Method and equipment for rapid separation of organic substances in potassium chloride purification
By designing a scraping device and negative pressure-assisted adsorption in the potassium chloride production equipment, the problem of the inability to collect the extractant and organic matter enriched in the foam was solved, achieving efficient separation and resource recovery, reducing production costs, and improving product purity and production process stability.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- SHANDONG JIAOKELU MEIDA NEW MATERIAL TECH CO LTD
- Filing Date
- 2026-03-31
- Publication Date
- 2026-06-23
AI Technical Summary
During the potassium chloride production process, the extractant and organic matter enriched in the foam cannot be effectively collected, leading to resource waste and increased production costs. After the foam adheres to the inner wall for a long time, it forms a stubborn adhesion layer, affecting the separation and purification effect and the stability of the production process.
A rapid potassium chloride separation and purification device was designed. It adopts a scraping device including a scraping motor, scraping rods and a collection tank. Combined with negative pressure assisted adsorption, a double-layer scraping system is formed to completely remove foam from the inner wall of the tank, achieving all-round foam removal. Organic matter is completely separated through cyclone separation and demulsification sedimentation tank.
It achieves efficient removal of organic matter, improves resource recovery rate, reduces production costs, ensures the stability and continuity of the production process, improves product purity, enhances equipment operation reliability, and adapts to different processing volume requirements.
Smart Images

Figure CN122254531A_ABST
Abstract
Description
Technical Field
[0001] This invention belongs to the technical field of separating and purifying organic matter from potassium chloride, and particularly relates to a method and equipment for rapidly separating and purifying organic matter from potassium chloride. Background Technology
[0002] In the production of potassium chloride (KCl), especially during purification from potassium halite or carnallite, organic reagents such as flotation agents, inhibitors, and frothers are often introduced. These organic substances remain in the final potassium chloride product, affecting not only its whiteness and purity, leading to a decline in product grade, but more seriously, poisoning the electrolytic cell electrodes for subsequent production of high-value-added chemical raw materials such as potassium hydroxide and potassium chlorate, significantly reducing production efficiency and increasing production costs.
[0003] To deeply remove residual organic matter from potassium chloride, industrial processes often employ the addition of extractants. However, this process generates foam rich in organic extractants, which easily adheres to the inner wall of the processing chamber, leading to a series of adverse effects: First, the extractants and organic matter enriched in the foam cannot be effectively collected, resulting in resource waste and increased production costs; second, prolonged adhesion of the foam to the inner wall can cause demulsification, releasing organic matter and impurities that form a stubborn adhesion layer on the wall surface. This layer is not only difficult to clean but also contaminates subsequent processed materials, interfering with the separation and purification effect, causing fluctuations in product purity, and seriously affecting the stability and continuity of the production process. Based on this, a method and equipment for the rapid separation and purification of potassium chloride that can solve the above problems are proposed. Summary of the Invention
[0004] This invention provides a device for rapidly separating organic matter in the purification of potassium chloride, aiming to solve the problems of ineffective collection of extractant and organic matter enriched in foam, resulting in resource waste and increased production costs; and the demulsification phenomenon that occurs when foam adheres to the inner wall for a long time, releasing organic matter and impurities that form a stubborn adhesion layer on the wall surface, which is not only difficult to clean, but also contaminates subsequent processed materials, interferes with the separation and purification effect, causes fluctuations in product purity, and seriously affects the stability and continuity of the production process.
[0005] The application is achieved in the following manner. The device for quickly separating organic substances in potassium chloride purification comprises a main box body for reaction, a discharge port arranged at the lower end of the main box body, a first scraping unit arranged in the main box body for scraping foam, the first scraping unit comprising a plurality of scraping motors arranged in the main box body in a circumferential array, an output end of each scraping motor being fixedly connected with a scraping rod, an end of the scraping rod being fixedly connected with an elastic scraping head, a collecting groove arranged in the main box body, a plurality of circumferential array arranged weir plates being fixedly connected in the collecting groove, the collecting groove being divided into multiple sections by the weir plates, each section corresponding to a scraping section of the scraping motors, and a first collecting port arranged in the collecting groove, the first collecting port being connected with an external collecting device through a first collecting pipe for collecting the scraped foam for subsequent processing.
[0006] Preferably, the lower end of the main box body is fixedly connected with a base, an adding box body for adding an extracting agent is arranged on the main box body, and adjacent first connecting pipes are connected through connecting curved pipes.
[0007] Preferably, the upper end of the scraping motor is fixedly connected with a connecting block, the upper end of the connecting block being connected with the main box body through an elastic rod.
[0008] Preferably, the scraping rod comprises a scraping outer rod, the scraping outer rod being fixedly connected with the output end of the scraping motor, a slot being arranged in the scraping outer rod, a scraping inner rod being inserted in the slot, the scraping inner rod being fixedly connected with the elastic scraping head, guide blocks being fixedly connected on both sides of the scraping inner rod, guide rods being fixedly connected in the slot, the guide rods penetrating through the guide blocks, and the guide blocks being connected with the slot through springs for providing elasticity.
[0009] Preferably, a second scraping unit for scraping the scraping rod is arranged in the main box body.
[0010] Preferably, the second scraping unit includes multiple sets of scraping blocks arranged in a circumferential array and fixedly connected to the main housing. Each set of scraping blocks consists of two scraping blocks symmetrically arranged. The inward side of each scraping block is rotatably connected to a first rotating plate via a first rotating shaft, which is located at the upper end of the connection. A scraping pad is fixedly connected to the first rotating plate. A second rotating plate is rotatably connected to the first rotating plate via a second rotating shaft, which is located at the lower end of the connection. A torsion spring is provided on the outer side of the second rotating shaft. A collection groove is provided on each scraping block. A second collection port is provided on the main housing. The second collection port is connected to an external collection device via a second connecting pipe. The first connecting pipe and the second connecting pipe are connected via a third connecting pipe. Push rods corresponding to the positions of the second rotating plates are fixedly connected to both sides of the scraping block's outer rod.
[0011] Preferably, the scraper pad is made of solvent-resistant nitrile rubber.
[0012] Preferably, the main housing has multiple negative pressure ports on both sides of the weir plate, and the negative pressure ports are connected to the connecting curved pipe through a fourth connecting pipe.
[0013] A method for rapidly separating organic matter from potassium chloride during purification, comprising the following steps: Step 1: Slurry preparation and preheating: Crude potassium chloride containing organic matter is mixed with saturated potassium chloride mother liquor at a specific temperature at a certain solid-liquid ratio to form potassium chloride slurry, and then preheated; the saturated potassium chloride mother liquor is a circulating mother liquor in the system that has had organic matter removed; Step 2: Coupled extraction-flotation: The preheated slurry is fed into the coupled extraction-flotation device, while microbubbles and a specific green extractant are introduced into the device. Step 3: Cyclone Separation and Enrichment: The gas-liquid-solid three-phase mixture discharged from the coupled extraction-flotation device enters a high-efficiency hydrocyclone; under the action of a strong centrifugal force field, the denser pure potassium chloride crystals and saturated mother liquor are discharged from the underflow outlet, while the less dense "bubble-extractant-organic matter" complex and a small amount of liquid are discharged from the overflow outlet, achieving one-time high-efficiency enrichment of organic matter; Step 4: Demulsification and phase separation: The overflow product obtained in Step 3 is sent to the demulsification settling tank. By adjusting the pH value or adding a small amount of demulsifier, the emulsion that may be formed is destroyed, so that the extractant phase (rich in organic matter), aqueous phase and gas phase are completely separated. The remaining mixed raw materials in the tank are removed by the scraping device. Step 5: Extractant regeneration and organic matter recovery: The separated organic-rich extractant enters a vacuum distillation unit for low-temperature distillation. Volatile organic matter is condensed and recovered as distillate, while the regenerated pure extractant is returned to Step 2 for recycling. Step Six: Product Post-processing: The pure potassium chloride slurry discharged from the underflow outlet in Step Three is dehydrated and dried to obtain a high-purity potassium chloride product; most of the separated mother liquor is returned to Step One for recycling, and a small portion is discharged from the system to control the concentration of impurity ions.
[0014] Compared with the prior art, the embodiments of this application have the following advantages: high separation efficiency and thorough removal of organic matter: the first scraping unit comprehensively scrapes the foam on the inner wall of the box, and the second scraping unit cleans the scraping rods in a targeted manner, forming a double-layer scraping system. With the help of negative pressure adsorption, all-round foam removal of "box wall - scraping rods - collection tank inner wall" is achieved, with a foam scraping efficiency of over 98%, effectively solving the problem of product purity reduction caused by organic matter residue.
[0015] Full resource recovery reduces production costs: The independent collection area and double-layer collection pipeline design ensure that extractant foam rich in organic matter is collected without any leakage. The filter screen design reduces the entrainment of potassium chloride fine crystals, and the extractant recovery rate is increased to over 95%, avoiding resource waste. The precise feeding design of the addition box reduces the ineffective consumption of extractant, further reducing operating costs.
[0016] Stable and reliable operation with strong adaptability: The telescopic buffer structure of the scraping rod and the axial compensation design of the elastic rod can adapt to the slight deformation of the inner wall of the box and the changes in foam thickness under different working conditions; the shock absorption and noise reduction design of the base and the selection of solvent-resistant and wear-resistant materials for key components ensure that the noise of the equipment is below 85dB during continuous operation and the service life is extended to 8-12 months, adapting to different processing volume requirements in laboratories and industrial settings.
[0017] Convenient operation and maintenance, ensuring continuous production: The design of drawer-type detachable filter screen and quick-connect pipeline facilitates regular cleaning and component replacement; the maintenance channel reserved in the base makes it convenient for operators to maintain the discharge port and valves; the automated linkage control of the equipment reduces manual intervention, avoids production interruptions caused by foam accumulation and demulsification, and ensures the continuity and stability of the purification process.
[0018] Environmentally friendly and pollution-free, enhancing product quality: The closed-loop collection design throughout the entire process avoids internal wall contamination and secondary material contamination caused by foam demulsification, ensuring the stable purity of potassium chloride products; no additional pollutants are generated, and the recovered organic matter can be reused, meeting clean production requirements and supporting the subsequent production of high value-added chemical products. Attached Figure Description
[0019] Figure 1 This is a schematic diagram of the overall structure of an apparatus for rapidly separating and purifying organic matter in potassium chloride, provided by the present invention. Figure 2This is a schematic diagram of the internal structure of the main casing in an apparatus for rapidly separating and purifying organic matter in potassium chloride, provided by the present invention. Figure 3 yes Figure 1 Enlarged structural diagram at point A; Figure 4 This is a schematic diagram of the internal structure of an apparatus for rapidly separating and purifying organic matter in potassium chloride, provided by the present invention. Figure 5 yes Figure 4 Enlarged structural diagram at point B; Figure 6 This is a schematic diagram of the overall structure of the second scraping unit in the device for rapid separation and purification of organic matter in potassium chloride provided by the present invention; Figure 7 yes Figure 6 Enlarged structural diagram at point C; Figure 8 This is a cross-sectional structural diagram of the scraping rod in an apparatus for rapidly separating and purifying organic matter in potassium chloride, provided by the present invention.
[0020] Figure reference numerals: 1. Main housing; 2. Scraping motor; 3. Elastic scraper head; 4. Collection trough; 5. Weir plate; 6. First collection port; 7. First collection pipe; 8. Base; 9. Adding housing; 10. Connecting curved pipe; 11. Connecting block; 12. Elastic rod; 13. Outer scraper rod; 14. Slot; 15. Inner scraper rod; 16. Guide block; 17. Guide rod; 18. Spring; 19. Scraper block; 20. First rotating shaft; 21. First rotating plate; 22. Scraper pad; 23. Second rotating shaft; 24. Second rotating plate; 25. Collection curved trough; 26. Second collection port; 27. Second connecting pipe; 28. Third connecting pipe; 29. Negative pressure port; 30. Fourth connecting pipe; 31. Push rod. Detailed Implementation
[0021] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs; the terminology used herein in the specification of the application is for the purpose of describing particular embodiments only and is not intended to be limiting of the application; the terms "comprising" and "having," and any variations thereof, in the specification, claims, and foregoing drawings of this application are intended to cover non-exclusive inclusion. The terms "first," "second," etc., in the specification, claims, or foregoing drawings of this application are used to distinguish different objects, not to describe a particular order.
[0022] In this document, the term "embodiment" means that a particular feature, structure, or characteristic described in connection with an embodiment may be included in at least one embodiment of this application. The appearance of this phrase in various places throughout the specification does not necessarily refer to the same embodiment, nor is it a separate or alternative embodiment mutually exclusive with other embodiments. It will be explicitly and implicitly understood by those skilled in the art that the embodiments described herein can be combined with other embodiments.
[0023] This invention provides a method for rapidly separating organic matter from potassium chloride during purification, the steps of which include: Step 1: Slurry preparation and preheating: Crude potassium chloride containing organic matter is mixed with saturated potassium chloride mother liquor at a specific temperature at a certain solid-liquid ratio to form potassium chloride slurry, and then preheated; the saturated potassium chloride mother liquor is the mother liquor that has been circulated in the system and has had organic matter removed. Step 2: Coupled extraction-flotation: The preheated slurry is fed into the coupled extraction-flotation device, while microbubbles and a specific green extractant are introduced into the device. Step 3: Cyclone Separation and Enrichment: The gas-liquid-solid three-phase mixture discharged from the coupled extraction-flotation device enters a high-efficiency hydrocyclone; under the action of a strong centrifugal force field, the denser pure potassium chloride crystals and saturated mother liquor are discharged from the underflow outlet, while the less dense "bubble-extractant-organic matter" complex and a small amount of liquid are discharged from the overflow outlet, achieving one-time high-efficiency enrichment of organic matter; Step 4: Demulsification and phase separation: The overflow product obtained in Step 3 is sent to the demulsification settling tank. By adjusting the pH value or adding a small amount of demulsifier, the emulsion that may be formed is destroyed, so that the extractant phase (rich in organic matter), aqueous phase and gas phase are completely separated. The remaining mixed raw materials in the tank are removed by the scraping device. Step 5: Extractant regeneration and organic matter recovery: The separated organic-rich extractant enters a vacuum distillation unit for low-temperature distillation. Volatile organic matter is condensed and recovered as distillate, while the regenerated pure extractant is returned to Step 2 for recycling. Step Six: Product Post-processing: The pure potassium chloride slurry discharged from the underflow outlet in Step Three is dehydrated and dried to obtain a high-purity potassium chloride product; most of the separated mother liquor is returned to Step One for recycling, and a small portion is discharged from the system to control the concentration of impurity ions.
[0024] The following is an example of extraction during the entire process: The crude potassium chloride to be processed contains 0.15% organic matter (as TOC).
[0025] S1. In the slurry preheating tank, 1 ton of crude potassium chloride is mixed with 3 cubic meters of saturated potassium chloride mother liquor (temperature 60℃) and preheated to 55℃.
[0026] S2. Pump the slurry into the coupled extraction-flotation device, while simultaneously introducing air (bubble diameter 10-50μm) through a micro-nano bubble generator, and pumping in tributyl citrate as a green extractant at a flow rate of 50L / h. Stir at 300rpm and retain for 15 minutes.
[0027] S3. The reaction mixture enters a high-efficiency hydrocyclone with an inlet pressure of 0.3 MPa. The underflow is pure potassium chloride slurry, and the overflow is rich in organic phase.
[0028] S4. Overflow into the demulsification settling tank, let stand for 30 minutes, and clear stratification will occur.
[0029] S5. The organic-rich tributyl citrate in the upper layer enters the vacuum distillation unit (temperature 100℃, vacuum degree -0.08MPa). The distillate is the recovered organic matter, and the tributyl citrate regenerated at the bottom of the vessel is returned to S2 for use.
[0030] S6. The potassium chloride slurry from the underflow is centrifuged, dehydrated, and then dried in a fluidized bed to obtain the finished potassium chloride product. Testing showed that the organic matter content in the product was reduced to below 0.01%, and the whiteness was significantly improved. The extractant recovery rate was greater than 98%, and the organic matter recovery rate was greater than 90%.
[0031] Synergistic and Innovative Process: This invention creatively couples two unit operations, "solvent extraction" and "bubble flotation," within the same device. The extractant is responsible for "dissolving" and "stripping" organic matter from the crystals, while microbubbles are responsible for "capturing" and "carrying" the organic matter enriched by the extractant. The two work synergistically to achieve deep and efficient removal of organic matter adhering to the surface and encapsulated in the crystal lattice, breaking through the limitations of single technologies.
[0032] The equipment has a novel structure: the core of this invention is a specially designed "coupled extraction-flotation device". By integrating a micro-nano bubble generator and an extractant dispersion system, it completes the complex separation process that traditionally requires multiple devices in one device, simplifying the process and reducing equipment investment and floor space.
[0033] High efficiency, energy saving, and resource recycling: Energy saving: The entire process is carried out in a saturated potassium chloride solution, which avoids the loss of potassium chloride due to dissolution, and the operating temperature is much lower than that of the calcination method, resulting in a significant reduction in energy consumption.
[0034] Resource recovery: Extractant and organic matter are recovered through vacuum distillation. The extractant can be recycled, reducing operating costs. The recovered organic matter can be used as chemical raw materials or fuel, realizing the resource utilization of waste and avoiding secondary pollution.
[0035] Effectiveness: The introduction of the hydrocyclone separator enhances the separation efficiency by utilizing centrifugal force, enabling the pure potassium chloride product to be quickly and thoroughly separated from the organic-rich phase, thus ensuring the high purity of the final product.
[0036] Environmentally friendly: The entire process is a physical separation process, which does not involve strong oxidants or produce toxic gases. The closed-loop circulation system greatly reduces wastewater discharge, making it a clean production technology. Please combine Figures 1-8 In one embodiment, an apparatus for rapidly separating organic matter in potassium chloride purification includes a scraping device comprising: a main housing 1, which is integrally formed from 304 stainless steel, with the inner wall polished (surface roughness Ra≤0.8μm) to reduce foam adhesion points; the volume is adapted according to the processing capacity (100-500L for laboratory equipment, 5-20m³ for industrial equipment) to ensure that the foam generation area is concentrated in the upper part of the housing, facilitating coverage by the scraping unit.
[0037] An inclined guide plate (30° to the horizontal) is installed at the discharge port at the lower end of the chamber to prevent the accumulation of potassium chloride slurry during the scraping process, which could then be used for reaction. Inside, there is a first scraping unit for removing foam. This first scraping unit includes a scraping motor 2, which is an explosion-proof geared motor. The power is adapted to the equipment scale (50-100W for laboratory equipment, 300-500W for industrial equipment). The speed can be adjusted via a frequency converter (5-15 r / min) to adapt to different foam generation amounts: when the foam layer thickness is ≥25mm, the speed automatically increases to 12-15 r / min; when the foam layer thickness is ≤10mm, the speed decreases to 5-8 r / min. Multiple scraping motors 2 are arranged in a circular array within the main chamber 1. The output end of each scraping motor 2 is fixedly connected to... The scraping rod has an elastic scraper head 3 fixedly connected to its end. The elastic scraper head 3 is integrally molded from solvent-resistant nitrile rubber (NBR) or fluororubber (FKM) with a Shore hardness of 50-60A, combining elasticity and wear resistance. The scraper head is arc-shaped with a radius of curvature that perfectly matches the inner wall of the box. The scraping surface width is 30-50mm, ensuring full contact with the inner wall. A collection trough 4 is located inside the main box 1. Multiple circumferentially arrayed weir plates 5 are fixedly connected inside the collection trough 4. The weir plates 5 are made of 304 stainless steel, with a height of 40mm. The bottom is welded to the bottom of the collection trough 4, and the top is rounded. Multiple weir plates 5 are evenly distributed along the circumference of the collection trough 4, dividing the collection trough 4 into 3-4 independent areas. Each area corresponds to the scraping range of one scraping motor 2, preventing foam from mixing and accumulating in different areas.
[0038] Combination Figure 3The correspondence between the weir plate 5 and the scraping unit: the center of each independent collection area coincides with the axis of the corresponding scraping motor 2, and the area width is slightly larger than the scraping coverage of the scraper head (leaving a 10mm margin on one side) to ensure that the scraped foam can fall completely into the corresponding area without any omissions. Multiple weir plates 5 divide the collection tank 4 into multiple sections, and each section corresponds to the scraping section of multiple scraping motors 2, as well as the first collection port 6. The first collection port 6 is set in the collection tank 4 and is connected to an external collection device through the first collection pipe 7. It is used to collect the scraped foam for further processing. A removable filter screen (50μm pore size) is installed in the collection port to filter out the potassium chloride fine crystals entrained in the foam. The filter screen edge is equipped with a sealing gasket to prevent unfiltered foam from leaking out. The filter screen adopts a drawer-type design, which is convenient to remove and clean regularly to avoid clogging.
[0039] A base 8 is fixedly connected to the lower end of the main housing 1. The base 8 at the lower end of the main housing 1 adopts a welded steel frame structure (material Q235 carbon steel, surface sprayed with epoxy anti-rust paint). The frame height is 300-500mm (suitable for industrial equipment). The bottom is fixed to the ground with expansion bolts to ensure the stability of the equipment during operation. Four to six shock-absorbing rubber pads (diameter 100mm, thickness 50mm, Shore hardness 60A) are set between the base 8 and the main housing 1 to absorb the vibration generated by the scraper motor 2 and reduce the noise of the equipment (noise controlled below 85dB). The base 8 frame has a reserved maintenance channel with a width of ≥600mm, facilitating maintenance of the discharge port and valves at the lower end of the main housing 1 by operators. The main housing 1 is equipped with an addition tank 9 for adding extractant. The addition tank 9 is a cylindrical container (made of 304 stainless steel) with a volume of 50-200L, fixed to the side wall of the main housing 1 by a bracket (at 2 / 3 of the height of the main housing 1). The top of the tank has a filling port with a sealed cap, and the bottom is connected to the main housing 1 via a second connecting pipe 27. A flow meter (accuracy ±2%) and a solenoid valve are installed sequentially on the second connecting pipe 27. The extractant addition amount (flow range 0.5-5L / h) can be precisely adjusted by a PLC control system to achieve dynamic matching with the foam generation amount (when the foam level sensor detects that the foam layer thickness is less than 10mm, the addition amount is automatically reduced by 10%-15%). Adjacent first connecting pipes are connected by a connecting curved pipe 10.
[0040] A connecting block 11 is fixedly connected to the upper end of the scraping motor 2, and the upper end of the connecting block 11 is connected to the main housing 1 through a spring rod 12.
[0041] Combination Figure 8The scraping rod includes an outer scraping rod 13, which is fixedly connected to the output end of the scraping motor 2. A slot 14 is provided inside the outer scraping rod 13, and an inner scraping rod 15 is inserted into the slot 14. The inner scraping rod 15 is fixedly connected to the elastic scraping head 3. Guide blocks 16 are fixedly connected to both sides of the inner scraping rod 15. A guide rod 17 is fixedly connected to the slot 14, and the guide rod 17 passes through the guide block 16. The guide block 16 is connected to the slot 14 through a spring 18 for providing elasticity. When the scraping head is subjected to force, the inner rod compresses the spring 18 and retracts into the slot 14 to achieve radial buffering (maximum shrinkage of 20mm), adapting to small deformations or local protrusions of the inner wall. Furthermore, the spring 18 can be adapted to different speeds, facilitating the scraping of foam of different thicknesses.
[0042] The main housing 1 is equipped with a second scraping unit for scraping the scraping rod.
[0043] Combination Figure 5 , Figure 6 and Figure 7The second scraping unit includes multiple sets of scraper blocks 19 arranged in a circular array, fixedly connected inside the main housing 1. The scraper blocks 19 are made of 304 stainless steel, and each set consists of two symmetrically arranged right-angled trapezoidal blocks (upper base 50mm, lower base 80mm, height 100mm), which are fixed to the inner wall of the main housing 1 by bolts and located below the first scraping unit (300-500mm from the bottom of the collection tank 4). Each set of scraper blocks 19 consists of two symmetrically arranged scraper blocks 19. The inward-facing side of the scraper block 19 is rotatably connected to a first rotating plate 21 via a first rotating shaft 20. The first rotating shaft 20 is located at... At the upper end of the connection, a scraper pad 22 is fixedly connected to the first rotating plate 21. A second rotating plate 24 is rotatably connected to the first rotating plate 21 via a second rotating shaft 23. The second rotating shaft 23 is located at the lower end of the connection. A torsion spring is provided on the outer side of the second rotating shaft 23. A collection groove 25 is provided on the scraper block 19. The collection groove 25 (semi-circular cross-section, 30mm in diameter) is integrally formed on the lower inner side of the scraper block 19. The groove extends from the top end of the scraper block 19 to the bottom end. The bottom of the groove is inclined towards the inner wall of the main box 1 (slope 5°). The end of the groove is connected to the second collection port 26 on the inner wall of the main box 1. The inner wall of the curved groove is coated with a polytetrafluoroethylene coating (0.1mm thick) to reduce the adhesion of the scraped material and ensure that the residual foam scraped from the scraping rod can flow smoothly into the second collection port 26 along the curved groove. The main body 1 has a second collection port 26, which is connected to an external collection device through a second connecting pipe 27. The first connecting pipe and the second connecting pipe 27 are connected through a third connecting pipe 28. Push rods 31 corresponding to the positions of the second rotating plate 24 are fixedly connected to both sides of the scraping rod 13. When the scraping rod moves the push rod 31 to the position of the second rotating plate 24, the push rod 31 pushes the second rotating plate 24 to rotate around the second rotating shaft 23. While compressing the torsion spring, it drives the first rotating plate 21 to rotate inward around the first rotating shaft 20, so that the scraping pad 22 gradually adheres to the surface of the scraping rod (contact pressure 5-8N). As the rod continues to move, the push rod 31 disengages from the second rotating plate 24, the torsion spring resets, and the two rotating plates return to their initial positions, completing one scraping action.
[0044] The material of the scraper pad 22 is solvent-resistant nitrile rubber.
[0045] The main housing 1 has multiple negative pressure ports 29 on both sides of the weir plate 5. These ports 29 are connected to the connecting curved pipe 10 via a fourth connecting pipe 30 (12mm inner diameter, PTFE material). The negative pressure ports 29 are collected and connected to the connecting curved pipe 10, utilizing the negative pressure (-0.01 to -0.015MPa) within the connecting curved pipe 10 to create a synergistic suction. An adjusting valve is installed on the fourth connecting pipe 30 to individually control the suction of each negative pressure port 29 area (adjusting the suction to -0.015MPa in the edge area and -0.01MPa in the center area), preventing excessive local suction from causing foam breakage. The negative pressure system is linked to a foam level sensor; when foam stagnation is detected in the collection tank 4, the corresponding negative pressure value is automatically increased by 5%-10%.
[0046] In summary, the working principle of this invention is as follows: During the reaction and material supply stage: crude potassium chloride containing residual organic matter reacts fully with the extractant precisely delivered by the addition tank 9 within the main tank 1, generating foam rich in organic extractant. The foam naturally rises to the upper part of the main tank 1. The addition tank 9 is linked to a foam level sensor via a PLC control system, dynamically adjusting the amount of extractant added based on the foam layer thickness to ensure that the reaction rate matches the amount of foam generated.
[0047] The first scraping and initial collection stage: Multiple scraping motors 2, arranged in a circular array, are activated. The scraping rods at their output ends drive the elastic scraper heads 3 to rotate. The elastic scraper heads 3, through their arc-shaped structure, fit tightly against the inner wall of the box, scraping away the foam adhering to the wall surface. The scraped foam falls into independent collection areas separated by weir plates 5 below, and converges along the gradient slope of the bottom wall of the collection trough 4 to the first collection port 6. After being filtered through a filter screen to obtain fine potassium chloride crystals, it is transported to an external collection device through the first collection pipe 7. The speed of the scraping motors 2 can be adaptively adjusted according to the thickness of the foam layer. Simultaneously, the telescopic structure of the scraping rods is buffered by springs 18, adapting to minor deformations of the inner wall and the scraping requirements of foams of varying thicknesses.
[0048] The second scraping and secondary collection stage: During the movement of the scraping rod, the push rods 31 on both sides synchronously push the second rotating plate 24, which drives the first rotating plate 21 to rotate inward through the torsion spring transmission. This causes the scraping pad 22 to fit tightly against the surface of the scraping rod, scraping off the foam residue adhering to the rod. The scraped residue flows into the second collection port 26 along the collection groove 25 on the scraper block 19. After merging with the first connecting pipe through the second connecting pipe 27, it enters the external collection device together, achieving thorough cleaning without dead angles.
[0049] Negative pressure assisted and coordinated collection stage: The negative pressure ports 29 on both sides of the weir plate 5 of the main tank 1 are connected to the connecting curved pipe 10 through the fourth connecting pipe 30, forming a coordinated suction force of -0.01 to -0.015 MPa to adsorb the fine foam remaining on the inner wall of the collection tank 4 and avoid foam retention and accumulation. The negative pressure system can dynamically adjust the suction force of each area according to the feedback of the foam liquid level sensor to ensure collection efficiency while preventing foam breakage.
[0050] Material discharge and stable equipment operation: The purified potassium chloride slurry is discharged through the discharge port at the lower end of the main tank 1. The shock-absorbing rubber pads of the base 8 absorb the vibration of the equipment during operation, ensuring overall stability. The wear-resistant and solvent-resistant materials of each component are adapted to the reaction environment, extending the continuous operation time of the equipment. The above are merely preferred embodiments of the present invention and are not intended to limit the present invention. 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. A method for rapidly separating organic matter from potassium chloride during purification, characterized in that, The steps include: Step 1: Slurry preparation and preheating: Crude potassium chloride containing organic matter is mixed with saturated potassium chloride mother liquor at a specific temperature at a certain solid-liquid ratio to form potassium chloride slurry, and then preheated; the saturated potassium chloride mother liquor is a circulating mother liquor in the system that has had organic matter removed; Step 2: Coupled extraction-flotation: The preheated slurry is fed into the coupled extraction-flotation device, while microbubbles and a specific green extractant are introduced into the device. Step 3: Cyclone Separation and Enrichment: The gas-liquid-solid three-phase mixture discharged from the coupled extraction-flotation device enters a high-efficiency hydrocyclone; under the action of a strong centrifugal force field, the denser pure potassium chloride crystals and saturated mother liquor are discharged from the underflow outlet, while the less dense "bubble-extractant-organic matter" complex and a small amount of liquid are discharged from the overflow outlet, achieving one-time high-efficiency enrichment of organic matter; Step 4: Demulsification and phase separation: The overflow product obtained in Step 3 is sent to the demulsification settling tank. By adjusting the pH value or adding a small amount of demulsifier, the emulsion that may be formed is destroyed, so that the extractant phase (rich in organic matter), aqueous phase and gas phase are completely separated. The remaining mixed raw materials in the tank are removed by the scraping device. Step 5: Extractant regeneration and organic matter recovery: The separated organic-rich extractant enters a vacuum distillation unit for low-temperature distillation. Volatile organic matter is condensed and recovered as distillate, while the regenerated pure extractant is returned to Step 2 for recycling. Step Six: Product Post-processing: The pure potassium chloride slurry discharged from the underflow outlet in Step Three is dehydrated and dried to obtain a high-purity potassium chloride product; most of the separated mother liquor is returned to Step One for recycling, and a small portion is discharged from the system to control the concentration of impurity ions.
2. A device for rapidly separating organic matter in potassium chloride purification, characterized in that, Using the scraping device as described in claim 1, the scraping device comprises: The main chamber (1) is used for the reaction to occur. It has a discharge port at its lower end and a first scraping unit for scraping off foam inside. The first scraping unit includes: A scraping motor (2) is provided, and the number of scraping motors (2) is multiple, and the multiple scraping motors (2) are arranged in a circumferential array inside the main housing (1). The output end of the scraping motor (2) is fixedly connected to a scraping rod, and the end of the scraping rod is fixedly connected to an elastic scraper head (3). A collection trough (4) is disposed inside the main housing (1). Multiple weir plates (5) arranged in a circular array are fixedly connected inside the collection trough (4). The multiple weir plates (5) divide the collection trough (4) into multiple segments, each segment corresponding to a scraping segment of a multiple scraping motor (2). The first collection port (6) is located in the collection tank (4) and is connected to an external collection device through the first collection pipe (7) for collecting the scraped foam for further processing.
3. The method and equipment for rapid separation and purification of organic matter in potassium chloride as described in claim 2, characterized in that, The lower end of the main box (1) is fixedly connected to a base (8), and an addition box (9) for adding extractant is provided on the main box (1). Adjacent first connecting pipes are connected by connecting curved pipes (10).
4. The method and equipment for rapid separation and purification of organic matter in potassium chloride as described in claim 2, characterized in that, The upper end of the scraping motor (2) is fixedly connected to a connecting block (11), and the upper end of the connecting block (11) is connected to the main housing (1) through a spring rod (12).
5. The method and apparatus for rapid separation and purification of organic matter in potassium chloride as described in claim 4, characterized in that, The scraping rod includes an outer scraping rod (13), which is fixedly connected to the output end of the scraping motor (2). A slot (14) is provided inside the outer scraping rod (13), and an inner scraping rod (15) is inserted into the slot (14). The inner scraping rod (15) is fixedly connected to the elastic scraper head (3). Guide blocks (16) are fixedly connected to both sides of the inner scraping rod (15). A guide rod (17) is fixedly connected inside the slot (14). The guide rod (17) passes through the guide block (16), and the guide block (16) is connected to the slot (14) by a spring (18) for providing elasticity.
6. The method and apparatus for rapid separation and purification of organic matter in potassium chloride as described in claim 4, characterized in that, The main housing (1) is provided with a second scraping unit for scraping the scraping rod.
7. The method and apparatus for rapid separation and purification of organic matter in potassium chloride as described in claim 6, characterized in that, The second scraping unit includes multiple sets of scraping blocks (19) arranged in a circumferential array and fixedly connected inside the main housing (1). Each set of scraping blocks (19) consists of two scraping blocks (19) arranged symmetrically. The inward side of each scraping block (19) is rotatably connected to a first rotating plate (21) via a first rotating shaft (20). The first rotating shaft (20) is located at the upper end of the connection. A scraping pad (22) is fixedly connected to the first rotating plate (21). A second rotating plate (24) is rotatably connected to the first rotating plate (21) via a second rotating shaft (23). The rotating shaft (23) is located at the lower end of the connection. A torsion spring is provided on the outer side of the second rotating shaft (23). A collection groove (25) is provided on the scraper (19). A second collection port (26) is provided on the main box (1). The second collection port (26) is connected to an external collection device through a second connecting pipe (27). The first connecting pipe and the second connecting pipe (27) are connected through a third connecting pipe (28). Push rods (31) corresponding to the positions of the second rotating plate (24) are fixedly connected to both sides of the scraper's outer rod (13).
8. The method and apparatus for rapid separation and purification of organic matter in potassium chloride as described in claim 7, characterized in that, The scraper pad (22) is made of solvent-resistant nitrile rubber.
9. The method and equipment for rapid separation and purification of organic matter in potassium chloride as described in claim 2, characterized in that, The main box (1) has multiple negative pressure ports (29) on both sides of the weir plate (5), and the negative pressure ports (29) are connected to the connecting curved pipe (10) through the fourth connecting pipe (30).