Extraction and oil removal integrated equipment and oil-free cerous carbonate preparation process

Abstract

The invention relates to the technical field of rare earth compound oil removal, and discloses extraction and oil removal integrated equipment and an oil-free cerous carbonate preparation process, the extraction and oil removal integrated equipment comprises a fine filter, a water inlet of the fine filter is used for being in butt joint with an extraction system, a water outlet of the fine filter is connected with a second pipeline through a first pipeline, and the second pipeline is provided with at least two flow dividing connectors; a third pipeline is connected to the flow dividing connector and used for being connected with an activated carbon adsorption column, the activated carbon adsorption column is connected with a resin adsorption column through a fourth pipeline, the resin adsorption column is connected with a composite fiber adsorption device through a fifth pipeline, and a water outlet of the composite fiber adsorption device is connected with a sixth pipeline. The sixth pipeline is provided with a pipeline oil content detector, the side wall of the sixth pipeline is connected with a seventh pipeline, and the free end of the seventh pipeline is connected with a reflux inlet of the fine filter; multi-stage adsorption oil removal is achieved, unqualified feed liquid can be subjected to backflow treatment, it is guaranteed that the discharged oil content reaches the standard, the treatment efficiency and stability are improved, and the maintenance cost is reduced.

Description

Technical Field

[0001] This invention relates to the field of rare earth compound degreasing technology, and particularly to an integrated extraction degreasing device and an oil-free cerium carbonate preparation process. Background Technology

[0002] Cerium carbonate is an important rare earth functional material with wide applications in high-end catalysis, optical glass, laser crystals, and pharmaceutical intermediates. These applications require cerium carbonate to have ultra-high purity (typically ≥99.9995%, i.e., 5N5), extremely low content of rare earth and non-rare earth impurities (and oil residue ≤0.5ppm), and good activity.

[0003] Currently, traditional preparation processes face key technical bottlenecks: severe organic phase residue: organic extractants (such as P507) used in the extraction process are prone to remain in the aqueous phase, and traditional single filtration oil removal methods are inefficient, resulting in excessive oil content in the product and affecting subsequent application performance. Summary of the Invention

[0004] The purpose of this invention is to provide an integrated extraction and oil removal device and an oil-free cerium carbonate preparation process, which solves the problem of low efficiency and excessive oil content in the product caused by the traditional single filtration and oil removal method mentioned in the background art.

[0005] The technical solution adopted in this invention is as follows: An integrated oil extraction and removal device includes a fine filter, an activated carbon adsorption column, a resin adsorption column, and a composite fiber adsorption device. The inlet of the fine filter is used to connect to the extraction system. The outlet of the fine filter is connected to a second pipe through a first pipe. The second pipe has at least two diversion interfaces, and a third pipe is connected to each diversion interface. The third pipe is used to connect to the activated carbon adsorption column. The activated carbon adsorption column is connected to the resin adsorption column through a fourth pipe. The resin adsorption column is connected to the composite fiber adsorption device through a fifth pipe. The outlet of the composite fiber adsorption device is connected to a sixth pipe. An oil content detector is installed on the sixth pipe. A seventh pipe is connected to the side wall of the sixth pipe, and the free end of the seventh pipe is connected to the return port of the fine filter. A first valve is connected to the outlet of the third pipe, a second valve is connected to the inlet and outlet of the fourth pipe, a third valve is connected to the inlet and outlet of the fifth pipe, a fourth valve is connected to the sixth pipe, and a fifth valve is connected to the seventh pipe.

[0006] The inner side of the thrust plate has a first concave cavity, and the lower end face of the thrust plate has a water inlet hole and a water outlet hole, with the water outlet hole communicating with the first concave cavity; the side of the thrust plate has connecting ears for installing a first support rod and a second support rod.

[0007] The inner side of the pressing plate has a second concave cavity, and the end face of the pressing plate has a water outlet cavity; the water outlet cavity communicates with the second concave cavity; the side of the pressing plate has a first bracket that overlaps with the first support rod.

[0008] The filter frame has a third cavity on both end faces, and a through groove through the third cavity on the filter frame. The filter frame has an inlet hole and an outlet hole on the lower end face, and the inlet hole is connected to the through groove. The side of the filter frame has a second bracket that overlaps with the first support rod.

[0009] The filter plate has a fourth cavity on both end faces, and the fourth cavity has a matrix of protrusions that are flush with the end faces of the filter plate; the lower end face of the filter plate has an inlet hole and an outlet hole, and the outlet hole communicates with the fourth cavity; the side of the filter plate has a second bracket that overlaps with the first support rod.

[0010] The filter paper has an inlet hole and an outlet hole on its lower end face. The lower side of the filter paper is flush with the filter frame and filter plate, and the top edge of the filter paper protrudes outside the filter frame and filter plate.

[0011] The inner wall of the second tank is connected to symmetrically arranged second mesh plates, and the gaps between the second mesh plates are filled with turbulence balls, the surface of which has several through holes.

[0012] The second top cover is equipped with a first telescopic rod. The piston end of the first telescopic rod extends into the second tank and passes through the second mesh plate. The lower end of the first telescopic rod is connected to a ring, and a cross rod is connected to the ring.

[0013] The lower side wall of the second tank is connected to a third branch pipe, and the upper side wall of the second tank is connected to a fourth branch pipe. The third and fourth branch pipes are connected to a second tee pipe. The two ends of the second tee pipe are connected to a second housing. A drive gear is rotatably connected inside the second housing. The drive gear is driven by a second motor. A chain meshes on the drive gear. First scrapers are installed on the chain at intervals. The opposite ports of the second housing are connected through a ninth pipe to form a circulating stirring channel for activated carbon particles or resin particles.

[0014] The inner wall of the first tank is connected to a first carrier plate, which is located above the filter assembly. A first shaft tube is rotatably connected to the first carrier plate. A first stirring blade is connected to the lower side wall of the first shaft tube. A first bevel gear is connected to the upper end of the first shaft tube. A second bevel gear meshes with the first bevel gear. The second bevel gear is driven by a third motor. The second bevel gear is mounted on a support frame, which is connected to the first carrier plate. A third bevel gear is rotatably connected to the support frame, which meshes with the second bevel gear. A shaft is connected to the third bevel gear, which has a clearance fit with the first shaft tube. A second stirring blade is connected to the lower end of the shaft.

[0015] A third bottom cover is connected to the lower end of the first tank. A rotating rod is rotatably connected to the third bottom cover. A second partition is installed inside the first tank. The top surface of the second partition has four second through holes arranged at equal angles. A third tube seat is rotatably connected to the second through holes. A first filter cartridge seat is connected to the third tube seat. A first filter tube is connected to the first filter cartridge seat. The upper end of the first filter tube is connected to a second filter cartridge seat. A fourth tube seat is connected to the top surface of the second filter cartridge seat. An end cap is connected to the fourth tube seat. Filter cloth is installed on the outer wall of the first filter tube. The third tube seat and the fourth... The tube base is connected to a positioning bolt, which is connected to a rotating rod. It also includes a frame mounted on a first base, on which a first rotating shaft is rotatably connected. The first rotating shaft is connected to a fourth motor via a belt drive. A second rotating shaft is provided at the upper end of the first rotating shaft, and the second rotating shaft is rotatably connected to the frame. A first eccentric shaft is connected to the upper end of the second rotating shaft, and a cross-shaped frame is rotatably connected to the first eccentric shaft. The four branches of the cross-shaped frame are rotatably connected to the second eccentric shafts. The four second eccentric shafts rotate synchronously, and the rotating rod is rotatably connected to the second eccentric shaft.

[0016] The inner wall of the first tank is connected to a second carrier plate, which is located above the filter assembly. A third housing is connected to the second carrier plate. A worm gear is rotatably connected inside the third housing. The worm gear meshes with a worm wheel driven by a fifth motor. A splined shaft is slidably connected to the worm wheel. A bracket is connected to the lower end of the splined shaft. A ring seat is connected to the bracket. Ear seats arranged at equal angles are connected to the side wall of the ring seat. A push rod is slidably connected to the ear seats. A return spring is connected to the push rod. The end face of the push rod has bristles. A second bearing seat is connected to the third housing. Two symmetrically arranged third bearing seats are connected to the second bearing seat. A guide rail is installed on the third bearing seat. A slide is slidably connected to the guide rail. A movable stage is installed on the slide. A first bearing seat rotatably connected to the tail end of the splined shaft is connected to the movable stage. A ball bearing slide is installed on the movable stage. A fourth bearing seat with a second lead screw is installed on the second bearing seat. The second lead screw is adapted to the ball bearing slide and is driven by a sixth motor.

[0017] The cleaning component includes a first base plate mounted on a slide tube, with symmetrically arranged second scrapers hinged to both ends of the first base plate, and second springs installed between the opposing second scrapers.

[0018] A fourth carrier plate is installed inside the first tank. A main shaft is rotatably connected to the fourth carrier plate and driven by an eighth motor. A third filter cartridge seat is symmetrically arranged and slidably connected to the side wall of the main shaft. A second filter tube is installed between the gaps in the third filter cartridge seats, and a filter cloth is installed on the outer wall of the second filter tube. A fourth spring is connected to the upper and lower ends of the third filter cartridge seat. A limit ring is connected to the free end of the fourth spring. A limit block is connected to the side wall of the main shaft by fastening bolts. An air bladder is fixed to the main shaft inside the second filter tube by a pipe clamp. The center of the main shaft has an airflow channel. A third partition plate is connected inside the first tank. A fifth pipe seat is rotatably connected to the third partition plate and connected to the lower end of the main shaft. A liquid channel is opened on the main shaft inside the second filter tube, and the liquid channel penetrates the bottom surface of the main shaft.

[0019] A cylindrical cam is connected to the side wall of the main shaft, and a ball head rod is slidably connected to the cylindrical cam. Guide rods arranged at equal angles are connected to the fourth carrier plate, and a sliding column is slidably connected to the guide rod. The side wall of the sliding column is connected to the ball head rod, and a pressure head is connected to the bottom surface of the sliding column. A ball is rotatably connected to the pressure head.

[0020] Furthermore, a process for preparing oil-free cerium carbonate using the aforementioned integrated extraction and oil removal equipment is proposed, comprising the following steps: Step 1. Raw material pretreatment: Prepare a solution of mixed rare earth chloride raw materials (mainly containing La, Ce, Pr and Nd) with a concentration of 250-350 g / L. Remove suspended solids by passing the solution through a 0.5 μm precision filter and adjust the pH of the solution to 1.5-2.5 by adding hydrochloric acid.

[0021] Step 2. Multi-stage extraction: The pretreated solution is pumped into a 180-stage series extraction tank for multi-stage separation and extraction, with a focus on enhancing the separation of La / Ce / Pr / Nd to obtain a high-purity cerium chloride solution; Step 3. Multi-stage combined degreasing: The high-purity cerium chloride solution obtained in Step 2 is sequentially passed through the following units for degreasing treatment: a. Pre-filtration unit: Employs a 0.5μm precision filter; b. Adsorption unit: consisting of an activated carbon adsorption column and a dedicated macroporous polymer resin adsorption column; c. Deep filtration unit: Employs a composite fiber oil absorption device; d. Online monitoring and feedback unit: Real-time monitoring of oil and impurity content; unqualified liquid is automatically returned to the corresponding adsorption unit for reprocessing to ensure that the oil content at the outlet is ≤0.5ppm.

[0022] Step 4. Preparation of low-impurity precipitant: In a closed reactor, high-purity carbon dioxide gas with a purity ≥99.99% is reacted with electronic-grade ammonia water under controlled temperature (15-25℃) and staged pressure increase (0.2→0.5MPa) conditions to obtain an ammonium carbonate precipitant solution with a non-rare earth impurity content ≤0.5PPm.

[0023] Step 5. Precise Precipitation: Transfer the high-purity cerium chloride solution obtained from the oil removal in Step 3 into the precipitation reactor, and perform precipitation in two stages: Initial stage: temperature 40-50℃, pH = 5.5-6.0; Later stage: temperature 55-65℃, pH = 6.5-7.0; at a flow rate of 0.1-1.2 m... 3 The precipitant prepared in step 4 is added at a rate of / h, and the reaction produces high-purity cerium carbonate precipitate.

[0024] Step 6. Washing and dehydration: The precipitated product is fed into a high-speed centrifuge to achieve solid-liquid separation of cerium carbonate and ammonium chloride. Then, it is washed at least 4 times with high-purity hot water with a conductivity ≤0.5μS / cm, followed by high-speed centrifugation and dehydration to obtain a high-purity, low-impurity, oil-free cerium carbonate product with a total rare earth content greater than 46%.

[0025] The beneficial effects of this invention are as follows: This integrated oil extraction and removal equipment achieves efficient and deep removal of oil from the feed liquid through a multi-stage purification structure consisting of a fine filter, activated carbon adsorption column, resin adsorption column, and composite fiber adsorption device. The filter components of the fine filter adopt an equally angled filter tube structure, which increases the filtration area and improves the purification effect of the feed liquid. Its matching feed liquid circulation stirring and bidirectional reverse stirring structure makes the feed liquid distribution more uniform. The self-cleaning structure, such as filter tube rotation, automatic brush cleaning, air bladder expansion for impurity removal, and scraper slag removal, effectively avoids filter cloth clogging and slag accumulation on the partition, ensuring the continuous and stable filtration efficiency of the fine filter. The activated carbon adsorption column and resin adsorption column extend the contact time between the feed liquid and the adsorption particles through a turbulence ball, a liftable cross bar, and an adsorption particle circulation stirring structure, achieving full and uniform contact between the two, while effectively preventing the adsorption particles from clumping and depositing. The adsorption and oil removal effect is significantly improved. The filter bed of the composite fiber adsorption device adopts a structure in which filter paper, filter frame, and filter plate are arranged in sequence, and a screw-driven clamping plate is used to achieve firm positioning. The filter paper, filter frame, and filter plate fit tightly to reduce the risk of leakage, which not only improves the oil retention effect but also facilitates the disassembly and replacement of filter media. The equipment is equipped with a pipeline oil separation detector and a matching return pipeline at the discharge end, which can realize the return of unqualified liquid after oil separation detection for secondary treatment, ensuring that the oil separation index of the final discharge meets the standard. The valves configured for each pipeline can flexibly realize on / off and diversion control, which facilitates the operation, maintenance, and repair of the equipment. The overall equipment structure is reasonably designed and the components have a high degree of coordination and strong operational stability, effectively improving the overall processing efficiency and oil removal effect of the liquid. At the same time, various automatic cleaning and convenient disassembly and assembly structures reduce the manual maintenance cost and operation difficulty.

[0026] Compared with existing technologies, the significant advantages of the preparation process of this invention are as follows: Firstly, it achieves complete removal of oil by pioneering a three-stage combined oil removal system of "filtration-resin adsorption-fine filtration", which stably controls the residual oil at ≤0.5ppm, solving the industry-wide problem of organic phase residue affecting product quality. Moreover, the three-stage process is compact and can be adapted to industrial continuous production scenarios. Secondly, it can control impurities from the source by independently preparing a low-impurity precipitant with non-rare earth impurities ≤0.5ppm, thus eliminating the introduction of external impurities from the source. Attached Figure Description

[0027] Figure 1 This is a schematic diagram of the main view structure of this application.

[0028] Figure 2 This is a top view of the structure of this application.

[0029] Figure 3 This is a schematic diagram of the main cross-sectional structure of the fine filter tank.

[0030] Figure 4 This is a schematic diagram of the front cross-sectional structure of the filter assembly.

[0031] Figure 5 This is a schematic diagram of the front cross-sectional structure of an activated carbon adsorption column.

[0032] Figure 6 This is a schematic diagram of the front cross-sectional structure of a ball locating pin.

[0033] Figure 7 This is a schematic diagram of the main structure of the push plate.

[0034] Figure 8 This is a three-dimensional structural diagram of the push plate.

[0035] Figure 9 This is a schematic diagram of the three-dimensional structure of the clamping plate.

[0036] Figure 10 This is a schematic diagram of the three-dimensional structure of the filter frame.

[0037] Figure 11 This is a schematic diagram of the three-dimensional structure of the filter plate.

[0038] Figure 12 This is a schematic diagram of the three-dimensional structure of filter paper.

[0039] Figure 13 This is a schematic diagram of the three-dimensional structure of the pump body.

[0040] Figure 14 This is a top view cross-sectional structural diagram of the pump body.

[0041] Figure 15 This is a schematic diagram of the front cross-sectional structure of the turbulence sphere.

[0042] Figure 16 This is a three-dimensional structural diagram of the first telescopic rod.

[0043] Figure 17 This is a schematic diagram of the front view cross-section of the ring.

[0044] Figure 18 This is a three-dimensional structural diagram of the second casing.

[0045] Figure 19 This is a schematic diagram of the main cross-sectional structure of the chain.

[0046] Figure 20 This is a schematic diagram of the main cross-sectional structure of the first scraper.

[0047] Figure 21 This is a schematic diagram of the main cross-sectional structure of the first stirring blade.

[0048] Figure 22 This is a schematic diagram of the main structure of the third bottom cover.

[0049] Figure 23 This is a schematic diagram of the main cross-sectional structure of the rotating rod.

[0050] Figure 24 This is a three-dimensional structural diagram of the second rotating shaft.

[0051] Figure 25 This is a schematic diagram of the front cross-sectional structure of the spline shaft.

[0052] Figure 26 This is a schematic diagram of the front cross-sectional structure of the top rod.

[0053] Figure 27 This is a schematic diagram of the three-dimensional structure of the guide rail.

[0054] Figure 28 This is a schematic diagram of the front sectional view of the vertical rod.

[0055] Figure 29 This is a schematic diagram of the three-dimensional structure of the indexing roller.

[0056] Figure 30 This is a schematic diagram of the front cross-sectional structure of the sliding tube.

[0057] Figure 31 This is a schematic diagram of the three-dimensional structure of the second scraper.

[0058] Figure 32 This is a schematic diagram of the three-dimensional structure of the third scraper.

[0059] Figure 33 This is a schematic diagram of the main sectional view of the slag storage tank.

[0060] Figure 34 This is a three-dimensional structural diagram of the slag storage tank.

[0061] Figure 35 This is a schematic diagram of the main axis in front view section.

[0062] Figure 36 This is a schematic diagram of the front cross-sectional structure of the airbag.

[0063] Figure 37 This is a schematic diagram of the front cross-sectional structure of a cylindrical cam.

[0064] Figure 38 This is a schematic diagram of the front cross-sectional structure of the sliding column.

[0065] In the diagram: 1. Fine filter; 2. Activated carbon adsorption column; 3. Resin adsorption column; 4. Composite fiber adsorption device; 6. First pipeline; 7. Second pipeline; 8. Diversion interface; 9. Third pipeline; 11. Fourth pipeline; 12. Fifth pipeline; 13. Sixth pipeline; 14. Pipeline oil separator; 15. Seventh pipeline; 17. First valve; 18. Second valve; 19. Third valve; 20. Fourth valve; 21. Fifth valve; 22. First base; 23. First support leg; 24. First tank; 25. First inlet pipe; 26. First outlet pipe; 27. Filter assembly; 28. First bottom cover; 29. ​​Drain pipe; 30. Lifting eye bolt; 31. First top cover; 32. Lead screw; 33. Rocker arm; 34. First bearing seat; 35. First partition plate; 36. First through hole; 37. First pipe seat; 38. First filter cartridge seat; 39. First filter tube; 40. Second filter cartridge seat; 41. End cap; 42. Filter cloth; 43. Second base; 44. Second foot seat; 45. Second tank body; 46. Second top cover; 47. Second inlet pipe; 48. Second bottom cover; 49. Second outlet pipe; 50. First filter cotton; 51. Ball bearing positioning pin; 52. First mesh plate; 53. Activated carbon granules; 54. Resin granules; 55. Third base; 56. Chassis; 57. Third inlet pipe; 58. Third outlet pipe; 59. Thrust plate; 60. Support seat; 61. Inlet hole; 62. Outlet hole; 63. First connecting seat; 64. Second connecting seat; 65. First support rod; 66. Second support rod; 67. Filter frame; 68. Filter plate; 69. Filter paper; 71. Pressing plate; 72. First lead screw; 73. Threaded seat; 74. Handwheel; 75. First cavity; 76. Connecting ear; 77. Second cavity; 78. Water outlet cavity; 79. First hanger; 80. Third cavity; 81. Through groove; 82. Second hanger; 83. Fourth cavity; 84. Protrusion; 85. First branch pipe; 86. Second branch pipe; 87. First tee pipe; 88. Second pipe seat; 89. Pump body; 90. First housing; 91. Right angle seat; 92. Rubber hose; 93. Triangular seat; 94. Pressure roller; 95. First motor; 96. Eighth pipe; 98. Second screen plate; 99. Turbulence ball; 100. Through hole; 101. First telescopic... 103. Rod; 104. Ring; 105. Cross rod; 106. Third branch pipe; 107. Fourth branch pipe; 108. Second tee pipe; 109. Second housing; 100. Drive gear; 111. Second motor; 112. Chain; 113. First scraper; 114. Ninth pipe; 115. First carrier plate; 116. First shaft tube; 117. First stirring blade; 118. First bevel gear; 119. Second bevel gear; 120. Third motor; 121. Support frame; 122. Third bevel gear; 123. Shaft; 124. Second stirring blade; 125. Third bottom cover; 126. Rotating rod; 127. Second partition plate; 128. Second through hole; 129. Third pipe seat; 130. Fourth pipe seat; 131. Positioning bolt;132. Frame; 133. First rotating shaft; 134. Belt drive; 135. Fourth motor; 136. Second rotating shaft; 137. First eccentric shaft; 138. Cross-shaped frame; 139. Second eccentric shaft; 140. Second carrier plate; 141. Third housing; 142. Worm gear; 143. Worm wheel; 144. Fifth motor; 145. Splined shaft; 146. Support; 147. Ring seat; 148. Ear seat; 149. Push rod; 50. Return spring; 151. Brush bristles; 152. Second bearing seat; 153. Third bearing seat; 154. Guide rail; 155. Slide; 156. Moving table; 157. First bearing seat; 158. Ball bearing slide; 159. Fourth bearing seat; 160. Second lead screw; 161. Sixth motor; 162. Third carrier plate; 163. Indexing roller; 164. Arc cam; 165. Second bearing seat; 166. Seventh motor 167. Vertical rod; 168. First spring; 169. Slide tube; 170. Cleaning component; 171. First base plate; 172. Second scraper; 173. Second spring; 174. Second base plate; 175. Third scraper; 176. Third spring; 177. Slag storage tank; 178. Slag inlet pipe; 179. Baffle; 180. Return pipe; 181. Discharge plug; 182. Fourth carrier plate; 183. Main shaft; 184. Eighth electric... Machine; 185. Third filter cartridge holder; 186. Second filter tube; 187. Fourth spring; 188. Limiting ring; 189. Fastening bolt; 190. Limiting block; 191. Airbag; 192. Pipe clamp; 193. Airflow channel; 194. Third partition; 195. Fifth pipe seat; 196. Feed channel; 197. Cylindrical cam; 198. Ball end rod; 199. Guide rod; 200. Sliding column; 201. Pressure head; 202. Ball. Detailed Implementation

[0066] The embodiments of the present invention are described in detail below. Examples of these embodiments are shown in the accompanying drawings, wherein the same or similar reference numerals denote the same or similar elements or elements having the same or similar functions throughout. The embodiments described below with reference to the accompanying drawings are exemplary and are only used to explain the present invention, and should not be construed as limiting the present invention.

[0067] In the description of this invention, it should be noted that, unless otherwise explicitly specified and limited, the terms "installation", "connection", and "joining" should be interpreted broadly. For example, they can refer to a fixed connection, a detachable connection, or an integral connection. Those skilled in the art can understand the specific meaning of the above terms in this invention based on the specific circumstances.

[0068] like Figure 1 and 2As shown in Embodiment 1, an integrated extraction and oil removal device includes a fine filter 1, an activated carbon adsorption column 2, a resin adsorption column 3, and a composite fiber adsorption device 4. The inlet of the fine filter 1 is used to connect to the extraction system. The outlet of the fine filter 1 is connected to a second pipe 7 via a first pipe 6. The second pipe 7 has at least two branch interfaces 8, and a third pipe 9 is connected to each branch interface 8. The third pipe 9 is used to connect to the activated carbon adsorption column 2. The outlet of the activated carbon adsorption column 2 is connected to a fourth pipe 11, which is used to connect to the resin adsorption column 3. The outlet of the resin adsorption column 3 is connected to a fifth pipe 12. Pipe 12 is used to connect the composite fiber adsorption device 4. The outlet of the composite fiber adsorption device 4 is connected to a sixth pipe 13. An oil content detector 14 is installed on the sixth pipe 13. A seventh pipe 15 is connected to the side wall of the sixth pipe 13. The free end of the seventh pipe 15 is connected to the return port of the fine filter 1. The outlet of the third pipe 9 is connected to a first valve 17. The inlet and outlet of the fourth pipe 11 are connected to a second valve 18. The inlet and outlet of the fifth pipe 12 are connected to a third valve 19. A fourth valve 20 is connected to the sixth pipe 13. A fifth valve 21 is connected to the seventh pipe 15. The technical problem that can be solved is that traditional single-method filtration and oil removal is inefficient, leading to excessive oil content in the product. Process: The extraction system feed liquid enters the fine filter 1, flows through the first pipe 6 to the second pipe 7, then through the diversion port 8 and the third pipe 9 into the activated carbon adsorption column 2, then through the fourth pipe 11 to the resin adsorption column 3, and the fifth pipe 12 to the composite fiber adsorption device 4. After filtration, it is tested by the oil content analyzer through the sixth pipe 13. Qualified products are discharged, while unqualified products are returned to the fine filter 1 through the seventh pipe 15. The opening and closing of the corresponding pipes are controlled by the first to fifth valves 21. Beneficial effects: Multi-stage adsorption oil removal is achieved; oil content can be returned for secondary treatment after testing; the diversion design improves processing efficiency; valve control facilitates opening, closing, and maintenance; ensures that the output oil content meets standards; improves processing efficiency and stability; and reduces maintenance costs.

[0069] like Figure 3As shown, as an optimization of Embodiment 1, the fine filter 1 includes a first base 22, on which a first leg 23 distributed circumferentially is connected, and a first tank 24 is connected to the first leg 23. The middle side wall of the first tank 24 has a first water inlet pipe 25, and the lower side wall of the first tank 24 has a first water outlet pipe 26. A filter assembly 27 is installed on the inner wall of the first tank 24, and the filter assembly 27 is used to purify the liquid from the first water inlet pipe 25. The lower port of the first tank 24 is connected to a first bottom cover 28, and the first bottom cover 28 has a drain pipe 29. The upper port of the first tank 24 is connected to a first top cover 31 by a lifting eye bolt 30. A lead screw 32 is rotatably connected to the top of the first top cover 31, and a rocker arm 33 is threaded onto the lead screw 32. The rocker arm 33 is L-shaped, and the lower end of the rocker arm 33 is rotatably connected to a first support seat 34, which is connected to the first tank 24. Technical problems that can be solved: The existing fine filter 1 is inconvenient to install and disassemble, has poor tank sealing and positioning, and cannot discharge filter residue in a timely manner. Operation process: The feed liquid enters the first tank 24 from the first inlet pipe 25, is purified by the filter assembly 27, and is discharged from the first outlet pipe 26. When the top cover needs to be opened, the screw 32 is rotated to rotate the rocker arm 33, causing the rocker arm 33 to disengage from the first support seat 34, thereby opening the top cover; the filter residue is discharged through the drain pipe 29 of the first bottom cover 28. Beneficial effects: The fine filter 1 has a stable structure, the top cover is easy to open and close, facilitating maintenance of the filter assembly 27, and the drain pipe 29 allows for timely discharge of filter residue, improving filtration stability.

[0070] like Figure 4 As shown, as an optimization of Embodiment 1, the filter assembly 27 includes a first partition 35, the surface of which is located between the surfaces of the first inlet pipe 25 and the first outlet pipe 26. The top surface of the first partition 35 has first through holes 36 arranged at equal angles. A first pipe seat 37 is installed on the first through hole 36. A first filter cartridge seat 38 is connected to the first pipe seat 37. A first filter tube 39 is connected to the first filter cartridge seat 38. The upper end of the first filter tube 39 is connected to a second filter cartridge seat 40. An end cap 41 is connected to the top surface of the second filter cartridge seat 40. A filter cloth 42 is installed on the outer wall of the first filter tube 39. Movement process: After the liquid enters the first tank 24, it is filtered by the filter cloth 42 and then flows to the first outlet pipe 26. Beneficial effects: The filter tubes arranged at equal angles increase the filtration area. The filter cloth 42 is firmly attached to the filter tubes and filter cartridge seats, the filtration path is clear, and the purification effect of the liquid is improved.

[0071] like Figure 5 and 6As shown, as an optimization of Embodiment 1, the activated carbon adsorption column 2 and resin adsorption column 3 include a second base 43, a second foot 44 arranged circumferentially connected to the second base 43, a second tank 45 connected to the second foot 44, a second top cover 46 connected to the upper port of the second tank 45, a second water inlet pipe 47 on the second top cover 46, a second bottom cover 48 connected to the lower port of the second tank 45, a second water outlet pipe 49 on the second bottom cover 48, a first filter cotton 50 filled at the bottom of the second tank 45, and a first mesh plate 52 connected to the inner wall of the second tank 45 by ball bearing positioning pins 51. The first mesh plate 52 is used to press down the first filter cotton 50, and activated carbon particles 53 or resin particles 54 are filled above the first mesh plate 52. The technical problem that can be solved is that the adsorbed particles in the existing adsorption column are easily loosened and displaced, the filter cotton is not firmly fixed, and the contact between the liquid and the adsorbed particles is insufficient. Movement Process: The feed solution enters the second tank 45 through the second inlet pipe 47, where it comes into contact with and is adsorbed by the activated carbon particles 53 or resin particles 54 inside the tank. Afterward, it is filtered by the first filter cotton 50 below the first mesh plate 52 and discharged through the second outlet pipe 49. Beneficial Effects: The first mesh plate 52 is fixed by ball bearing positioning pins 51, effectively compressing the filter cotton, improving the stability of the contact between the adsorbed particles and the feed solution, and enhancing the adsorption effect.

[0072] like Figure 7As shown, as an optimization of Embodiment 1, the composite fiber adsorption device 4 includes a third base 55, on which a housing 56 is mounted. A third inlet pipe 57 and a third outlet pipe 58 are connected to the housing 56. A thrust plate 59 and a support base 60 are installed inside the housing 56, arranged opposite to each other. The third inlet pipe 57 is connected to an inlet hole 61 on the thrust plate 59, and the third outlet pipe 58 is connected to an outlet hole 62 on the thrust plate 59. A first connecting seat 63, symmetrically arranged vertically, is connected to the outer end face of the thrust plate 59. A second connecting seat 64 is connected to the outer end face of the support base 60. A first support rod 65 is connected between the support base 60 and the thrust plate 59, located at the center of the side of the thrust plate 59. A second support rod 66 is connected by a gap and is located on the bottom surface of the thrust plate 59. Several filter frames 67 and several filter plates 68 are overlapped on the first support rod 65. Filter paper 69 is installed between the filter frames 67 and the filter plates 68 to form a filter bed for filtering oil in the liquid. The filter bed is positioned by pressing by a pressure plate 71. The outer end face of the pressure plate 71 is rotatably connected to a first lead screw 72. A threaded seat 73 is threaded on the first lead screw 72 and connected to the support seat 60. A handwheel 74 is connected to the free end of the first lead screw 72. The filter bed is arranged in the order of thrust plate 59, filter paper 69, filter frame 67, filter paper 69, filter plate 68, filter paper 69, and pressure plate 71, and the bottom surfaces of the filter frames 67 and filter plates 68 abut against the second support rod 66. Movement Process: Rotating the handwheel 74 drives the first lead screw 72 to rotate, which in turn drives the pressure plate 71 to squeeze the filter bed through the threaded seat 73. The liquid enters the water inlet 61 of the thrust plate 59 from the third water inlet pipe 57, flows through the filter bed composed of filter paper 69, filter frame 67, and filter plate 68, and the oil is trapped and purified before being discharged from the third water outlet pipe 58. To disassemble, rotate the handwheel 74 in the opposite direction to loosen the pressure plate 71 and remove the filter frame 67, filter plate 68, and filter paper 69. Beneficial Effects: The filter bed is reasonably arranged, the pressure plate 71 is firmly positioned by the lead screw, and disassembly and assembly are convenient. The filter paper 69, filter frame 67, and filter plate 68 work together to form a high-efficiency oil removal filter bed, improving the oil removal efficiency.

[0073] like Figure 8 As shown, as an optimization of Embodiment 1, the inner side of the thrust plate 59 has a first recess 75, and the lower end face of the thrust plate 59 has a water inlet 61 and a water outlet 62, with the water outlet 62 communicating with the first recess 75; the side of the thrust plate 59 has connecting ears 76 for mounting a first support rod 65 and a second support rod 66. Beneficial effects: Clear water inlet and outlet paths, smooth material flow, and the connecting ears 76 improve the stability of the support rod installation, ensuring the reliability of the filter bed structure.

[0074] like Figure 9As shown, as an optimization of Embodiment 1, the inner side of the pressing plate 71 has a second concave cavity 77, and the end face of the pressing plate 71 has a water outlet cavity 78; the water outlet cavity 78 communicates with the second concave cavity 77; the side of the pressing plate 71 has a first bracket 79 that overlaps with the first support rod 65. Beneficial effects: The water outlet channel is smooth, improving the material discharge efficiency; the first bracket 79 ensures reliable connection between the pressing plate 71 and the support rod, enhancing the pressing stability of the filter bed.

[0075] like Figure 10 As shown, as an optimization of Embodiment 1, the filter frame 67 has a third cavity 80 on both end faces, and a through groove 81 penetrating the third cavity 80 on the filter frame 67. The lower end face of the filter frame 67 has an inlet hole 61 and an outlet hole 62, with the inlet hole 61 communicating with the through groove 81. The side of the filter frame 67 has a second bracket 82 that overlaps with the first support rod 65. Beneficial effects: The through groove 81 and the third cavity 80 increase the contact area between the liquid and the filter, improving filtration uniformity; the second bracket 82 ensures the filter frame 67 is securely installed.

[0076] like Figure 11 As shown, as an optimization of Embodiment 1, the filter plate 68 has a fourth cavity 83 on both end faces, and the fourth cavity 83 has a matrix of protrusions 84 arranged on it, with the protrusions 84 flush with the end faces of the filter plate 68; the lower end face of the filter plate 68 has a water inlet hole 61 and a water outlet hole 62, with the water outlet hole 62 communicating with the fourth cavity 83; the side of the filter plate 68 has a second bracket 82 that overlaps with the first support rod 65. Beneficial effects: The protrusions 84 increase the filtration area and make the liquid evenly distributed, improving the filtration effect; the second bracket 82 ensures the filter plate 68 is securely installed.

[0077] like Figure 12 As shown, as an optimization of Embodiment 1, the lower end face of the filter paper 69 is provided with a water inlet hole 61 and a water outlet hole 62. The lower side of the filter paper 69 is flush with the filter frame 67 and the filter plate 68, and the top edge of the filter paper 69 protrudes outside the filter frame 67 and the filter plate 68. Beneficial effects: Reduces the risk of leakage, improves filtration sealing, and the protruding top edge design facilitates filter paper 69 replacement, reducing maintenance costs.

[0078] like Figure 13 and 14As shown, as an optimization of Embodiment 1, the side wall of the first tank 24 is connected to a first branch pipe 85 and a second branch pipe 86. The first branch pipe 85 and the second branch pipe 86 are located above the first partition 35. A first tee pipe 87 is connected to the first branch pipe 85 and the second branch pipe 86. The two ends of the first tee pipe 87 are connected to a second pipe seat 88. A pump body 89 is connected to the second pipe seat 88. The pump body 89 includes a first housing 90. A right-angle seat 91 is installed inside the first housing 90. A rubber tube 92 is installed on the right-angle seat 91. One end of the rubber tube 92 is connected to the second pipe seat 88. A triangular seat 93 is rotatably connected inside the first housing 90. A pressure roller 94 is rotatably connected to the triangular seat 93. The pressure roller 94 is used to squeeze the rubber tube 92. The triangular seat 93 is driven by a first motor 95. The opposite ends of the rubber tube 92 are connected through an eighth pipe 96 to form a liquid circulation and stirring channel. The stirring makes the liquid evenly distributed in the filter assembly 27. Technical problems that can be solved: In the existing fine filter 1, the liquid distribution is uneven, the filter element 27 is easily clogged due to uneven force, and the purification efficiency is low. Movement process: The first motor 95 drives the triangular seat 93 to rotate, which in turn drives the pressure roller 94 to squeeze the rubber tube 92, causing the liquid in the first branch pipe 85 and the second branch pipe 86 to circulate through the rubber tube 92 and the eighth pipe 96, stirring the liquid above the first partition 35. Beneficial effects: The circulating and stirring of the liquid achieves uniform distribution, avoids local clogging of the filter element 27, and improves the service life and purification efficiency of the filter element 27.

[0079] like Figure 15 As shown, as an optimization of Embodiment 1, the inner wall of the second tank 45 is connected to symmetrically arranged second mesh plates 98. The gaps between the second mesh plates 98 are filled with turbulence-inducing balls 99. The surface of the turbulence-inducing balls 99 has several through holes 100. By setting the turbulence-inducing balls 99, the liquid can be evenly injected into the second tank 45. Technical problem solved: In existing adsorption columns, the liquid flows too quickly, resulting in insufficient contact with the adsorbed particles and low adsorption efficiency. Beneficial effect: The turbulence-inducing balls 99 achieve uniform dispersion of the liquid, prolong the contact time between the liquid and the adsorbed particles, and improve adsorption efficiency.

[0080] like Figure 16 and 17 As shown, as an optimization of Embodiment 1, a first telescopic rod 101 is installed on the second top cover 46. The piston end of the first telescopic rod 101 extends into the second tank 45 and passes through the second mesh plate 98. A ring 103 is connected to the lower end of the first telescopic rod 101, and a cross rod 104 is connected to the ring 103. By setting the liftable ring 103, the clumping of activated carbon particles 53 or resin particles 54 can be prevented, and the fluidity can be improved. Technical problem solved: Activated carbon particles 53 or resin particles 54 in the adsorption column are prone to clumping, resulting in poor fluidity and affecting the adsorption effect. Beneficial effects: Prevents clumping of adsorption particles, improves particle fluidity, ensures sufficient contact between the liquid and particles, and enhances the adsorption effect.

[0081] like Figure 18-20 As shown, as an optimization of Embodiment 1, a third branch pipe 105 is connected to the lower side wall of the second tank 45, and a fourth branch pipe 106 is connected to the upper side wall of the second tank 45. A second three-way pipe 107 is connected to the third branch pipe 105 and the fourth branch pipe 106. A second housing 108 is connected to both ends of the second three-way pipe 107. A drive gear 109 is rotatably connected inside the second housing 108. The drive gear 109 is driven by a second motor 110. A chain 111 meshes with the drive gear 109, and first scrapers 112 are installed on the chain 111 at intervals. The opposite ports of the second housing 108 are connected through a ninth pipe 113, forming a circulating stirring channel for activated carbon particles 53 or resin particles 54. Stirring makes the mixture of the liquid and activated carbon particles 53 or resin particles 54 more uniform. The technical problem that can be solved is: uneven mixing of the liquid and adsorption particles in the adsorption column, easy particle deposition, and low adsorption efficiency. Movement Process: The second motor 110 drives the drive gear 109 to rotate, which in turn moves the chain 111 and scraper, causing the activated carbon particles 53 or resin particles 54 in the second tank 45 to circulate through the third branch pipe 105, the ninth pipe 113, and the fourth branch pipe 106, achieving thorough mixing with the liquid. Beneficial Effects: The circulating stirring of the particles improves the uniformity of mixing with the liquid, prevents particle sedimentation, and enhances the adsorption effect.

[0082] like Figure 21As shown, in Embodiment 2, unlike Embodiment 1, a first carrier plate 115 is connected to the inner wall of the first tank 24. The first carrier plate 115 is located above the filter assembly 27. A first shaft tube 116 is rotatably connected to the first carrier plate 115. A first stirring blade 117 is connected to the lower side wall of the first shaft tube 116. A first bevel gear 118 is connected to the upper end of the first shaft tube 116. A second bevel gear 119 meshes with the first bevel gear 118. The second bevel gear 119 is driven by a third motor 120. A bevel gear 119 is mounted on a support frame 121, which is connected to a first carrier plate 115. A third bevel gear 122 is rotatably connected to the support frame 121, meshing with the second bevel gear 119. A shaft 123 is connected to the third bevel gear 122, and the shaft 123 is clearance-fitted with a first shaft tube 116. A second stirring blade 124 is connected to the lower end of the shaft 123. By setting the first stirring blade 117 and the second stirring blade 124 to rotate in opposite directions, the liquid is made more uniform. The technical problem solved: In the existing fine filter 1, the liquid is stirred in a single direction, resulting in uneven mixing and affecting filtration efficiency. Motion process: The third motor 120 drives the second bevel gear 119 to rotate, causing the first bevel gear 118 and the third bevel gear 122 to rotate in opposite directions. This, in turn, causes the first shaft tube 116 (driving the first stirring blade 117) and the shaft 123 (driving the second stirring blade 124) to rotate in opposite directions, thus performing bidirectional stirring of the liquid. Beneficial effects: Two-way stirring enhances the uniformity of liquid mixing, improves the purification efficiency of the filter element 27, and shortens the processing time.

[0083] like Figure 22-24As shown, in Embodiment 3, unlike Embodiment 1, a third bottom cover 125 is connected to the lower end of the first tank 24. A rotating rod 126 is rotatably connected to the third bottom cover 125. A second partition 127 is installed inside the first tank 24. The top surface of the second partition 127 has four second through holes 128 arranged at equal angles. A third tube seat 129 is rotatably connected to the second through holes 128. A first filter cartridge seat 38 is connected to the third tube seat 129. A first filter tube 39 is connected to the first filter cartridge seat 38. A second filter cartridge seat 40 is connected to the upper end of the first filter tube 39. A fourth tube seat 130 is connected to the top surface of the second filter cartridge seat 40. An end cap 41 is connected to the fourth tube seat 130. A filter cloth 42 is installed on the outer wall of the first filter tube 39. A positioning bolt 131 is connected to the fourth tube seat 130, and the positioning bolt 131 is connected to the rotating rod 126; it also includes a frame 132 mounted on the first base 22, a first rotating shaft 133 rotatably connected to the frame 132, and a fourth motor 135 connected to the first rotating shaft 133 via a belt drive 134; a second rotating shaft 136 is provided at the upper end of the first rotating shaft 133, and the second rotating shaft 136 is rotatably connected to the frame 132; a first eccentric shaft 137 is connected to the upper end of the second rotating shaft 136, a cross-shaped frame 138 is rotatably connected to the first eccentric shaft 137, and the four branches of the cross-shaped frame 138 are rotatably connected to second eccentric shafts 139, the four second eccentric shafts 139 rotate synchronously, and the second eccentric shafts 139 are rotatably connected to the rotating rod 126. The technical problem that can be solved: In the existing fine filter 1, the filter assembly 27 is fixed, the filter cloth 42 is easily clogged, and the filtration efficiency drops rapidly. Movement Process: The fourth motor 135 drives the first rotating shaft 133 to rotate via the belt drive 134, which in turn drives the second rotating shaft 136 and the first eccentric shaft 137 to rotate. This causes the second eccentric shaft 139 on the cross-shaped frame 138 to drive the rotating rod 126 to rotate, thereby rotating the filter tube. Beneficial Effects: The rotation of the filter tube makes the filter cloth 42 less prone to clogging, extends the service life of the filter assembly 27, and improves the stability of filtration efficiency.

[0084] like Figure 25-27As shown, as an optimization of Embodiment 3, a second carrier plate 140 is connected to the inner wall of the first tank 24. The second carrier plate 140 is located above the filter assembly 27. A third housing 141 is connected to the second carrier plate 140. A worm gear 142 is rotatably connected inside the third housing 141. The worm gear 142 meshes with a worm wheel 143 driven by a fifth motor 144. A splined shaft 145 is slidably connected to the worm wheel 143. A bracket 146 is connected to the lower end of the splined shaft 145. A ring seat 147 is connected to the bracket 146. Ear seats 148 arranged at equal angles are connected to the side wall of the ring seat 147. A top rod 149 is slidably connected to the ear seats 148. A return spring 150 is connected to the top rod 149. The end face of the top rod 149 is... The filter has bristles 151 for cleaning the filter cloth 42. A second support seat 152 is connected to the third housing 141, and two symmetrically arranged third support seats 153 are connected to the second support seat 152. A guide rail 154 is mounted on the third support seat 153, and a slide seat 155 is slidably connected to the guide rail 154. A moving stage 156 is mounted on the slide seat 155, and a first bearing seat 157 is connected to the moving stage 156 and rotatably connected to the tail end of the splined shaft 145. A ball bearing slide 158 is mounted on the moving stage 156. A fourth support seat 159 with a second lead screw 160 is mounted on the second support seat 152. The second lead screw 160 is adapted to the ball bearing slide 158 and driven by a sixth motor 161. The technical problem it solves is that the surface of the filter cloth 42 in the existing fine filter 1 is not thoroughly cleaned, manual cleaning is cumbersome, and maintenance costs are high. Movement Process: The fifth motor 144 drives the worm gear 143 to rotate, which in turn drives the worm 142 and splined shaft 145 to rotate, causing the top rod 149 on the bracket 146, ring seat 147, and ear seat 148 to rotate. The ring seat 147 corresponds to the filter cloth 42. The sixth motor 161 drives the second lead screw 160 to rotate, which, through the ball bearing slide 158, drives the moving stage 156 and splined shaft 145 to move along the guide rail 154, realizing the comprehensive cleaning of the filter cloth 42 by the brush bristles 151. Beneficial Effects: Automatic cleaning of the filter cloth 42 without manual disassembly, reducing maintenance costs and ensuring filtration efficiency.

[0085] like Figures 28-30As shown in Embodiment 4, unlike Embodiment 1, a third carrier plate 162 is rotatably connected to the inner wall of the first tank 24. Indexing rollers 163 arranged at equal angles are connected to the third carrier plate 162. The indexing rollers 163 are driven by an arc-shaped cam 164, which is mounted on a second bearing seat 165 connected to the first tank 24. The arc-shaped cam 164 is driven by a seventh motor 166. A vertical rod 167 is connected to the bottom surface of the third carrier plate 162, corresponding to the indexing rollers 163. A first spring 168 is connected to the lower end of the vertical rod 167, and a sliding tube 169 is connected to the lower end of the first spring 168. A cleaning component 170 is connected to the bottom surface of the sliding tube 169. The technical problem that can be solved is that filter residue easily accumulates on the first partition 35 of the existing fine filter 1, making cleaning inconvenient and affecting the flow of the liquid. Movement Process: The seventh motor 166 drives the arc-shaped cam 164 to rotate, which in turn drives the indexing roller 163 and the third carrier plate 162 to rotate intermittently. This causes the vertical rod 167, the slide tube 169, and the cleaning component 170 to rotate with the third carrier plate 162. The cleaning component 170, rotating with the third carrier plate 162, cleans the deposits on the partition plate. Beneficial Effects: Automatically cleans the filter residue on the partition plate, ensuring smooth flow of the filtrate, improving filtration efficiency, and reducing maintenance workload.

[0086] like Figure 31 As shown, the first type of cleaning component 170 includes a first base plate 171 mounted on a slide tube 169. Symmetrically arranged second scrapers 172 are hinged to both ends of the first base plate 171. The second scrapers 172 are used to clean deposits on the first partition 35. Second springs 173 are installed between the opposing second scrapers 172. Beneficial effects: The springs ensure a tight fit between the scrapers and the partition, resulting in good cleaning performance; the hinged design of the scrapers prevents damage to the partition and expands the cleaning range.

[0087] like Figure 32 As shown, the second type of cleaning component 170 includes a second base plate 174 mounted on the slide tube 169. The second base plate 174 is arc-shaped, and a third scraper 175 is hinged to the second base plate 174. The third scraper 175 is used to clean the deposits on the first partition 35. A third spring 176 is connected at the angle between the second base plate 174 and the third scraper 175. Advantages: The arc-shaped base plate adapts to the partition, and the spring ensures a tight fit between the scraper and the surface, resulting in thorough cleaning and strong adaptability.

[0088] like Figure 33 and 34As shown, as an optimization of Embodiment 4, a slag storage tank 177 is connected to the side wall of the first partition 35. The slag storage tank 177 is used to collect the sediment in the first tank 24. The slag storage tank 177 is funnel-shaped. The side wall of the slag storage tank 177 has a slag inlet pipe 178. The port of the slag inlet pipe 178 has an inclined baffle 179. The top surface of the slag storage tank 177 has a return pipe 180, which sends the clean liquid back into the first tank 24. A discharge plug 181 is installed at the lower end of the slag storage tank 177. Technical problem that can be solved: The cleaned filter residue is easy to flow back into the liquid, the filter residue is inconvenient to collect, and the purification effect is affected. Movement process: The sediment scraped off by the cleaning component 170 enters the slag storage tank 177 through the slag inlet pipe 178 (guided by the baffle 179). The clean liquid in the slag storage tank 177 returns to the first tank 24 through the return pipe 180. The filter residue is discharged through the discharge plug 181. Beneficial effects: Thorough collection of filter residue prevents backflow and contamination of the liquid, and the discharge plug 181 facilitates filter residue cleaning, thus improving the purification effect.

[0089] like Figure 35 and 36As shown, in Embodiment 5, unlike Embodiment 1, a fourth carrier plate 182 is installed inside the first tank 24. A main shaft 183 is rotatably connected to the fourth carrier plate 182. The main shaft 183 is driven by an eighth motor 184. A symmetrically arranged third filter cartridge seat 185 is slidably connected to the side wall of the main shaft 183. A second filter tube 186 is installed in the third filter cartridge seat 185 with gaps. A filter cloth 42 is installed on the outer wall of the second filter tube 186. A fourth spring 187 is connected to the upper and lower ends of the third filter cartridge seat 185. A limit ring 188 is connected to the free end of the fourth spring 187. A limit block 190 is connected to the side wall of the main shaft 183 by fastening bolts 189. The limit block 190 is used for... At the position of the blocking and limiting ring 188; an air bladder 191 is fixed to the main shaft 183 inside the second filter tube 186 by a pipe clamp 192. The center of the main shaft 183 has an airflow channel 193, which is used to inject air into the air bladder 191. The inflated air bladder 191 can clean the deposits on the filter cloth 42. A third partition 194 is connected inside the first tank 24. A fifth pipe seat 195 is rotatably connected to the third partition 194. The fifth pipe seat 195 is connected to the lower end of the main shaft 183. A liquid channel 196 is opened on the main shaft 183 inside the second filter tube 186. The liquid channel 196 penetrates the bottom surface of the main shaft 183 and sends the filtered liquid to the outlet. Technical problems that can be solved: The existing fine filter 1 requires disassembly to clean the deposits on the filter cloth 42, which is cumbersome. The filter tube is not firmly fixed, and the liquid filtration path is unreasonable. Movement Process: The eighth motor 184 drives the main shaft 183 to rotate, which in turn drives the second filter tube 186 to rotate. After the liquid is filtered through the filter cloth 42 on the outer wall of the second filter tube 186, it enters the outlet through the liquid channel 196 and is discharged. When the filter cloth 42 needs to be cleaned, air is injected into the air bladder 191 through the airflow channel 193. The air bladder 191 expands and squeezes the filter cloth 42 to remove the deposits. Beneficial Effects: The expansion of the air bladder 191 automatically cleans the deposits on the filter cloth 42 without disassembly, making maintenance convenient; the filter tube is firmly positioned, the liquid filtration path is smooth, and the purification efficiency is improved.

[0090] like Figure 37 and 38As shown, as an optimization of Embodiment 5, a cylindrical cam 197 is connected to the side wall of the main shaft 183, and a ball joint rod 198 is slidably connected to the cylindrical cam 197. Guide rods 199 arranged at equal angles are connected to the fourth carrier plate 182, and a sliding column 200 is slidably connected to the guide rods 199. The side wall of the sliding column 200 is connected to the ball joint rod 198, and a pressure head 201 is connected to the bottom surface of the sliding column 200. A ball 202 is rotatably connected to the pressure head 201, and the ball 202 is used to push the upper third filter cartridge seat 185 to reciprocate. Movement process: The rotation of the main shaft 183 drives the cylindrical cam 197 to rotate, causing the ball joint rod 198 to drive the sliding column 200 to slide up and down along the guide rod 199. The pressure head 201, through the ball 202, pushes the third filter cartridge seat 185 to reciprocate up and down, causing the second filter tube 186 and filter cloth 42 to move up and down. Beneficial effects: The up-and-down reciprocating motion of the filter tube enhances the contact effect between the filter cloth 42 and the liquid, while assisting the air bag 191 in cleaning up the attached substances, thus improving filtration and self-cleaning efficiency.

[0091] Furthermore, the traditional preparation process currently faces the following key technical bottlenecks: 1. Insufficient extraction and separation precision and efficiency: The purity of cerium carbonate produced by traditional extraction processes is generally below 99.99% (4N), with major rare earth impurities (such as La and Pr) around 20 ppm and Nd around 10 ppm. To achieve higher purity, extremely long extraction stages are often required, resulting in low production efficiency, high costs, and complex control. 2. Impurities introduced by precipitants: Commercially available precipitants themselves contain many impurities and additives, becoming the main source of rare earth impurities (such as Fe, Ca, and Si) in the product. Simultaneously, due to the presence of oily additives remaining in the precipitated product, complete separation is impossible. Therefore, an oil-free cerium carbonate preparation process using an integrated extraction and oil removal device is proposed.

[0092] Example 1 1. Raw material pretreatment: Take a mixed rare earth chloride solution (CeO2 / REO=50%, REO=280g / L, pH=4.0-5.0), filter it using a 0.22μm polytetrafluoroethylene filter at a pressure of 0.25MPa, add a small amount of hydrochloric acid to adjust the pH to 2.0, and obtain the pretreated solution.

[0093] 2. Multi-stage extraction: The pretreated solution was pumped into a 180-stage extraction system at a flow rate of 10 L / h. The parameters for the La / Ce / Pr / Nd separation stages (180 stages in total) were as follows: temperature 35-55℃, organic-aqueous phase ratio (O / A) = 1.0-7.0, aqueous phase HCl concentration 4.5-5.5 mol / L, and stirring speed 280-320 rpm. After extraction, the relative purity of CeO2 in the obtained cerium chloride solution was ≥99.9995%, and the key rare earth impurities La2O3 / REO ≤3.5 ppm and Pr6O2 ≤3.5 ppm. 11 / REO≤0.5PPm, Nd2O3 / REO≤0.5PPm, total amount of other impurities≤0.5PPm, total≤5PPm.

[0094] 3. Multi-stage oil removal: The extracted cerium chloride solution is sequentially passed through precision pre-filtration → activated carbon adsorption → special macroporous polymer adsorption → composite fiber filtration at a certain flow rate. The oil content at the outlet is ≤0.5 ppm, and the total amount of non-rare earth impurities is ≤0.5 ppm.

[0095] 4. Preparation of precipitant and precipitation: (1) In a closed reaction vessel, CO2 gas with a purity of 99.999% and electronic grade ammonia water are introduced, and the reaction temperature is controlled at 15-25℃ and the pressure is 0.2→0.5MPa. After 2 hours of reaction, ammonium carbonate precipitant with a non-rare earth impurity content ≤0.5PPm is obtained. (2) Continuous precipitation by stage: The degreased cerium chloride solution (containing CeO2=50g / L) is added to the reactor at a temperature of 45~55℃, and the precipitant prepared in step 4 is added at a flow rate of 0.5m. 3 / h, until pH=5.5-6.0, age for 1 hour, separate solid and liquid, heat the filtrate to 65℃, add ammonium carbonate precipitant dropwise until pH=6.5-7.0, keep warm for 0.5 hours after the reaction is complete, and centrifuge to dehydrate.

[0096] 5. Washing and dehydration: The precipitate was washed 5 times with 50℃ high-purity hot water (conductivity ≤0.4μS / cm) for 15 minutes each time, and then dehydrated by high-speed centrifugation at 9000rpm to obtain a white powdered cerium carbonate product.

[0097] The products obtained in the examples were tested, and the results are as follows: -Purity: CeO2 / REO≥99.9995% (meets 5N5 standard); - Rare earth impurities: La2O3 / REO ≤ 3.5 ppm, Pr6O 11 / REO≤0.5PPm、 Nd2O3 / REO≤0.5ppm, total amount of other impurities≤0.5ppm, total ≤5ppm; - Single non-rare earth impurities: Fe2O3≤1.0PPm, CaO≤1.0PPm, SiO2≤1.0PPm MgO≤1.0PPm; Al2O3≤1.0PPm, PbO≤1.0PPm, Na2O≤1.0PPm, ZnO≤1.0ppm, SO4 2- ≤1.0PPm - Oil content: ≤0.3 ppm (meets the requirement of ≤0.5 ppm); - Acid solubility: Solubility in 1 mol / L HNO3 ≥ 99.5%.

[0098] This invention, through process integration, fully meets the requirements of target indicators and high-end application scenarios.

[0099] (III) Beneficial Effects Compared with existing technologies, this invention has significant advantages. Firstly, it achieves complete oil removal by pioneering a three-stage combined oil removal system of "filtration-resin adsorption-fine filtration," which stably controls residual oil at ≤0.5 ppm, solving the industry-wide problem of organic phase residue affecting product quality. Moreover, the three-stage process is tightly integrated and can be adapted to industrial continuous production scenarios. Secondly, it can control impurities at the source by independently preparing a low-impurity precipitant with non-rare earth impurities ≤0.5 ppm, thus eliminating the introduction of external impurities at the source.

[0100] Although the present invention has been described in detail with reference to the foregoing examples, those skilled in the art can still make and modify the technical solutions described in the foregoing embodiments, or make equivalent substitutions for some of the technical features. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present invention should be included within the protection scope of the present invention.

Claims

1. An integrated extraction and oil removal device, characterized in that, The system includes a fine filter (1), an activated carbon adsorption column (2), a resin adsorption column (3), and a composite fiber adsorption device (4). The inlet of the fine filter (1) is used to connect to the extraction system. The outlet of the fine filter (1) is connected to a second pipe (7) through a first pipe (6). The second pipe (7) has at least two branch interfaces (8). A third pipe (9) is connected to the branch interfaces (8). The third pipe (9) is used to connect to the activated carbon adsorption column (2). The activated carbon adsorption column (2) is connected to the resin adsorption column (3) through a fourth pipe (11). The resin adsorption column (3) is connected to the composite fiber adsorption device (4) through a fifth pipe (12). The outlet of the adsorption device (4) is connected to the sixth pipe (13), the sixth pipe (13) is equipped with a pipe oil detector (14), the side wall of the sixth pipe (13) is connected to the seventh pipe (15), the free end of the seventh pipe (15) is connected to the return port of the fine filter (1); the outlet of the third pipe (9) is connected to the first valve (17), the inlet and outlet of the fourth pipe (11) are connected to the second valve (18), the inlet and outlet of the fifth pipe (12) are connected to the third valve (19), the sixth pipe (13) is connected to the fourth valve (20), and the seventh pipe (15) is connected to the fifth valve (21).

2. The integrated extraction and oil removal equipment according to claim 1, characterized in that, The fine filter (1) includes a first base (22), on which are connected circumferentially distributed first legs (23), and on which are connected a first tank (24). The middle side wall of the first tank (24) has a first inlet pipe (25), and the lower side wall of the first tank (24) has a first outlet pipe (26). A filter assembly (27) is installed on the inner wall of the first tank (24), and the filter assembly (27) is used to purify the liquid from the first inlet pipe (25); the first tank (24) 4) The lower port is connected to the first bottom cover (28), and the first bottom cover (28) has an vent pipe (29); the upper port of the first tank (24) is connected to the first top cover (31) by a lifting eye bolt (30), the top of the first top cover (31) is rotatably connected to a screw rod (32), and a rocker arm (33) is threaded on the screw rod (32). The rocker arm (33) is L-shaped, and the lower end of the rocker arm (33) is rotatably connected to the first bearing seat (34). The first bearing seat (34) is connected to the first tank (24).

3. The integrated extraction and oil removal equipment according to claim 2, characterized in that, The filter assembly (27) includes a first partition (35), the surface of which is located between the surfaces of the first inlet pipe (25) and the first outlet pipe (26). The top surface of the first partition (35) has a first through hole (36) arranged at equal angles. A first pipe seat (37) is installed on the first through hole (36). A first filter cartridge seat (38) is connected to the first pipe seat (37). A first filter tube (39) is connected to the first filter cartridge seat (38). A second filter cartridge seat (40) is connected to the upper end of the first filter tube (39). An end cap (41) is connected to the top surface of the second filter cartridge seat (40). A filter cloth (42) is installed on the outer wall of the first filter tube (39).

4. The integrated extraction and oil removal equipment according to claim 1, characterized in that, The activated carbon adsorption column (2) and the resin adsorption column (3) include a second base (43), a second foot (44) arranged circumferentially connected to the second base (43), a second tank (45) connected to the second foot (44), a second top cover (46) connected to the upper port of the second tank (45), a second water inlet pipe (47) on the second top cover (46), a second bottom cover (48) connected to the lower port of the second tank (45), a second water outlet pipe (49) on the second bottom cover (48), a first filter cotton (50) filled at the bottom of the second tank (45), a first mesh plate (52) connected to the inner side wall of the second tank (45) by a ball positioning pin (51), the first mesh plate (52) used to press down the first filter cotton (50), and the first mesh plate (52) used to fill activated carbon particles (53) or resin particles (54).

5. The integrated extraction and oil removal equipment according to claim 1, characterized in that, The composite fiber adsorption device (4) includes a third base (55), a housing (56) is installed on the third base (55), a third water inlet pipe (57) and a third water outlet pipe (58) are connected to the housing (56), a thrust plate (59) and a support base (60) are installed inside the housing (56) and are arranged opposite to each other. The third water inlet pipe (57) is connected to the water inlet hole (61) on the thrust plate (59), and the third water outlet pipe (58) is connected to the water outlet hole (62) on the thrust plate (59). The outer end face of the thrust plate (59) is connected to a first connecting seat (63) arranged symmetrically on the upper and lower sides. The outer end face of the support base (60) is connected to a second connecting seat (64). A first support rod (65) is connected between the support base (60) and the thrust plate (59). The first support rod (65) is located on the thrust plate (59). In the middle of the side of the first support rod (65), a second support rod (66) is connected to the gap between the support base (60) and the thrust plate (59). The second support rod (66) is located on the bottom surface of the thrust plate (59). Several filter frames (67) and several filter plates (68) are attached to the first support rod (65). Filter paper (69) is installed between the filter frames (67) and the filter plates (68) to form a filter bed for filtering oil in the liquid. The filter bed is positioned by pressing the pressure plate (71). The outer end face of the pressure plate (71) is rotatably connected to the first lead screw (72). The first lead screw (72) is threadedly connected to the threaded seat (73), which is connected to the support base (60). The free end of the first lead screw (72) is connected to the handwheel (74). The bottom surfaces of the filter frames (67) and filter plates (68) abut against the second support rod (66).

6. The integrated extraction and oil removal equipment according to claim 2, characterized in that, The side wall of the first tank (24) is connected to a first branch pipe (85) and a second branch pipe (86). The first branch pipe (85) and the second branch pipe (86) are located above the first partition (35). A first tee pipe (87) is connected to the first branch pipe (85) and the second branch pipe (86). A second pipe seat (88) is connected to both ends of the first tee pipe (87). A pump body (89) is connected to the second pipe seat (88). The pump body (89) includes a first housing (90). The pump body (89) is installed inside the first housing (90). There is a right-angle seat (91), on which a rubber tube (92) is installed. One end of the rubber tube (92) is connected to a second tube seat (88). A triangular seat (93) is rotatably connected inside the first housing (90). A pressure roller (94) is rotatably connected to the triangular seat (93). The pressure roller (94) is used to squeeze the rubber tube (92). The triangular seat (93) is driven by a first motor (95). The opposite ends of the rubber tube (92) are connected through an eighth pipe (96) to form a material circulation and stirring channel.

7. The integrated extraction and oil removal equipment according to claim 2, characterized in that, The inner wall of the first tank (24) is rotatably connected to a third carrier plate (162). The third carrier plate (162) is connected to indexing rollers (163) arranged at equal angles. The indexing rollers (163) are driven by an arc cam (164). The arc cam (164) is located on a second bearing seat (165). The second bearing seat (165) is connected to the first tank (24). The arc cam (164) is driven by a seventh motor (166). The bottom surface of the third carrier plate (162) is connected to a vertical rod (167). The vertical rod (167) corresponds to the indexing rollers (163). The lower end of the vertical rod (167) is connected to a first spring (168). The lower end of the first spring (168) is connected to a slide tube (169). The bottom surface of the slide tube (169) is connected to a cleaning component (170).

8. The integrated extraction and oil removal equipment according to claim 7, characterized in that, The cleaning component (170) includes a second base plate (174) disposed on the slide tube (169). The second base plate (174) is arc-shaped. A third scraper (175) is hinged on the second base plate (174). A third spring (176) is connected at the angle between the second base plate (174) and the third scraper (175).

9. The integrated extraction and oil removal equipment according to claim 8, characterized in that, The first partition (35) is connected to a slag storage tank (177) on its side wall. The slag storage tank (177) is funnel-shaped. The side wall of the slag storage tank (177) has a slag inlet pipe (178). The port of the slag inlet pipe (178) has an inclined baffle (179). The top surface of the slag storage tank (177) has a return pipe (180). The lower end of the slag storage tank (177) is equipped with a discharge plug (181).

10. A process for preparing oil-free cerium carbonate using the integrated extraction and oil removal equipment according to any one of claims 1-9, characterized in that, Includes the following steps: a. Raw material pretreatment: Adjust the concentration of the mixed rare earth chloride solution to 250-350 g / L, filter it through a 0.5 μm precision filter, add hydrochloric acid to the filtrate to adjust the pH to 1.5-2.5, and obtain the pretreated solution; b. Extraction: The pretreated liquid is pumped into a multi-stage series extraction tank for multi-stage separation to obtain a high-purity cerium chloride solution; c. Multi-stage combined oil removal: The high-purity cerium chloride solution obtained in step b is sequentially filtered, activated carbon adsorbed, special resin adsorbed, and fiber deep filtered, with online monitoring and feedback to ensure that the oil content is ≤0.5ppm; d. Preparation of low-impurity precipitant: High-purity carbon dioxide and electronic-grade ammonia are reacted under controlled temperature and pressure to obtain an ammonium carbonate precipitant with an impurity content ≤0.5 ppm; e. Precise precipitation: Add the precipitant obtained in step d to the high-purity cerium chloride solution obtained in step c to carry out a staged precipitation reaction; f. Washing and dehydration: The precipitated product is centrifuged at high speed, washed with high-purity hot water, and then centrifuged at high speed to obtain the final product.

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