second, and third vertical channels are 0.05~3 mm;

[0036] The oleophilic and hydrophobic fibers and the hydrophilic and oleophilic fibers are woven together to obtain a first fiber coalescing filler with a pore size of 50~1500 μm;

[0037] The hydrophilic fibers are woven to obtain a second fiber coalescing filler with a pore size of 1~500 μm.

[0038] Preferred options also include:

[0039] An oil phase feed tank is used to store oils; the oil phase feed tank is connected to an oil phase inlet.

[0040] A purified oil phase storage tank, which is connected to the oil phase discharge port;

[0041] An ion-rich aqueous phase storage tank, which is connected to the aqueous phase storage tank.

[0042] Secondly, the present invention also provides a method for micro-dispersed extraction and removal of oil ion impurities, applied to the aforementioned micro-dispersed extraction and removal device for oil ion impurities, comprising the following steps:

[0043] The grease is fed into the oil phase distribution plate through the oil phase feed hole;

[0044] The aqueous phase in the aqueous phase storage tank is introduced into the aqueous phase distribution plate through the first aqueous phase inlet hole;

[0045] The aqueous phase in the aqueous phase storage tank enters the first extraction tank through the second aqueous phase inlet / outlet port;

[0046] In this process, the oil is sheared into oil droplets by the aqueous phase in the oil-water shear tank and then enters the droplet collection tank. The oil droplets in the droplet collection tank then enter the second extraction tank and are extracted by the aqueous phase.

[0047] The extracted oil-water mixture enters the first phase separation tank, and after being captured, coalesced, and demulsified by the first fiber coalescing packing, it enters the oil-water phase separation buffer tank. The lower aqueous phase enters the aqueous phase storage tank, and the upper oil phase enters the second phase separation tank. After being separated by the second fiber coalescing packing, the upper oil phase is discharged through the oil phase outlet to obtain the purified grease.

[0048] Preferably, it includes the following steps:

[0049] The aqueous phase includes water, acidic aqueous solution, and aqueous solution containing a complexing agent;

[0050] The acid in the acidic aqueous solution is selected from one or more of hydrochloric acid, sulfuric acid, nitric acid, phosphoric acid, formic acid, acetic acid, citric acid, oxalic acid, and lactic acid.

[0051] The complexing agent in the aqueous solution is selected from one or more of citrate, acetate, EDTA, DTPA, NTA, aminocarboxylic acid compounds or their salts, and the concentration of the complexing agent in the aqueous solution is 0.0001~1 mol / L.

[0052] A pH sensor is used to monitor the pH value of the aqueous phase in the aqueous phase storage tank. The pH of the aqueous phase in the aqueous phase storage tank is maintained at 1.5~7.0 by adding aqueous phase, acid or alkali solution to the aqueous phase storage tank.

[0053] Preferably, the extraction temperature is 20~95℃;

[0054] The flow rate of grease entering the oil phase distribution plate through the oil phase feed hole is 1~5000 mL / h, and the flow rate of aqueous phase entering the aqueous phase distribution plate through the first aqueous phase inlet hole is 0.1~5000 mL / h.

[0055] The flow rate of the aqueous phase entering the first extraction tank is 1~10000 mL / h.

[0056] The micro-dispersive extraction and removal device and method for oil and fat ion impurities of the present invention have the following advantages over the prior art:

[0057] The present invention relates to a micro-dispersion extraction and removal device and method for removing ionic impurities from oils and fats, comprising a micro-dispersion component including an aqueous phase distribution plate, an oil phase distribution plate, and a droplet generation plate. This component shears the oil into oil droplets, significantly shortening the mass transfer distance of ionic impurities from waste oils to the aqueous phase, thereby improving extraction efficiency and effectiveness. During the oil droplet flotation process, the present invention maintains a short-lifespan micro-dispersion state, ensuring a continuous spatial connection between the extraction process and the subsequent phase separation process, without relying on prolonged strong stirring. By adjusting the direction and velocity of the aqueous phase flow, the present invention controls the apparent flotation velocity and residence time of the oil droplets, allowing for adjustment of the oil-water contact time and mass transfer degree without changing the height of the micro-dispersion component and the second extraction tank, and providing operational control space for the ion removal process of different waste oil raw materials. The present invention employs functionally differentiated bi-stage fiber coalescing packing. The first fiber coalescing packing achieves rapid capture, coalescence, demulsification, and main phase separation of oil and water droplets after micro-dispersion extraction; the second fiber coalescing packing achieves deep interception, coalescence, and discharge of trace amounts of entrained water in the oil phase during preliminary purification. This dual-stage structure avoids prolonged stratification due to excessively small droplets after micro-dispersion extraction, and also reduces the risk of ion-rich aqueous phase entrainment into the oil phase product. The invention incorporates an aqueous phase replenishment tank, acid / alkali solution storage tanks, and a pH sensor. The pH, volume, and ion load of the circulating aqueous phase can be regulated by adding acid or alkali, replenishing with fresh aqueous phase, and discharging ion-rich aqueous phase. This mitigates the formation of complexes, precipitates, or colloids caused by localized pH unevenness, reduces interfacial contamination and oil phase loss, and improves continuous operation stability. This invention is suitable for removing ion impurities from waste cooking oil, kitchen waste oil, swill oil, waste animal and vegetable oils, and their mixtures before preparing green jet fuel, biodiesel, or hydrogenation feedstock. It offers advantages such as compact equipment, low energy consumption, high degree of continuous operation, and flexible process control. Attached Figure Description

[0058] To more clearly illustrate the technical solutions in the embodiments of the present invention or the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present invention. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0059] Figure 1 This is a schematic diagram of the structure of the micro-dispersion extraction and removal device for oil and fat ion impurities of the present invention;

[0060] Figure 2 This is an exploded view of the aqueous phase distribution plate, oil phase distribution plate, droplet generation plate, and cover plate in the micro-dispersed component of the present invention.

[0061] Figure 3 This is a schematic diagram of the structure of the micro-dispersed component of the present invention;

[0062] Figure 4 This is a top view and a cross-sectional view of the aqueous phase distribution plate of the present invention;

[0063] Figure 5 This is a top view and a cross-sectional view of the oil phase distribution plate of the present invention;

[0064] Figure 6 The images show a top view and a cross-sectional view of the droplet generating plate of the present invention.

[0065] Figure 7 This is a top view and a cross-sectional view of the cover plate of the present invention;

[0066] Figure 8 This is a schematic diagram of the extraction and separation component of the present invention;

[0067] Figure 9 This is a schematic diagram illustrating the generation of oil droplets according to the present invention;

[0068] Figure 10 This is a schematic diagram illustrating the contact between the aqueous phase and oil droplets in the present invention, and the countercurrent and cocurrent extraction processes.

[0069] Figure 11 This is a schematic diagram of the connection structure of the first phase separation tank, the oil-water phase separation buffer tank, and the second phase separation tank of the present invention.

[0070] Figure 12 To characterize Fe using the fluorescence response of Rhodamine B 3+ The cross-oil-water interface migration behavior;

[0071] Figure 13 To extract Fe from the oil according to the methods in Example 1 and Comparative Example 1. 3+ Extraction efficiency curve;

[0072] Figure 14 To obtain different apparent mass transfer rate constants of ions according to the methods of Example 1 and Comparative Example 1;

[0073] Figure 15 The content of each ion in the oil before and after extraction was tested according to the method in Example 1;

[0074] Figure 16 The method in Example 1 was used to test the water content of the oil phase before it entered the second phase separation tank and the water content after it passed through the second phase separation tank. Detailed Implementation

[0075] To make the objectives, technical solutions, and advantages of the embodiments of the present invention clearer, the technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some, not all, of the embodiments of the present invention. The components of the embodiments of the present invention described and shown in the accompanying drawings can generally be arranged and designed in various different configurations.

[0076] Therefore, the following detailed description of the embodiments of the invention provided in the accompanying drawings is not intended to limit the scope of the claimed invention, but merely to illustrate selected embodiments of the invention. All other embodiments obtained by those skilled in the art based on the embodiments of the invention without inventive effort are within the scope of protection of the invention.

[0077] It should be noted that similar labels and letters in the following figures indicate similar items. Therefore, once an item is defined in one figure, it does not need to be further defined and explained in subsequent figures.

[0078] In the description of this invention, it should be understood that the orientation or positional relationship indicated by terms such as "above" is based on the orientation or positional relationship shown in the accompanying drawings, or the orientation or positional relationship in which the product of this invention is usually placed when in use, or the orientation or positional relationship in which those skilled in the art are usually understood. It is only for the convenience of describing this invention and simplifying the description, and is not intended to indicate or imply that the device or element referred to must have a specific orientation, or be constructed and operated in a specific orientation. Therefore, it should not be construed as a limitation of this invention.

[0079] Furthermore, the terms "first," "second," etc., are used only to distinguish descriptions and should not be interpreted as indicating or implying relative importance.

[0080] The technical solutions of the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention. Obviously, the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative effort are within the scope of protection of the present invention.

[0081] This application provides a device for the micro-dispersion extraction and removal of oil and fat ion impurities, such as... Figures 1-11 As shown, it includes:

[0082] Micro-dispersed components, comprising:

[0083] A water phase distribution plate 1 has a water tank 10 on its upper end face and a first water phase inlet hole 11 on its side, which is connected to the water tank 10.

[0084] The lower end face of the oil phase distribution plate 2 abuts against the upper end face of the water phase distribution plate 1. An oil groove 20 is provided on the upper end face of the oil phase distribution plate 2. An oil phase feed hole 21 is provided on the side of the oil phase distribution plate 2, and the oil phase feed hole 21 is connected to the oil groove 20. Multiple first vertical channels 22 are provided on the oil phase distribution plate 2 around the outer periphery of the oil groove 20, and the first vertical channels 22 are connected to the water groove 10.

[0085] A droplet generating plate 3 has its lower end face abutting against the upper end face of an oil phase distribution plate 2. A droplet collecting groove 30 is formed on the upper end face of the droplet generating plate 3. Multiple oil-water shear grooves 31 are formed on the droplet generating plate 3 outside the droplet collecting groove, and the oil-water shear grooves 31 are connected to the droplet collecting groove 30. A second vertical channel 32 is formed inside the droplet generating plate 3 corresponding to the first vertical channel 22. The upper end of the second vertical channel 32 is connected to the oil-water shear groove 31, and the lower end is connected to the first vertical channel 22. Multiple third vertical channels 33 are formed inside the droplet generating plate 3 corresponding to the oil tank 20. The upper end of the third vertical channel 33 is connected to the oil-water shear groove 31, and the lower end is connected to the oil tank 20. The third vertical channels 33 are located inside the second vertical channels 32.

[0086] Extraction and separation components, comprising:

[0087] First extraction tank 4;

[0088] The second extraction vessel 41 is coaxially disposed inside the first extraction vessel 4;

[0089] The lower end face of the second extraction tank 41 abuts against the lower end face of the first extraction tank 4, and the upper end extends out of the first extraction tank 4; the upper end face of the droplet generating plate 3 abuts against the lower end face of the first extraction tank 4; the droplet collecting tank 30 is connected to the interior of the second extraction tank 41.

[0090] The first extraction tank 4 has a second aqueous phase inlet / outlet hole 40 on one side. The second extraction tank 41 has a first aqueous phase inlet / outlet pipe 42 and a second aqueous phase inlet / outlet pipe 43 on its side and inside the first extraction tank, respectively, along the vertical direction. The second aqueous phase inlet / outlet pipe 43 extends out of the first extraction tank 4.

[0091] The present invention provides a micro-dispersion extraction and removal device for oil and fat ion impurities, comprising a micro-dispersion component and an extraction and separation component. The micro-dispersion component includes an aqueous phase distribution plate 1, an oil phase distribution plate 2, and a droplet generating plate 3, stacked sequentially from bottom to top. The aqueous phase distribution plate 1 has an annular water tank 10 on its upper surface and a first aqueous phase inlet 11 on its side, the first aqueous phase inlet 11 being connected to the annular water tank 10. The oil phase distribution plate 2 has an oil tank 20 on its upper surface and an oil phase feed hole 21 on its side. The oil phase feed hole 21 connects to the oil tank 20. Multiple vertically arranged first vertical channels 22 are provided on the oil phase distribution plate 2 around the outer periphery of the oil tank 20 and corresponding to the annular water tank 10. The lower end of each first vertical channel 22 connects to the water tank 10. A droplet generating plate 3 has a circularly shaped droplet collecting groove 30 on its upper surface. Multiple oil-water shear grooves 31 are radially arranged on the upper surface of the droplet generating plate 3 and located within the droplet collecting groove 30. Each oil-water shear groove 31 connects to the droplet collecting groove 30. The shear groove 31 corresponds one-to-one with the first vertical channel 22. A second vertical channel 32 is provided within the droplet generating plate 3 corresponding to the first vertical channel 22. Multiple third vertical channels 33 are provided within the droplet generating plate 3 corresponding to the oil tank 20. The first vertical channel 22, oil-water shear groove 31, second vertical channel 32, and third vertical channel 33 are all one-to-one. The upper end of the second vertical channel 32 connects to the oil-water shear groove 31, and the lower end connects to the first vertical channel 22. The upper end of the third vertical channel 33 connects to the oil-water shear groove 31. The groove 31 is connected to the lower end of the oil tank 20; the water tank 10, the oil tank 20, and the droplet collection tank 30 are all coaxially arranged; the projection of the oil tank 20 in the horizontal plane is located in the water tank 10, and the projection of the droplet collection tank 30 in the horizontal plane is located in the oil tank 20; the extraction and separation assembly includes: a first extraction tank 4 and a second extraction tank 41, the second extraction tank 41 is coaxially arranged in the first extraction tank 4, the upper end face of the droplet generating plate 3 is attached to the lower end face of the first extraction tank 4, and the droplet collection tank 30 is connected to the interior of the second extraction tank 41.

[0092] The working principle of the micro-dispersion extraction and removal device for oil ion impurities of the present invention is as follows: Aqueous phase is introduced into the first aqueous phase inlet 11 of the aqueous phase distribution plate 1. The aqueous phase enters the water tank 10 through the first aqueous phase inlet 11, and moves upward through the first vertical channel 22 into the second vertical channel 32, continuing upward and entering the oil-water shearing tank 31. Oil is introduced into the oil phase inlet 21 of the oil phase distribution plate 2. The oil enters the oil tank 20 through the oil phase inlet 21, and then enters the oil-water shearing tank 31 through the third vertical channel 33. In the oil-water shearing tank 31, the aqueous phase shears the oil into oil droplets (e.g., ...). Figure 9 As shown); Figure 8 As shown, the oil droplets 44 enter the second extraction tank 41 and move upward under the action of buoyancy (as shown). Figure 10 As shown in Figure a), if the aqueous phase enters the first extraction tank 4 through the second aqueous phase inlet / outlet 40, then enters the second extraction tank 41 through the first aqueous phase inlet / outlet pipe 42, and flows out through the second aqueous phase inlet / outlet pipe 43, the aqueous phase comes into contact with the oil droplets and undergoes countercurrent extraction (as shown in Figure a). Figure 10 (As shown in b); if the aqueous phase enters the second extraction tank 41 through the second aqueous phase inlet / outlet pipe 43 and flows upward in the second extraction tank 41, then enters the first extraction tank 4 through the first aqueous phase inlet / outlet pipe 42, and finally flows out through the second aqueous phase inlet / outlet hole 40, in this way, the aqueous phase contacts the oil droplets and performs co-current extraction (as shown in b). Figure 10 (As shown in c). When the aqueous extractant and oil droplets rise in the same direction, forming a co-current flow, the aqueous flow increases the apparent rising velocity of the oil droplets and shortens their residence time. When the aqueous extractant and oil droplets rise in opposite directions, forming a counter-current flow, the aqueous flow decreases the apparent rising velocity of the oil droplets and prolongs their residence time. During the extraction process, ionic impurities in the oil are extracted into the aqueous phase, thus achieving the removal of ionic impurities from the oil.

[0093] Further reference Figure 2 As shown, a cover plate 34 is also provided on the droplet generating plate 3. A droplet collecting hole 35 is provided on the cover plate 34 corresponding to the droplet collecting groove 30. The droplet collecting hole 35 is coaxial with the droplet collecting groove 30 and has the same diameter. The lower end of the cover plate 34 is also provided with an upper shear groove (such as...) corresponding to the oil-water shear groove. Figure 2 The upper shear groove (numbered 36) on the lower end face of the cover plate 34 is connected to the droplet collection hole 35. The upper shear groove on the cover plate 34 is identical in shape, size, position, and dimensions to the oil-water shear groove on the droplet generating plate 3. The two oil-water shear grooves form an oil-water shear channel, within which the aqueous phase shears the oil into oil droplets. If the cover plate 34 is included, its upper end face is attached to the lower end face of the first extraction tank 4, and the droplet collection hole 35 connects to the interior of the second extraction tank 41.

[0094] Further, refer to Figure 4The diagram shows a top view and a cross-sectional view of the aqueous phase distribution plate 1. The aqueous phase distribution plate 1 is a circular plate, a square plate, or a polygonal plate, preferably a square plate. Its side length is 20~200 mm (i.e., both length and width are 20~200 mm), preferably 40~80 mm, and its thickness is 1~20 mm, preferably 3~8 mm. The projection of the water tank 10 on the plane is annular, wherein the diameter of the inner circle is 5~80 mm, preferably 20~30 mm, the diameter of the outer circle is 10~120 mm, preferably 25~40 mm, the width of the tank is 1~20 mm, preferably 2~8 mm, and the depth of the water tank 10 is 0.1~10 mm, preferably 0.5~3 mm. The diameter of the first aqueous phase inlet hole 11 is 0.2~10 mm, preferably 1~5 mm. The first aqueous phase inlet hole 11 communicates with the water tank 10 along the side of the aqueous phase distribution plate 1, and is used to uniformly introduce the aqueous phase extractant into the water tank 10.

[0095] refer to Figure 5 The diagram shows a top view and a cross-sectional view of the oil phase distribution plate 2. The oil phase distribution plate 2 is a circular plate, a square plate, or a polygonal plate, preferably a square plate. Its side length is 20-200 mm, preferably 40-80 mm, and its thickness is 1-20 mm, preferably 3-8 mm. The projection of the oil groove 20 on the plane is annular, wherein the diameter of the inner circle is 2-70 mm, preferably 10-25 mm, the diameter of the outer circle is 5-100 mm, preferably 15-35 mm, the groove width is 0.5-20 mm, preferably 2-8 mm, and the depth of the oil groove 20 is 0.1-10 mm, preferably 0.5-3 mm. The first vertical channels 22 are arranged at intervals along the outer periphery of the oil groove 20, with a number of 4-128, preferably 8-48, and a hole diameter of 0.05-3 mm, preferably 0.2-1.0 mm, and a height of 0.5-20 mm, preferably 2-8 mm. The diameter of the oil phase feed hole 21 is 0.2~10 mm, preferably 1~5 mm. The oil phase feed hole 21 is connected to the oil tank 20 along the side of the oil phase distribution plate 2, and is used to uniformly introduce the grease into the oil tank 20.

[0096] refer to Figure 6As shown, this is a top view and a cross-sectional view of the droplet generating plate 3. The droplet generating plate 3 has a side length of 20~200 mm, preferably 40~80 mm, and a thickness of 1~20 mm, preferably 3~8 mm. The projection of the droplet collecting groove 30 on the plane is a circle with a diameter of 1~50 mm, preferably 5~20 mm, and a depth of 0.1~10 mm, preferably 0.5~3 mm. The oil-water shearing groove 31 is arranged radially along the outer periphery of the droplet collecting groove 30, with a width of 0.05~5 mm, preferably 0.1~2 mm, a depth of 0.02~3 mm, preferably 0.05~1 mm, and a length of 1~50 mm, preferably 5~20 mm. The second vertical channel 32 and the third vertical channel 33 are respectively connected to the oil-water shearing groove 31. The aperture of both is 0.05~3 mm, preferably 0.2~1.0 mm, and the height is 0.5~20 mm, preferably 2~8 mm.

[0097] refer to Figure 7 The diagram shows a top view and a cross-sectional view of the cover plate 34. The cover plate 34 is positioned above the droplet generating plate 3 and, together with the droplet generating plate 3, defines the oil-water shear channel and seals the droplet collecting groove 30. The cover plate 34 is a circular, square, or polygonal plate, preferably a square plate. Its side length matches that of the droplet generating plate 3, being 20-200 mm, preferably 40-80 mm, and its thickness is 0.5-20 mm, preferably 2-6 mm. The projection of the droplet collecting hole 35 onto the plane is a circle, with a diameter of 1-50 mm, preferably 5-20 mm, and a depth of 0.5-20 mm, preferably 2-6 mm. An upper shear groove 36 is provided on the lower end of the cover plate 34 corresponding to the position of the oil-water shear groove 31. The upper shear groove 36 and the oil-water shear groove 31 on the droplet generating plate 3 together form a closed oil-water shear channel. The width of the upper shear groove 36 is 0.05~5 mm, preferably 0.1~2 mm; the depth is 0.02~3 mm, preferably 0.05~1 mm; and the length is 1~50 mm, preferably 5~20 mm.

[0098] In some embodiments, it also includes:

[0099] A primary fiber coalescing phase separation assembly, comprising:

[0100] The first phase separation tank 5 is provided with a first fiber coalescing filler 51, which is made of oleophilic and hydrophobic fibers and hydrophilic and oleophobic fibers through weaving; the upper end of the second extraction tank extends out of the first extraction tank and is connected to one end of the first phase separation tank.

[0101] Oil-water phase separation buffer tank 6, one side of which is connected to the other end of the first phase separation tank 5;

[0102] Aqueous phase storage tank 7, the upper end of which is connected to the lower end of oil-water phase buffer tank 6;

[0103] The water phase storage tank 7 is equipped with a first water phase pipe 71, a second water phase pipe 72, and a third water phase pipe 73. One end of the first water phase pipe 71 is connected to the water phase storage tank 7, and the other end is connected to the first water phase inlet 11.

[0104] One end of the second water phase pipeline 72 is connected to the water phase storage tank 7, and the other end is connected to the second water phase inlet / outlet 40;

[0105] One end of the third water phase pipeline 73 is connected to the water phase storage tank 7, and the other end is connected to the second water phase inlet / outlet pipe 43.

[0106] Specifically, in the above embodiment, the aqueous phase and oil droplets undergo extraction in the second extraction tank. The extracted oil-water mixture enters the first phase separation tank 5. Since the first phase separation tank 5 is equipped with a first fiber coalescing packing 51, which is woven from oleophilic and hydrophobic fibers, the oil-water mixture undergoes capture, collision, coalescence, growth, and demulsification on the surface of the first fiber coalescing packing 51. The aqueous phase preferentially aggregates on the surface of the hydrophilic and hydrophobic fibers, while the oil phase preferentially wets and passes through the oleophilic and hydrophobic fiber regions, thereby promoting the capture, coalescence, and growth of dispersed droplets, forming an oil phase and an ion-rich aqueous phase that are easily separated by gravity (the oil phase has a lower density than the water phase, the oil phase is located in the upper layer, and the water phase is located in the lower layer). After coalescence treatment in the first phase separation tank 5, the oil-water mixture... The oil-water mixture enters the oil-water phase buffer tank 6, where it settles under gravity to form an ion-rich aqueous phase (lower layer) and a preliminarily purified oil phase (upper layer). The lower aqueous phase then enters the aqueous phase storage tank 7. The aqueous phase storage tank 7 stores the aqueous phase (i.e., the aqueous phase extractant). A portion of the aqueous phase enters the water tank through the first aqueous phase pipe 71 and the first aqueous phase inlet hole 11 to shear the oil and form oil droplets. Another portion of the aqueous phase enters the first extraction tank 4 through the second aqueous phase pipe 72 and the second aqueous phase inlet / outlet hole 40 as the extractant, and then enters the second extraction tank 41 to extract the oil droplets. The aqueous phase in the second extraction tank 41 then returns to the aqueous phase storage tank 7 through the second aqueous phase inlet / outlet pipe 43 and the third aqueous phase pipe 73 to form a circulation loop.

[0107] In some embodiments, it also includes:

[0108] A secondary fiber coalescing dewatering assembly, comprising:

[0109] The second phase separation tank 8 is provided with a second fiber coalescing packing 81, which is made of hydrophilic fibers through weaving.

[0110] One end of the second phase separation tank 8 is connected to the upper end of the oil-water phase separation buffer tank 6 via a pipeline;

[0111] The second phase separation tank 8 has a water phase outlet 82 at the lower end and an oil phase outlet 83 at the upper end.

[0112] In the above embodiment, the upper oil phase in the oil-water phase separation buffer tank 6 enters the second phase separation tank 8 through a pipeline; the second phase separation tank 8 is provided with a second fiber coalescing packing 81, which is made of hydrophilic fibers through weaving; the tiny water droplets entrained in the oil phase are intercepted, coalesced and discharged on the surface of the hydrophilic water-capturing fiber packing to obtain a low-water-content purified oil phase product; finally, the tiny water droplets entrained in the oil phase are discharged through the water phase outlet 82 at the lower end of the second phase separation tank 8 after aggregation, while the finally purified oil phase is collected through the oil phase outlet 83 at the upper end of the second phase separation tank 8 to obtain the purified oil phase product.

[0113] In some embodiments, the first fiber coalescing filler is obtained by weaving oleophilic and hydrophobic fibers and hydrophilic and oleophobic fibers, with a mass ratio of oleophilic and hydrophobic fibers to hydrophilic and oleophobic fibers of 1:9 to 9:1, preferably 3:7 to 7:3; the first fiber coalescing filler is configured with a multi-level pore structure by cross weaving, X-shaped weaving, Ω-shaped weaving, layered laying, radial gradient laying, or a combination thereof; the average diameter of the oleophilic and hydrophobic fibers is 20 to 1000 μm, preferably 50 to 500 μm; the oleophilic and hydrophobic fibers are woven to obtain a porous first fiber coalescing filler with a porosity of 70% to 98%, preferably 85% to 95%; and a pore size distribution of 50 to 1500 μm, preferably 100 to 800 μm. The oleophilic and hydrophobic fibers include one or more of the following: polypropylene (PP) fibers, polyethylene (PE) fibers, polytetrafluoroethylene (PTFE) fibers, polyvinylidene fluoride (PVDF) fibers, polystyrene (PS) fibers, polyurethane (PU) fibers, polyester fibers, hydrophobically modified glass fibers, or hydrophobically modified metal fibers. The hydrophilic and oleophilic fibers include one or more of the following: cellulose fibers, cotton fibers, wood pulp fibers, viscose fibers, polyamide fibers, polyacrylonitrile (PAN) fibers, polyvinyl alcohol (PVA) fibers, hydrophilic modified polyester fibers, hydrophilic modified glass fibers, stainless steel fibers, or modified fibers with surface grafted hydroxyl, carboxyl, sulfonic acid, or polyethylene glycol segments.

[0114] In some embodiments, the second fiber coalescing packing is formed by weaving, winding, stacking, or pressing hydrophilic fibers to create a porous fiber coalescing packing. It is used to intercept, capture, and coalesce entrained micro-water droplets under continuous oil phase flow conditions, allowing the coalesced water droplets to enter the water collection area under gravity and be discharged through the water phase outlet 82. The pore size distribution of the second fiber coalescing packing is smaller than that of the first fiber coalescing packing. The packing porosity is 60%–98%, preferably 80%–95%; the main pore size distribution is 1–500 μm, preferably 10–100 μm; the average fiber diameter of the hydrophilic fibers is 1–500 μm, preferably 5–100 μm. The hydrophilic water-capturing fibers include one or more of the following: cotton fibers, wood pulp fibers, viscose fibers, polyamide fibers, polyacrylonitrile fibers, polyvinyl alcohol fibers, hydrophilic modified polyester fibers, hydrophilic modified glass fibers, stainless steel fibers, ceramic fibers, or modified fibers with hydroxyl, carboxyl, amide, or sulfonic acid groups on their surface. The primary fiber coalescing packing is used to treat the oil-water micro-dispersion system after extraction. Its main objectives are demulsification, coarse coalescence, and oil-water phase separation. Therefore, composite fiber packing with larger pore size, high porosity, and heterogeneous wettability is preferred to reduce pressure drop and the risk of secondary emulsification. The secondary fiber coalescing packing is used to treat the preliminary purified oil phase after primary phase separation. Its main objective is to deeply remove tiny water droplets entrained in the oil phase. Therefore, fiber packing with smaller pore size, finer fibers, and hydrophilic water-capturing type is preferred to improve the ability to intercept, coalesce, and discharge trace water droplets.

[0115] refer to Figure 11 As shown, the first phase separation tank 5 is provided with first supports 50 at relative intervals, and the first fiber coalescing packing 51 is installed between the two first supports 50; the second phase separation tank 8 is provided with second supports 80 at relative intervals, and the second fiber coalescing packing is installed between the two second supports 80; the oil-water mixture after coalescing treatment in the first phase separation tank 5 enters the oil-water phase separation buffer tank 6, with the upper layer being the oil phase and the lower layer being the water phase, forming a stable oil-water interface 60 between the oil phase and the water phase, and the lower water phase entering the water phase storage tank 7; the upper oil phase enters the second phase separation tank 8, and the tiny water droplets entrained in the oil phase are intercepted and coalesced on the surface of the second fiber coalescing packing, and finally discharged through the water phase discharge port 82, while the finally purified oil phase is discharged through the oil phase discharge port 83 at the upper end of the second phase separation tank 8, and the purified oil phase product is collected.

[0116] In some embodiments, the aqueous phase storage tank 7 is further provided with a pH sensor 75 for monitoring the pH value of the aqueous phase in the aqueous phase storage tank;

[0117] It also includes: an aqueous phase replenishment tank 76 and an acid and alkali solution storage tank 77;

[0118] Among them, the aqueous phase replenishment tank 76 and the acid and alkali solution storage tank 77 are respectively connected to the aqueous phase storage tank.

[0119] In some embodiments, the aqueous phase storage tank 7 is also equipped with a liquid level sensor 74.

[0120] In the above embodiments, the aqueous phase storage tank 7 is also equipped with a pH sensor 75 and a liquid level sensor 74. The pH sensor 75 is used to monitor the pH value of the aqueous phase in the aqueous phase storage tank 7 and adjust the pH of the aqueous phase according to the monitored pH value. Specifically, the aqueous phase replenishment tank 76 stores the aqueous phase, and the acid and alkali solution storage tank 77 stores acid solutions (such as hydrochloric acid, sulfuric acid, nitric acid, phosphoric acid, formic acid, acetic acid, citric acid, oxalic acid, lactic acid, etc.) or alkali solutions (such as NaOH, KOH, ammonia, etc.). The pH value of the aqueous phase in the aqueous phase storage tank 7 is adjusted by adding the aqueous phase or by passing acid or alkali solutions. In this invention, the aqueous phase system is mainly based on acid extraction, and pH adjustment is mainly achieved by adding acid and replenishing with fresh aqueous phase. If the pH of the aqueous phase is lower than the target range, it can be adjusted by replenishing with fresh aqueous phase, reducing the amount of acid added, discharging some of the ion-rich aqueous phase, and / or adding a small amount of alkali solution. If the pH is higher than the target range, it is adjusted by adding acid. The alkaline solution is mainly used for pH feedback adjustment and does not change the preferred technical solution of using an acidic aqueous phase for ion impurity extraction. The liquid level sensor 74 is used to detect the liquid level of the aqueous phase in the aqueous phase storage tank 7. If the liquid level is too low, aqueous phase is added to the aqueous phase storage tank 7.

[0121] In some embodiments, it also includes:

[0122] Oil phase feed tank 9 is used to store oils and fats; oil phase feed tank 9 is connected to oil phase inlet port 21.

[0123] Purified oil phase storage tank 84, which is connected to oil phase discharge port 83;

[0124] An ion-rich aqueous phase storage tank 78 is connected to an aqueous phase storage tank 7.

[0125] In the above embodiment, the oil phase raw material tank 9 stores the oil to be processed. The oil to be processed enters the oil tank through the pipeline and the oil phase feed hole 21. The pipeline is equipped with a metering pump 91 to regulate the flow rate of the oil, and a valve can also be installed. In this invention, other pipelines are equipped with metering pumps to regulate the flow rate of the corresponding materials. The purified oil phase is discharged through the oil phase discharge port 83 at the upper end of the second phase separation tank 8 and collected in the purified oil phase storage tank 84. As the extraction continues, the aqueous phase in the aqueous phase storage tank 7 contains more and more impurity ions. Some of the aqueous phase containing impurity ions can be discharged to the ion-rich aqueous phase storage tank 78.

[0126] Based on the same inventive concept, the present invention also provides a method for the micro-dispersion extraction and removal of oil ion impurities, applied to the above-mentioned micro-dispersion extraction and removal device for oil ion impurities, comprising the following steps:

[0127] S1. The grease is fed into the oil phase distribution plate through the oil phase feed hole;

[0128] S2. The aqueous phase in the aqueous phase storage tank is introduced into the aqueous phase distribution plate through the first aqueous phase inlet hole;

[0129] S3. The aqueous phase in the aqueous phase storage tank is introduced into the first extraction tank through the second aqueous phase inlet / outlet port;

[0130] In this process, the oil is sheared into oil droplets by the aqueous phase in the oil-water shear tank and enters the droplet collection tank. The oil droplets in the droplet collection tank enter the second extraction tank and are extracted by the aqueous phase. At this time, the aqueous phase comes into contact with the oil droplets and performs countercurrent extraction.

[0131] The extracted oil-water mixture enters the first phase separation tank, and after being captured, coalesced, and demulsified by the first fiber coalescing packing, it enters the oil-water phase separation buffer tank. The lower aqueous phase enters the aqueous phase storage tank, and the upper oil phase enters the second phase separation tank. After being separated by the second fiber coalescing packing, the upper oil phase is discharged through the oil phase outlet to obtain the purified grease.

[0132] Specifically, the oil enters the oil tank through the oil phase inlet and eventually enters the oil-water shearing tank; the aqueous phase enters the water tank through the first aqueous phase inlet and eventually enters the oil-water shearing tank; in the oil-water shearing tank, the aqueous phase shears the oil into micro-sized oil droplets; the oil droplets enter the second extraction tank; simultaneously, the aqueous phase enters the first extraction tank through the second aqueous phase inlet and outlet and eventually flows into the second extraction tank; the oil droplets float upwards under buoyancy, while the aqueous phase extractant forms a co-current and counter-current flow relative to the upward direction of the oil droplets; by adjusting the direction of the aqueous phase flow and the apparent linear velocity... The apparent rise velocity and residence time of oil droplets are varied to control the oil-water contact time and the degree of migration of ionic impurities into the aqueous phase. The co-current mode is used to increase the apparent rise velocity of oil droplets, shorten the residence time, and reduce the risk of secondary emulsification, while the counter-current mode is used to decrease the apparent rise velocity of oil droplets, extend the residence time, and improve mass transfer. Simultaneously, the pH value of the aqueous phase in the storage tank is monitored using a pH sensor, with a preset pH range of 1.5–7.0, preferably 2.5–6.5. Based on the pH detection results, acid, alkali, and / or fresh aqueous phase extractant are added to adjust the pH of the aqueous phase. Maintaining within a preset range; the extracted oil-water mixture is introduced into the first phase separation tank, where it undergoes capture, collision, aggregation, growth, and demulsification on the surface of the first fiber coalescing packing. The aqueous phase preferentially aggregates on the surface of the hydrophilic and oleophobic fibers, while the oil phase preferentially wets and passes through the hydrophilic and oleophobic fiber regions, thereby promoting the capture, aggregation, and growth of dispersed droplets, forming an oil phase and an ion-rich aqueous phase that are easily separated by gravity. The oil-water mixture after coalescence treatment in the first phase separation tank enters the oil-water phase separation buffer tank, where it settles under gravity to form an ion-rich aqueous phase (lower layer). The process begins with a pre-purified oil phase (upper layer). This pre-purified oil phase then enters a second phase separation tank, where tiny water droplets entrained in the oil phase are trapped, coalesced, and discharged on the surface of the hydrophilic second fiber coalescing packing, resulting in an oil phase product with reduced ionic impurities and low water content. The ion-rich aqueous phase enters an aqueous phase storage tank, with a portion flowing back to the aqueous phase distribution plate, another portion flowing back to the first extraction tank, and the remaining portion being discharged to the ion-rich aqueous phase storage tank. Fresh aqueous phase extractant is added to the aqueous phase storage tank to maintain stable circulating aqueous phase volume, pH, and ion load.

[0133] In the above embodiments, the adjustment of the pH of the aqueous phase is used to suppress the formation of metal soaps, complexes, precipitates or colloids caused by local pH unevenness, and to reduce mass transfer resistance and oil phase loss caused by emulsion layers, deposits or interface films.

[0134] The oil to be processed in this invention is waste oil, specifically gutter oil, kitchen waste oil, swill oil, waste animal and vegetable oil, frying waste oil, acidified oil, oil refining byproducts, palm oil processing waste oil, or a mixture thereof; the ionic impurities in the oil include Na. + K + Ca 2+ Mg2+ Fe 2+ Fe 3+ Cu 2+ Zn 2+ Al 3+ Mn 2+ Ni 2+ Cr 3+ One or more metal ions, as well as chlorine-, phosphorus-, sulfur-containing ionic compounds, salts, metal soaps, ash precursors, or combinations thereof.

[0135] In some embodiments, the aqueous phase includes water, an acidic aqueous solution, or an aqueous solution containing a complexing agent;

[0136] The acid in the acidic aqueous solution is selected from one or more of hydrochloric acid, sulfuric acid, nitric acid, phosphoric acid, formic acid, acetic acid, citric acid, oxalic acid, and lactic acid, and the concentration of the acid is 0.001~2 mol / L, preferably 0.005~0.5 mol / L; the complexing agent in the aqueous solution is selected from one or more of citrate, acetate, EDTA (ethylenediaminetetraacetic acid), DTPA (diethylenetriaminepentaacetic acid), NTA (nitrotriacetic acid), aminocarboxylic acid compounds or their salts, and the concentration of the complexing agent in the aqueous solution is 0.0001~1 mol / L, preferably 0.001~0.2 mol / L.

[0137] A pH sensor is used to monitor the pH value of the aqueous phase in the aqueous phase storage tank. The pH of the aqueous phase in the aqueous phase storage tank is maintained at 1.5~7.0 by adding acid, alkali or aqueous phase to the aqueous phase storage tank.

[0138] It also includes a heating module, which is used to heat the oil and water phase in the first extraction tank and the second extraction tank to ensure the extraction temperature. Specifically, the extraction temperature is 20~95℃, preferably 35~75℃.

[0139] The flow rate of grease entering the oil phase distribution plate through the oil phase feed hole is 1~5000 mL / h, and the flow rate of aqueous phase entering the aqueous phase distribution plate through the first aqueous phase inlet hole is 0.1~5000 mL / h.

[0140] The flow rate of the aqueous phase entering the first extraction tank is 1~10000 mL / h.

[0141] In this invention, the aqueous phase shears the oil into oil droplets with a size of 1~2000 μm, preferably 10~500 μm.

[0142] Furthermore, such as Figure 12 As shown, the mass transfer process of ionic impurities in oil droplets was verified using a microchannel chip; this microchannel chip includes: an aqueous phase channel, an oil channel, and a shear channel, which can be referenced. Figure 9As shown (for ease of verification, an aqueous phase channel containing Fe is introduced), 3+ The oil contains impurities, and a channel through which water containing Rhodamine B (RhB) is introduced. Both oil and water enter a shear channel, where the oil shears the water into aqueous droplets. Rhodamine B exhibits a fluorescence response under excitation conditions of approximately 550 nm and emission conditions of approximately 580 nm. This fluorescence response is influenced by Fe... 3+ As the concentration increases, the fluorescence intensity undergoes a quenching change, which can be used to indicate Fe within microchannels. 3+ The process of migration from the oil-water interface to the aqueous phase; from Figure 12 It can be seen from this that the Fe in the oil 3+ Fe gradually migrates into the aqueous droplets, and the Fe in the aqueous droplets 3+ As the concentration increases, the fluorescence intensity decreases; the results indicate that the mass transfer process in the micro-dispersed channel can reach a stable plateau in the range of seconds to minutes; similarly, in this invention, the aqueous phase shears the oil into oil droplets, and impurity ions in the oil droplets can rapidly migrate into the aqueous phase.

[0143] The present invention relates to a micro-dispersion extraction and removal device and method for removing ionic impurities from oils and fats, comprising a micro-dispersion component including an aqueous phase distribution plate, an oil phase distribution plate, and a droplet generation plate. This component shears the oil into oil droplets, significantly shortening the mass transfer distance of ionic impurities from waste oils to the aqueous phase, thereby improving extraction efficiency and effectiveness. During the oil droplet flotation process, the present invention maintains a short-lifespan micro-dispersion state, ensuring a continuous spatial connection between the extraction process and the subsequent phase separation process, without relying on prolonged strong stirring. By adjusting the direction and velocity of the aqueous phase flow, the present invention controls the apparent flotation velocity and residence time of the oil droplets, allowing for adjustment of the oil-water contact time and mass transfer degree without changing the height of the micro-dispersion component and the second extraction tank, and providing operational control space for the ion removal process of different waste oil raw materials. The present invention employs functionally differentiated bi-stage fiber coalescing packing. The first fiber coalescing packing achieves rapid capture, coalescence, demulsification, and main phase separation of oil and water droplets after micro-dispersion extraction; the second fiber coalescing packing achieves deep interception, coalescence, and discharge of trace amounts of entrained water in the oil phase during preliminary purification. This dual-stage structure avoids prolonged stratification due to excessively small droplets after micro-dispersion extraction, and also reduces the risk of ion-rich aqueous phase entrainment into the oil phase product. The invention incorporates an aqueous phase replenishment tank, acid / alkali solution storage tanks, and a pH sensor. The pH, volume, and ion load of the circulating aqueous phase can be regulated through acid addition, fresh aqueous phase replenishment, and ion-rich aqueous phase discharge. This mitigates the formation of complexes, precipitates, or colloids caused by localized pH unevenness, reduces interfacial contamination and oil phase loss, and improves continuous operation stability. This invention is suitable for removing ion impurities from waste cooking oil, kitchen waste oil, swill oil, waste animal and vegetable oils, and their mixtures before preparing green jet fuel, biodiesel, or hydrogenation feedstock. It offers advantages such as compact equipment, low energy consumption, high degree of continuous operation, and flexible process control.

[0144] The following detailed embodiments further illustrate the micro-dispersion extraction and removal device and method for oil and fat ion impurities according to the present invention. This section further describes the content of the present invention in conjunction with specific embodiments, but should not be construed as limiting the present invention. Unless otherwise specified, the technical means used in the embodiments are conventional means well known to those skilled in the art. Unless otherwise specified, the reagents, methods, and equipment used in the present invention are conventional reagents, methods, and equipment in the art.

[0145] In the following embodiments, the water phase distribution plate is a square plate with a side length of 60 mm (i.e., both the length and width are 60 mm) and a thickness of 5 mm; the projection of the water tank on the plane is annular, wherein the diameter of the inner circle is 25 mm, the diameter of the outer circle is 35 mm, the width of the tank is 5 mm, and the depth of the tank is 1 mm; the diameter of the first water phase inlet hole is 0.5 mm.

[0146] The oil phase distribution plate is a square plate with a side length of 60 mm and a thickness of 5 mm. The projection of the oil groove on the plane is annular, with the inner circle having a diameter of 12 mm, the outer circle having a diameter of 22 mm, a groove width of 5 mm, and a groove depth of 1 mm. Sixteen first vertical channels are arranged at intervals along the outer circumference of the oil groove, each with a diameter of 0.5 mm and a height of 5 mm. The diameter of the oil phase feed hole is 0.5 mm.

[0147] The droplet generating plate has a side length of 60 mm and a thickness of 5 mm; the projection of the droplet collecting groove on the plane is a circle with a diameter of 6 mm and a depth of 1 mm; the oil-water shearing grooves (the same number as the first vertical channel, 16 in total) are arranged radially along the outer periphery of the droplet collecting groove, with a width of 0.5 mm, a depth of 1 mm, and a length of 15 mm; the second vertical channel (16 in total) and the third vertical channel (16 in total) are respectively connected to the oil-water shearing grooves, with an aperture of 0.5 mm and a height of 5 mm;

[0148] The cover plate is a square plate with a side length of 60 mm matching the droplet generating plate and a thickness of 3 mm. The projection of the droplet collecting hole on the plane is a circle with a diameter of 6 mm and a depth of 3 mm. An upper shear groove is provided on the lower end of the cover plate corresponding to the oil-water shear groove. The upper shear groove has a width of 0.5 mm, a depth of 1 mm, and a length of 15 mm.

[0149] In the following embodiments, the first fiber coalescing filler is a filler with an average pore size of 400 μm and an average porosity of 90% obtained by weaving polypropylene (PP) fibers, polyvinyl alcohol (PVA) fibers or cross-linked polyvinyl alcohol fibers.

[0150] The second fiber coalescing filler is a filler with an average pore size of 40 μm and an average porosity of 85%, obtained by weaving polyamide fibers.

[0151] Example 1

[0152] This embodiment provides a method for the micro-dispersion extraction and removal of ionic impurities in oils and fats, using Fe... 3+ Mg 2+ and Ca 2+ Waste oil is the target for treatment, and the above-mentioned oil ion impurity micro-dispersion extraction and removal device is used for treatment, specifically including the following steps:

[0153] S1. The grease is fed into the oil phase distribution plate through the oil phase feed hole;

[0154] S2. The aqueous phase in the aqueous phase storage tank is introduced into the aqueous phase distribution plate through the first aqueous phase inlet hole;

[0155] S3. The aqueous phase in the aqueous phase storage tank is introduced into the first extraction tank through the second aqueous phase inlet / outlet port;

[0156] In this process, the oil is sheared into oil droplets by the aqueous phase in the oil-water shear tank and enters the droplet collection tank. The oil droplets in the droplet collection tank enter the second extraction tank and are extracted by the aqueous phase. At this time, the aqueous phase comes into contact with the oil droplets and performs countercurrent extraction.

[0157] The extracted oil-water mixture enters the first phase separation tank, and after being captured, coalesced and demulsified by the first fiber coalescing packing, it enters the oil-water phase separation buffer tank. The lower aqueous phase enters the aqueous phase storage tank, and the upper oil phase enters the second phase separation tank. After being separated by the second fiber coalescing packing, the upper oil phase is discharged through the oil phase outlet to obtain the purified oil.

[0158] Among them, waste oil Fe before treatment 3+ Mg 2+ and Ca 2+ The initial concentrations were approximately 110 ppm, 102 ppm, and 108 ppm, respectively.

[0159] The aqueous phase is a citric acid-acetic acid buffer solution with a pH of 2.6 (wherein, the concentration of citric acid is 0.005 mol / L, the concentration of acetic acid is 0.002 mol / L, and the pH of the aqueous phase is adjusted to 2.6 by adjusting the amount of acetic acid added); the extraction temperature is 30℃; the flow rate of the oil phase entering the oil phase distribution plate through the oil phase inlet is 50 mL / h; the flow rate of the aqueous phase entering the aqueous phase distribution plate through the first aqueous phase inlet is 50 mL / h; the flow rate of the aqueous phase entering the first extraction tank is 60 mL / h; under the above conditions, the oil and aqueous phases enter the micro-dispersion component respectively, forming oil droplets with an average size of approximately 180 μm in the oil-water shear tank.

[0160] Comparative Example 1

[0161] This comparative example provides a method for removing oil ions, including the following steps:

[0162] S1. In a glass reactor, add 50 mL of Fe... 3+ Mg 2+ and Ca 2+ Waste oil (Fe 3+ Mg 2+ and Ca 2+ The initial concentrations were approximately 110 ppm, 102 ppm, and 108 ppm, respectively. 50 mL of a citric acid-acetic acid buffer solution with pH=2.6 (wherein the concentration of citric acid was 0.005 mol / L, the concentration of acetic acid was 0.002 mol / L, and the pH of the aqueous phase was adjusted to 2.6 by adjusting the amount of acetic acid added) was used for extraction at 30°C with a 25 mm diameter polytetrafluoroethylene magnetic stir bar at 800 rpm.

[0163] The oil was extracted according to the methods in Example 1 and Comparative Example 1 to obtain Fe. 3+ Extraction efficiency curve as shown Figure 13 As shown. Figure 13 The extraction efficiency (%) is calculated as follows: (Fe in the oil before extraction) 3+ Content - Fe in the extracted oil 3+ Content) / Fe in the oil before extraction 3+ Content × 100%.

[0164] The Mg in Example 1 and Comparative Example 1 was obtained using the same method described above. 2+ Ca 2+ The extraction efficiency curve was further fitted using an apparent first-order kinetic model to obtain the apparent mass transfer rate constant, as shown in the figure. Figure 14 As shown.

[0165] from Figures 13-14 As can be seen from this, the method of the present invention Fe 3+ Mg 2+ and Ca 2+ The apparent mass transfer rate constants are approximately 1.55 min. -1 1.13 min -1 and 1.21 min -1 In contrast, the apparent mass transfer rate constant in the conventional stirred extraction system of Comparative Example 1 was approximately 0.09 min. -1 0.09 min -1 and 0.08 min -1This indicates that the micro-dispersive extraction method used in this invention improves efficiency by approximately 12.6 to 17.2 times compared to conventional stirred extraction systems, demonstrating that this invention can significantly enhance ion cross-interface migration within a short residence time.

[0166] Following the method in Example 1, the content of each ion in the oil before and after extraction was tested as follows: Figure 15 As shown. Figure 15 As shown, before treatment, Fe in the oil phase 3+ Mg 2+ and Ca 2+ The contents were approximately 110, 102, and 108 ppm, respectively; after treatment, the Fe content in the oil phase was... 3+ Mg 2+ and Ca 2+ The contents were reduced to approximately 2, 6, and 7 ppm, respectively, corresponding to removal rates of approximately 98.2%, 94.1%, and 93.5%. These results demonstrate that this invention can simultaneously reduce the content of multiple metal ion impurities in waste oil systems, making it suitable for pretreatment of waste oil before it enters green jet fuel, biodiesel, or hydrodeoxygenation processes.

[0167] Further following the method in Example 1, the water content of the oil phase before entering the second phase separation tank was tested (i.e., Figure 16 The water content before dehydration in the middle stage, and the water content after the second phase separation tank (i.e., the water content before dehydration in the middle stage), and the water content after the second phase separation tank. Figure 16 After dehydration, the results are as follows Figure 16 As shown.

[0168] from Figure 16 The results show that the water content of the initially purified oil phase before entering the second phase separation tank was approximately 574.3 ppm. After dehydration by the second fiber coalescing packing, the water content of the oil phase was reduced to approximately 91.0 ppm, a reduction of approximately 84.2%. This result indicates that the second fiber coalescing packing can effectively remove trace amounts of water phase entrained in the initially purified oil phase, thereby reducing the risk of ion-rich aqueous phases, acidic components, or complexing agents entering subsequent hydrogenation or storage and transportation stages along with the oil phase.

[0169] Furthermore, following the method in Example 1, the pH of the aqueous phase was adjusted to 3.6 and 5.8. The results showed that the extraction efficiency was highest at pH=2.6, followed by pH=3.6, and the extraction efficiency was significantly reduced at pH=5.8. This indicates that an acidic aqueous phase is conducive to promoting the migration of metal ions or metal soap impurities into the aqueous phase.

[0170] It is understood that the technical features of the above embodiments can be combined arbitrarily. For the sake of brevity, not all possible combinations of the technical features in the above embodiments are described. However, as long as there is no contradiction in the combination of these technical features, they should be considered to be within the scope of this specification.

[0171] The above are merely preferred embodiments of this application, and only specifically describe the technical principles of this application. These descriptions are only for explaining the principles of this application and should not be construed as limiting the scope of protection of this application in any way. Based on this explanation, any modifications, equivalent substitutions, and improvements made within the spirit and principles of this application, as well as other specific embodiments of this application that can be conceived by those skilled in the art without creative effort, should be included within the scope of protection of this application.

Claims

1. A device for micro-dispersion extraction and removal of oil ionic impurities, characterized in that, include: Micro-dispersed components, comprising: A water phase distribution plate has a water tank on its upper surface and a first water phase inlet hole on its side, which is connected to the water tank. An oil phase distribution plate has its lower end face abutting against the upper end face of the water phase distribution plate. An oil groove is formed on the upper end face of the oil phase distribution plate. An oil phase feed hole is provided on the side of the oil phase distribution plate, and the oil phase feed hole is connected to the oil groove. A plurality of first vertical channels are formed on the oil phase distribution plate around the outer periphery of the oil groove, and the first vertical channels are connected to the water groove. A droplet generating plate has its lower end face abutting against the upper end face of an oil phase distribution plate. A droplet collecting groove is formed on the upper end face of the droplet generating plate. Multiple oil-water shear grooves are formed on the droplet generating plate outside the droplet collecting groove, and these oil-water shear grooves are connected to the droplet collecting groove. A second vertical channel is formed inside the droplet generating plate corresponding to a first vertical channel, with its upper end connected to the oil-water shear groove and its lower end connected to the first vertical channel. Multiple third vertical channels are formed inside the droplet generating plate corresponding to an oil groove, with their upper ends connected to the oil-water shear groove and their lower ends connected to the oil groove. The third vertical channels are located inside the second vertical channels. Extraction and separation components, comprising: First extraction tank; The second extraction vessel is coaxially disposed inside the first extraction vessel; The lower end face of the second extraction vessel abuts against the lower end face of the first extraction vessel, and the upper end extends out of the first extraction vessel; the upper end face of the droplet generating plate abuts against the lower end face of the first extraction vessel; the droplet collecting groove communicates with the interior of the second extraction vessel; The first extraction tank has a second aqueous phase inlet / outlet hole on one side. The second extraction tank has a first aqueous phase inlet / outlet pipe and a second aqueous phase inlet / outlet pipe respectively on the side of the second extraction tank and inside the first extraction tank along the vertical direction. The second aqueous phase inlet / outlet pipe extends out of the first extraction tank.

2. The oil and fat ion impurity micro-dispersion extraction and removal device as described in claim 1, characterized in that, Also includes: A primary fiber coalescing phase separation assembly, comprising: The first phase separation tank is provided with a first fiber coalescing packing material, which is made of oleophilic and hydrophobic fibers and hydrophilic and oleophobic fibers through weaving; the upper end of the second extraction tank extends out of the first extraction tank and is connected to one end of the first phase separation tank. An oil-water phase separation buffer tank, one side of which is connected to the other end of the first phase separation tank; Aqueous phase storage tank, the upper end of which is connected to the lower end of the oil-water phase buffer tank; The aqueous phase storage tank is equipped with a first aqueous phase pipe, a second aqueous phase pipe, and a third aqueous phase pipe. One end of the first aqueous phase pipe is connected to the aqueous phase storage tank, and the other end is connected to the first aqueous phase inlet. One end of the second water phase pipeline is connected to the water phase storage tank, and the other end is connected to the second water phase inlet / outlet. One end of the third water phase pipeline is connected to the water phase storage tank, and the other end is connected to the second water phase inlet / outlet pipe.

3. The micro-dispersion extraction and removal device for oil and fat ion impurities as described in claim 2, characterized in that, Also includes: A secondary fiber coalescing dewatering assembly, comprising: The second phase separation tank is equipped with a second fiber coalescing packing material, which is made of hydrophilic fibers through weaving. One end of the second phase separation tank is connected to the upper end of the oil-water phase separation buffer tank; The second phase separation tank is provided with a water phase outlet at the lower end and an oil phase outlet at the upper end.

4. The micro-dispersion extraction and removal device for oil and fat ion impurities as described in claim 2, characterized in that, The aqueous phase storage tank is also equipped with a pH sensor to monitor the pH value of the aqueous phase in the tank. It also includes: aqueous phase replenishment tank and acid / alkali solution storage tank; The aqueous phase replenishment tank and the acid / alkali solution storage tank are respectively connected to the aqueous phase storage tank.

5. The micro-dispersion extraction and removal device for oil and fat ion impurities as described in claim 2, characterized in that, The aqueous storage tank is also equipped with a liquid level sensor.

6. The micro-dispersion extraction and removal device for oil and fat ion impurities as described in claim 3, characterized in that, The width of the oil-water shear groove is 0.05~5 mm; The apertures of the first, second, and third vertical channels are 0.05~3 mm; The oleophilic and hydrophobic fibers and the hydrophilic and oleophilic fibers are woven together to obtain a first fiber coalescing filler with a pore size of 50~1500 μm; The hydrophilic fibers are woven to obtain a second fiber coalescing filler with a pore size of 1~500 μm.

7. The micro-dispersion extraction and removal device for oil and fat ion impurities as described in claim 3, characterized in that, Also includes: An oil phase feed tank is used to store oils; the oil phase feed tank is connected to an oil phase inlet. A purified oil phase storage tank, which is connected to the oil phase discharge port; An ion-rich aqueous phase storage tank, which is connected to the aqueous phase storage tank.

8. A method for micro-dispersed extraction and removal of oil ion impurities, applied to the micro-dispersed extraction and removal apparatus for oil ion impurities as described in any one of claims 1 to 7, characterized in that, Includes the following steps: The grease is fed into the oil phase distribution plate through the oil phase feed hole; The aqueous phase in the aqueous phase storage tank is introduced into the aqueous phase distribution plate through the first aqueous phase inlet hole; The aqueous phase in the aqueous phase storage tank enters the first extraction tank through the second aqueous phase inlet / outlet port; In this process, the oil is sheared into oil droplets by the aqueous phase in the oil-water shear tank and then enters the droplet collection tank. The oil droplets in the droplet collection tank then enter the second extraction tank and are extracted by the aqueous phase. The extracted oil-water mixture enters the first phase separation tank, and after being captured, coalesced, and demulsified by the first fiber coalescing packing, it enters the oil-water phase separation buffer tank. The lower aqueous phase enters the aqueous phase storage tank, and the upper oil phase enters the second phase separation tank. After being separated by the second fiber coalescing packing, the upper oil phase is discharged through the oil phase outlet to obtain the purified grease.

9. The method for micro-dispersed extraction and removal of oil ionic impurities as described in claim 8, characterized in that, The aqueous phase includes water, acidic aqueous solution, and aqueous solution containing a complexing agent; The acid in the acidic aqueous solution is selected from one or more of hydrochloric acid, sulfuric acid, nitric acid, phosphoric acid, formic acid, acetic acid, citric acid, oxalic acid, and lactic acid. The complexing agent in the aqueous solution is selected from one or more of citrate, acetate, EDTA, DTPA, NTA, aminocarboxylic acid compounds or their salts, and the concentration of the complexing agent in the aqueous solution is 0.0001~1 mol / L; A pH sensor is used to monitor the pH value of the aqueous phase in the aqueous phase storage tank. The pH of the aqueous phase in the aqueous phase storage tank is maintained at 1.5~7.0 by adding aqueous phase, acid or alkali solution to the aqueous phase storage tank.

10. The method for micro-dispersed extraction and removal of oil ionic impurities as described in claim 8, characterized in that, The extraction temperature is 20~95℃; The flow rate of grease entering the oil phase distribution plate through the oil phase feed hole is 1~5000 mL / h, and the flow rate of aqueous phase entering the aqueous phase distribution plate through the first aqueous phase inlet hole is 0.1~5000 mL / h. The flow rate of the aqueous phase entering the first extraction tank is 1~10000 mL / h.

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