An o-sulfonic acid separation apparatus based on cooling crystallization

Abstract

The present application relates to the technical field of crystallization separation, and particularly relates to a cooling crystallization-based o-sulfonic acid separation device, which comprises a crystallization separation kettle, the inside of the crystallization separation kettle is provided with a ring-shaped crystallization bin, and the device further comprises a ring-shaped clamping block which is circumferentially arranged outside the side wall of the crystallization separation kettle and is uniformly provided with a plurality of horizontal guide grooves in the middle in a circumferential manner. The cooling crystallization plate slides along the horizontal guide grooves of the ring-shaped clamping block, when the plate body slides into the kettle, the low-temperature surface of the plate body induces the crystallization and precipitation of o-sulfonic acid in the liquid, when the plate body slides outwards, the elastic scraper automatically scrapes off the crystalline substances adhered to the surface of the plate body, prevents scaling, and the volume area of the cooling crystallization plate in the ring-shaped crystallization bin is adjusted by sliding to adjust the cooling speed, solves the problems of temperature control lag and scaling of the cooling surface of the traditional device, realizes efficient, continuous and low-consumption operation of the o-sulfonic acid crystallization process, and greatly improves the product purity and production efficiency.

Description

Technical Field

[0001] This invention relates to the field of crystallization separation technology, and in particular to a separation device for o-sulfonic acid based on cooling crystallization. Background Technology

[0002] o-Synovial acid, as an important class of organic sulfonic acid compounds, is a key intermediate in the synthesis of dyes, pharmaceutical raw materials, and fine chemicals such as pesticides. Furthermore, o-sulfonic acid is a key precursor in the production of DSD acid, and the quality and efficiency of its preparation process directly determine the performance and production capacity of DSD acid products. During its industrial production, a large amount of inorganic sulfuric acid byproducts are often generated, forming a complex mixture of o-sulfonic acid and sulfuric acid. Therefore, the efficient and economical separation and purification of the target o-sulfonic acid from the sulfuric acid mixture has become a core technical challenge for improving the quality of pharmaceutical-grade products, reducing production costs, and realizing resource utilization. The cooling crystallization method based on solubility differences is widely considered a potential separation method suitable for application in the manufacturing of raw materials and formulations due to its simple operation and good results.

[0003] In the separation process based on cooling crystallization, the core equipment needs to achieve precise and rapid control of the feed liquid temperature to induce the preferential supersaturation precipitation of the target o-sulfonic acid and form easily separable crystals. However, the temperature control accuracy and response speed of existing crystallization equipment are insufficient, and the cooling pipes are generally used as the main cold source interface, which has the lowest surface temperature and is very easy to become the primary nucleation point. The precipitated crystals firmly adhere to the metal pipe wall to form a hard scale layer, which not only drastically reduces the heat transfer efficiency and increases energy consumption, but also forces the equipment to be shut down frequently for cleaning, greatly reducing production continuity and increasing maintenance costs and operational risks. Summary of the Invention

[0004] In view of this, the purpose of this invention is to propose an o-sulfonic acid separation device based on cooling crystallization, in order to solve the problem that current o-sulfonic acid separation devices use cooling pipes as the main cold source interface, resulting in crystals that firmly adhere to the metal pipe wall to form a hard scale layer, which reduces heat transfer efficiency, increases energy consumption, requires frequent shutdowns for cleaning, and leads to a decrease in overall production efficiency.

[0005] To achieve the above objectives, the present invention provides a cooling crystallization-based o-sulfonic acid separation device, comprising a crystallization separation vessel, wherein the crystallization separation vessel is provided with an annular crystallization chamber, and further comprising: A ring-shaped clamping block is arranged around the outside of the side wall of the crystallization separation vessel. Multiple horizontal guide grooves are evenly arranged in the middle of the ring-shaped clamping block in a circular shape. The inner end of the horizontal guide groove penetrates the side wall of the crystallization separation vessel and is provided with a cleaning opening. Elastic scrapers are symmetrically arranged on the left and right sides of the cleaning opening. A cooling crystallization plate is fitted and slidably disposed inside the horizontal guide groove. A hollow flow guide chamber is provided inside the cooling crystallization plate. Cooling inlet and cooling outlet are respectively connected to the upper and lower sides of the outer end of the hollow flow guide chamber. A central conveying cylinder is vertically positioned at the center of the annular crystallization chamber. The bottom and top of the side wall of the central conveying cylinder are respectively provided with an input opening and an output opening. A conveying turbine is fitted and rotated at the center of the interior of the central conveying cylinder. A ring-shaped circulating filter plate is fitted and slidably disposed outside the input opening at the bottom of the central conveying cylinder. A central discharge cylinder is connected to the bottom of the central conveying cylinder. A separation discharge port is provided on the side wall of the central discharge cylinder. A sliding sealing plate is fitted and slidably disposed in the middle of the central discharge cylinder.

[0006] Furthermore, a horizontal adjustment frame is provided above the cooling crystallization plate, a translation guide rail is provided in the middle of the horizontal adjustment frame, a translation adjustment screw is provided parallel to the outer side of the translation guide rail, a translation adjustment motor is connected to the shaft end of the translation adjustment screw, a horizontal traction slider is slidably provided in the middle of the translation guide rail, an adjustment sleeve is provided in the middle of the horizontal traction slider, the horizontal traction slider is connected to the translation adjustment screw through the adjustment sleeve, and an adjustment traction frame is provided at the outer end of the cooling crystallization plate, the horizontal traction slider is connected to the adjustment traction frame.

[0007] Furthermore, symmetrical horizontal translation guide rods are arranged on the left and right sides of the outer end of the horizontal guide groove, and symmetrical translation sliding sleeves are arranged on the left and right sides of the adjusting traction frame. The adjusting traction frame is slidably connected to the translation guide rods through the translation sliding sleeves.

[0008] Furthermore, an annular guide rail is arranged around the top of the annular clamping block, and the horizontal adjustment frame is slidably connected to the annular guide rail. The horizontal adjustment frame is slidably and rotatably arranged around the crystallization separation vessel via the annular guide rail. A rotary traction block is connected below the horizontal traction slider. A rotary traction slot is provided in the middle of the top of the adjustment traction frame. The rotary traction slot and the rotary traction block are mutually engaged. A rotary adjustment motor is provided at the bottom of the horizontal adjustment frame. A rotary adjustment gear is connected to the shaft end of the rotary adjustment motor. An adjustment gear ring is arranged around the middle of the annular guide rail. The rotary adjustment gear and the adjustment gear ring are mutually meshed.

[0009] Furthermore, multiple conveying baffles are uniformly and parallelly arranged in the vertical direction inside the hollow flow guide chamber, and conveying openings are provided on the opposite side of adjacent conveying baffles. Horizontal telescopic pipes are connected to the outer ends of both the cooling inlet and the cooling outlet, and the outer ends of both the cooling inlet and the cooling outlet are connected to the annular cooler through the horizontal telescopic pipes.

[0010] Furthermore, the annular cooler has multiple cooling fins arranged evenly and parallel in the vertical direction in the middle, and multiple vertical conveying pipes are embedded in the middle of the cooling fins. The upper and lower ends of the vertical conveying pipes are respectively provided with an annular input pipe and an annular output pipe. A circulating conveying pump is provided in the middle of the annular input pipe. The outer ends of the cooling input port and the cooling output port are respectively connected to the annular input pipe and the annular output pipe through horizontal telescopic pipes.

[0011] Furthermore, the horizontal telescopic tube includes a fixed sleeve and a sliding sleeve. The sliding sleeve is fitted and slidably disposed inside the fixed sleeve. The inner end of the sliding sleeve is connected to a cooling inlet or a cooling outlet. The outer end of the fixed sleeve is connected to an annular inlet or an annular outlet. A sliding sealing ring is arranged around the inner end opening of the fixed sleeve. An annular conveying chamber is provided in the middle of the side wall of the fixed sleeve. Multiple conveying openings are evenly arranged in the horizontal direction in the middle of the inner wall of the fixed sleeve. The conveying openings are connected to the annular inlet or annular outlet through the annular conveying chamber.

[0012] Furthermore, a vertical washing pipe is vertically arranged on the inner side of the elastic scraper, and multiple washing nozzles are evenly arranged on the side wall of the vertical washing pipe along the vertical direction. An annular washing pipe is connected to the outer end of the vertical washing pipe, and a booster pump is connected to the outer end of the annular washing pipe.

[0013] Furthermore, the top surface of the sliding sealing plate is a conical structure, and a synchronous connecting frame is connected to the center of the top surface of the sliding sealing plate. A sliding filter plate is connected to the top of the synchronous connecting frame. The sliding filter plate is fitted and slidably disposed inside the central conveying cylinder. A first hydraulic telescopic rod is connected to the bottom of the sliding sealing plate. The telescopic end and the fixed end of the first hydraulic telescopic rod are respectively connected to the sliding sealing plate and the central discharge cylinder.

[0014] Furthermore, an annular washing filter plate is nested and slidably arranged on the outer side of the central discharge cylinder. A lateral adjusting rod is connected to the top of the annular washing filter plate. The top of the lateral adjusting rod is connected to the annular circulating filter plate. A second hydraulic telescopic rod is connected to the outer side of the lateral adjusting rod. The telescopic end and the fixed end of the second hydraulic telescopic rod are respectively connected to the sliding sealing plate and the central discharge cylinder. The second hydraulic telescopic rod drives the annular washing filter plate and the annular circulating filter plate to slide up and down synchronously through the lateral adjusting rod.

[0015] The beneficial effects of this invention are as follows: As can be seen from the above description, the o-sulfonic acid separation equipment based on cooling crystallization provided by this invention uses a cooling crystallization plate for cooling crystallization. The cooling crystallization plate can slide periodically along the horizontal guide groove of the annular clamping block. When the plate slides into the vessel, its low-temperature surface induces the o-sulfonic acid in the liquid to crystallize and precipitate. When the plate slides outward, the elastic scrapers on both sides of the cleaning opening automatically scrape off the crystals adhering to the plate surface to prevent scaling. The cooling speed can be adjusted by sliding and adjusting the volume and area of ​​the cooling crystallization plate inside the annular crystallization chamber. The dynamic sliding temperature control of the cooling crystallization plate and the self-cleaning of the elastic scrapers solve the problems of lagging temperature control and scaling on the cooling surface in traditional equipment. Combined with the turbine forced circulation, the o-sulfonic acid crystallization process is achieved with high efficiency, continuous operation, and low consumption, which greatly improves product purity and production efficiency. Attached Figure Description

[0016] To more clearly illustrate the technical solutions in this invention or the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are only for this invention. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0017] Figure 1 This is a schematic diagram of the crystallization separation vessel according to an embodiment of the present invention; Figure 2 This is a front view of an embodiment of the present invention. Figure 3 This is a schematic diagram of the structure of the ring-shaped clamping block according to an embodiment of the present invention; Figure 4 This is a schematic diagram of the bottom structure of the crystallization separation vessel according to an embodiment of the present invention; Figure 5 This is a schematic diagram of the internal structure of the crystallization separation vessel according to an embodiment of the present invention; Figure 6 This is a schematic diagram of the structure of the central conveyor tube in the washing state according to an embodiment of the present invention; Figure 7 This is a schematic diagram of the structure of the central conveying cylinder in the crystalline state according to an embodiment of the present invention; Figure 8 This is a schematic diagram of the cooling crystallization plate according to an embodiment of the present invention; Figure 9 This is a schematic diagram of the structure of the horizontal adjustment frame according to an embodiment of the present invention; Figure 10 This is a schematic diagram of the structure of the horizontal telescopic tube according to an embodiment of the present invention.

[0018] The diagram is marked as follows: 1. Crystallization separation vessel; 101. Annular crystallization chamber; 102. Central conveyor cylinder; 103. Inlet opening; 104. Outlet opening; 105. Conveying turbine; 106. Rotary drive shaft; 107. Conveying motor; 2. Annular clamping block; 201. Horizontal guide groove; 202. Cleaning opening; 203. Elastic scraper; 204. Translation guide rod; 205. Annular guide rail; 206. Adjusting gear ring; 3. Cooling crystallization plate; 301 302. Hollow flow guide chamber; 303. Conveying baffle plate; 304. Conveying opening; 305. Cooling inlet; 306. Cooling outlet; 307. Adjusting traction frame; 308. Translational sliding sleeve; 409. Rotary traction slot; 400. Horizontal adjusting frame; 401. Rotary adjusting gear; 402. Rotary adjusting motor; 403. Translational guide rail; 404. Translational adjusting screw; 405. Translational adjusting motor; 406. Horizontal traction slider; 407. 7. Rotary traction block; 408. Adjusting screw sleeve; 5. Horizontal telescopic pipe; 501. Sliding sleeve; 502. Fixed sleeve; 503. Sliding sealing ring; 504. Annular conveyor bin; 505. Conveying opening; 6. Annular cooler; 601. Annular input pipe; 602. Annular output pipe; 603. Circulating conveying pump; 604. Vertical conveying pipe; 605. Cooling fins; 7. Vertical washing pipe; 701. Washing nozzle; 70 2. Annular washing pipe; 703. Booster pump; 8. Central discharge cylinder; 801. Separation discharge port; 802. Annular collection tray; 803. Collection conveying pipe; 804. Sliding sealing plate; 805. Synchronous connecting frame; 806. Sliding filter plate; 807. First hydraulic telescopic rod; 9. Annular washing filter plate; 901. Annular circulating filter plate; 902. Lateral adjusting rod; 903. Closed guide sleeve; 904. Second hydraulic telescopic rod. Detailed Implementation

[0019] To make the objectives, technical solutions, and advantages of this invention clearer, the invention will be further described in detail below with reference to specific embodiments.

[0020] It should be noted that, unless otherwise defined, the technical or scientific terms used in this invention should have the ordinary meaning understood by one of ordinary skill in the art to which this invention pertains. The terms "first," "second," and similar terms used in this invention do not indicate any order, quantity, or importance, but are merely used to distinguish different components. Terms such as "comprising" or "including" mean that the element or object preceding the word encompasses the elements or objects listed following the word and their equivalents, without excluding other elements or objects. Terms such as "connected" or "linked" are not limited to physical or mechanical connections, but can include electrical connections, whether direct or indirect. Terms such as "upper," "lower," "left," and "right" are used only to indicate relative positional relationships; when the absolute position of the described object changes, the relative positional relationship may also change accordingly.

[0021] like Figure 1 , Figure 2 , Figure 3 , Figure 4 , Figure 5 , Figure 6 , Figure 7 , Figure 8 , Figure 9 , Figure 10 As shown, an o-sulfonic acid separation device based on cooling crystallization includes a crystallization separation vessel 1, the interior of which is provided with an annular crystallization chamber 101, and further includes: An annular clamping block 2 is arranged around the outside of the side wall of the crystallization separation vessel 1. Multiple horizontal guide grooves 201 are evenly arranged in the middle of the annular clamping block 2 in a circular shape. The inner end of the horizontal guide groove 201 penetrates the side wall of the crystallization separation vessel 1 and is provided with a cleaning opening 202. Elastic scrapers 203 are symmetrically arranged on the left and right sides of the cleaning opening 202. The cooling crystallization plate 3 is fitted and slidably disposed inside the horizontal guide groove 201. The interior of the cooling crystallization plate 3 is provided with a hollow flow guide chamber 301. The upper and lower sides of the outer end of the hollow flow guide chamber 301 are respectively connected to a cooling inlet 304 and a cooling outlet 305. The central conveying cylinder 102 is vertically arranged at the center of the annular crystallization chamber 101. The bottom and top of the side wall of the central conveying cylinder 102 are respectively provided with an input opening 103 and an output opening 104. A conveying turbine 105 is fitted and rotated at the center of the interior of the central conveying cylinder 102. A ring-shaped circulating filter plate 901 is fitted and slidably disposed outside the input opening 103 at the bottom of the central conveying cylinder 102. A central discharge cylinder 8 is connected to the bottom of the central conveying cylinder 102. A separation discharge port 801 is provided on the side wall of the central discharge cylinder 8. A sliding sealing plate 804 is fitted and slidably disposed in the middle of the central discharge cylinder 8.

[0022] In this embodiment, the device injects a mixture of o-sulfonic acid and sulfuric acid into the annular crystallization chamber 101 of the crystallization separation vessel 1. The cooling medium enters the hollow guide chamber 301 inside the cooling crystallization plate 3 through the cooling inlet 304 and flows out through the cooling outlet 305, thus cooling the surface of the plate. The cooling crystallization plate 3 can slide periodically along the horizontal guide groove 201 of the annular clamping block 2. When the plate slides into the vessel, its low-temperature surface induces the o-sulfonic acid in the liquid to crystallize and precipitate. When the plate slides outward, the elastic scrapers 203 on both sides of the cleaning opening 202 automatically scrape off the crystals adhering to the surface of the plate to prevent scaling. The cooling crystallization plate 3 is adjusted by sliding to be in the annular position. The internal volume and area of ​​the crystallization chamber 101 are adjusted to regulate the cooling rate. Precise temperature control is achieved through a temperature sensor installed inside the annular crystallization chamber 101. The conveying turbine 105 inside the central conveying cylinder 102 can be activated as needed. The conveying turbine 105 is connected to a conveying motor 107 via a centrally located rotary drive shaft 106. The conveying motor 107 drives the conveying turbine 105 to rotate via the rotary drive shaft 106, thereby driving the liquid material to be drawn in from the bottom inlet opening 103 and discharged through the top outlet opening 104, forming a forced circulation flow. The annular circulation filter plate 901 slides outside the inlet opening 103, allowing liquid containing... The molten crystal enters the central conveyor cylinder 102. When closed, it traps the crystals, allowing only the liquid to pass through. The crystals flow with the liquid into the central discharge cylinder 8. The opening of the separation discharge port 801 is controlled by adjusting the position of the sliding sealing plate 804, achieving the separation and discharge of the crystals and mother liquor. The cooling crystallization plates 3 can be independently slidable for temperature control, and each plate can be moved out of the cooling zone individually, avoiding localized overcooling caused by continuous low temperatures. This achieves programmed gradient cooling, improves crystal particle size uniformity, and allows for precise control of staged cooling, enabling o-sulfonic acid to preferentially precipitate in larger, more uniform, and higher-purity crystal form, while minimizing the precipitation or inclusion of sulfuric acid in the crystals, and facilitating subsequent processing. Washing ultimately achieves efficient separation and low sulfuric acid residue. The conveying turbine 105 drives the directional flow of the liquid, accelerating heat transfer and solute diffusion, shortening the crystallization cycle. At the same time, the sliding sealing plate 804 adjusts the opening of the discharge port. Combined with the timing control of the crystallization plate sliding, scraping, and filtering actions, it supports continuous operation of the entire process, significantly reducing the frequency of downtime for cleaning and improving production efficiency. Thus, the device solves the problems of lagging temperature control and scaling on the cooling surface of traditional equipment by dynamically sliding the cooling crystallization plate 3 and self-cleaning the elastic scraper 203. Combined with the turbine forced circulation, it achieves efficient, continuous, and low-consumption operation of the o-sulfonic acid crystallization process, greatly improving product purity and production efficiency.

[0023] like Figure 1 , Figure 2 , Figure 3 , Figure 4 , Figure 5 , Figure 6 , Figure 7 , Figure 8 , Figure 9 and Figure 10 As shown, preferably, the device drives the translation adjustment screw 404 to rotate via the translation adjustment motor 405, which in turn drives the adjustment sleeve 408, which is threadedly engaged with it, to move axially. The horizontal traction slider 406 is linked with the screw via the adjustment sleeve 408 and slides horizontally along the translation guide rail 403. The slider is connected to the adjustment traction frame 306 via the horizontal adjustment frame 4, and the traction cooling crystallizing plate 3 moves synchronously forward and backward within the horizontal guide groove 201. The translation sliding sleeves 307 on the left and right sides of the adjustment traction frame 306 are nested on the translation guide rod 204. The translation guide rod 204 and the translation guide rail 403 are arranged parallel to each other, forming a double sliding constraint. The translation guide rail 403 controls the axial movement accuracy of the horizontal traction slider 406, while the translation guide rod 204 inhibits the adjustment traction. The radial sway of the guide frame 306 ensures that the crystallizing plate slides smoothly without jamming. The speed and direction of the translation adjustment screw 404 are precisely controlled by the translation adjustment motor 405, realizing digital adjustment of the sliding speed and displacement of the crystallizing plate to meet the dynamic temperature control requirements of different cooling stages. The cooperation between the translation sliding sleeve 307 and the translation guide rod 204 eliminates lateral clearance, avoids the crystallizing plate from tilting, and ensures that the elastic scraper 203 completely scrapes away the crystals on the plate surface. Thus, the device achieves high-precision, low-vibration horizontal sliding of the cooling crystallizing plate 3 through the precision transmission of the motor screw and the rigid traction of the double guide rails, ensuring reliable execution of the scraping action, eliminating motion deviation, maximizing the synergistic efficiency of temperature control and scale removal, and providing a stable power foundation for continuous production.

[0024] like Figure 1 , Figure 2 , Figure 3 , Figure 4 , Figure 5 , Figure 6 , Figure 7 , Figure 8 , Figure 9 and Figure 10As shown, preferably, the rotary adjustment motor 402 of the device drives the rotary adjustment gear 401 to rotate, which meshes with the adjustment gear ring 206 on the annular guide rail 205, causing the horizontal adjustment frame 4 to rotate around the crystallization separation vessel 1 along the annular guide rail 205. The horizontal adjustment frame 4 stops when it rotates directly above the target cooling crystallization plate 3. At this time, the rotary traction block 407 at its bottom engages with the rotary traction slot 308 at the top of the adjustment traction frame 306 at the outer end of the cooling crystallization plate 3. The translation adjustment motor 405 drives the horizontal traction slider 406 to move horizontally, and the locking mechanism... The mechanism transmits power to the adjusting traction frame 306, which pulls the cooling crystallizing plate 3 to slide precisely within the horizontal guide groove 201. Thus, through the rotational positioning of the horizontal adjusting frame 4, all cooling crystallizing plates 3 can be operated sequentially using only one set of translation motor and screw mechanism, significantly reducing equipment complexity and manufacturing costs. The interlocking design of the rotating traction block 407 and the slot ensures no slippage or idle stroke during power transmission, guaranteeing the consistency of the sliding displacement of each crystallizing plate. The horizontal adjusting frame 4 can be rotated to any position of the crystallizing plate, enabling rapid positioning and individual maintenance of faulty plates without the need for overall shutdown.

[0025] like Figure 1 , Figure 2 , Figure 3 , Figure 4 , Figure 5 , Figure 6 , Figure 7 , Figure 8 , Figure 9 and Figure 10 As shown, preferably, the cooling medium enters the hollow guide chamber 301 from the cooling inlet 304 and flows vertically through multiple conveying baffles 302. The medium zigzags between the conveying openings 303 on opposite sides of adjacent baffles to prolong the residence time and fully absorb the heat from the plates. The outer ends of the cooling inlet 304 and the cooling outlet 305 are connected to the annular cooler 6 via horizontal telescopic pipes 5. The horizontal telescopic pipes 5 expand and contract synchronously with the sliding of the cooling crystallizing plates 3 to compensate for displacement deviations and maintain a leak-free pipeline seal. The medium flows into the annular cooler... The medium flows through the annular output pipe 602 of the cooler 6 and then into the vertical conveying pipe 604. When the medium flows in the vertical conveying pipe 604, the cooling fins 605 dissipate heat through air convection. A cooling fan can be installed on the outside of the cooling fins 605 to improve the heat dissipation effect. The vertical conveying pipe 604 is then conveyed to the circulating conveying pump 603 after being gathered through an annular main pipe. The circulating conveying pump 603 pressurizes and conveys the cooling medium to the annular input pipe 601, and then returns to the cooling input port 304 through the horizontal telescopic pipe 5 to complete the cooling cycle.

[0026] like Figure 1 , Figure 2 , Figure 3 , Figure 4 , Figure 5 , Figure 6 , Figure 7 , Figure 8 , Figure 9 and Figure 10 As shown, preferably, the horizontal telescopic tube 5 of the device includes a fixed sleeve 502 and a sliding sleeve 501. The sliding sleeve 501 is nested inside the fixed sleeve 502 and slides within it. The two are sealed by a sliding sealing ring 503 to maintain zero leakage of the medium. The cooling medium is transported from the annular inlet pipe 601 or the annular outlet pipe 602 to the annular conveying chamber 504, and then through the conveying opening 505 to the cavity of the fixed sleeve 502, and continues to be transported to the sliding sleeve 501, and then to the cooling inlet port 304 or the cooling outlet port 305. When the cooling crystallizing plate 3 slides outward, it drives the sliding sleeve 501 to move outward, blocking more of the conveying opening. The hole 505 reduces the effective flow area of ​​the opening, thereby automatically reducing the medium flow rate. When the cooling crystallizing plate 3 slides inward, it drives the sliding sleeve 501 to move inward, exposing more of the conveying opening 505, increasing the effective flow area of ​​the opening, and thus automatically increasing the medium flow rate. Therefore, when the crystallizing plate is deep into the liquid and strong cooling is required, the flow rate automatically increases; when it is withdrawing from the scraping process and weak cooling is required, the flow rate automatically decreases. This achieves dynamic distribution of cooling capacity on demand, with real-time linkage between flow rate changes and plate displacement, resulting in faster response speed, avoiding temperature overshoot, and providing on-demand cooling and energy saving. Traditional equipment has a constant cooling flow rate, while this design can reduce idle flow and reduce pump power consumption.

[0027] like Figure 1 , Figure 2 , Figure 3 , Figure 4 , Figure 5 , Figure 6 , Figure 7 , Figure 8 , Figure 9 and Figure 10 As shown, preferably, the inner side of the elastic scraper 203 of the device is vertically provided with a vertical washing pipe 7. The booster pump 703 inputs the washing liquid into the annular washing pipe 702, and then delivers it to the vertical washing pipe 7. It is then sprayed out at high pressure from the washing nozzle 701 to cover the plate surface. When the cooling crystallization plate 3 slides outward to the scraping station, the washing nozzle 701 sprays simultaneously to clean the crystals. Then the elastic scraper 203 completely scrapes off the crystals, resulting in higher overall cleaning efficiency.

[0028] like Figure 1 , Figure 2 , Figure 3 , Figure 4 , Figure 5 , Figure 6 , Figure 7 , Figure 8 , Figure 9 and Figure 10As shown, preferably, an annular washing filter plate 9 is nested and slidably arranged on the outer side of the central discharge cylinder 8 of the device. A lateral adjusting rod 902 is connected to the top of the annular washing filter plate 9. The lateral adjusting rod 902 is slidably connected to the bottom plate of the crystallization separation vessel 1 through the outer closed guide sleeve 903. The top of the lateral adjusting rod 902 is connected to the annular circulating filter plate 901. A second hydraulic telescopic rod 904 is connected to the outer side of the lateral adjusting rod 902. The telescopic end and the fixed end of the second hydraulic telescopic rod 904 are respectively connected to the sliding sealing plate 804 and the central discharge cylinder 8. The second hydraulic telescopic rod 904 drives the annular washing filter plate 9 and the annular circulating filter plate 9 through the lateral adjusting rod 902. During crystallization, the sliding filter plate 806 is located at the bottom of the central conveying cylinder 102, and the sliding sealing plate 804 is located inside the central discharge cylinder 8 and above the separation discharge port 801. After crystallization, the sliding sealing plate 804 and the sliding filter plate 806 slide upwards simultaneously, causing the sliding sealing plate 804 to move to the top of the central discharge cylinder 8, i.e., the bottom of the central conveying cylinder 102. At this time, the sliding filter plate 806 moves to the middle of the interior of the central conveying cylinder 102, above the input opening 103. At this time, the annular circulating filter plate 901 is located above the input opening 103, keeping the input opening 103 open. Then, the conveying turbine 105 continues to work, mixing... The liquid is drawn into the central conveying cylinder 102 through the inlet 103. Crystals are filtered and separated by the sliding filter plate 806 and trapped inside the central conveying cylinder 102, specifically between the sliding filter plate 806 and the sliding sealing plate 804. After the crystals are filtered and collected inside the central conveying cylinder 102, the sliding filter plate 806 and the sliding sealing plate 804 are connected by a synchronous connecting frame 805. The first hydraulic telescopic rod 807 can drive the sliding sealing plate 804 and the sliding filter plate 806 to move downwards synchronously, causing the sliding sealing plate 804 to move below the separation outlet 801. At this time, the annular washing filter plate 9 slides to the outside of the separation outlet 801, and then the liquid can pass through the separation outlet 801. The crystals are discharged, while the crystals are intercepted by the annular washing filter plate 9 and located inside the central discharge cylinder 8. Then, washing liquid can be conveyed to the annular crystallization chamber 101 to wash the crystals inside the central discharge cylinder 8. Finally, the annular washing filter plate 9 slides open the separation discharge port 801 to discharge the crystals. The cone-shaped structure of the sliding sealing plate 804 prevents crystals from accumulating and getting stuck. An annular collection plate 802 is arranged around the lower outer side of the separation discharge port 801. The outer side of the annular collection plate 802 is connected to the collection and conveying pipe 803 to facilitate the collection and conveying of materials. Thus, crystallization, filtration, washing and discharge are integrated into a single device, and the four-stage action is completed sequentially in a closed system, eliminating material transfer contamination and improving product purity.

[0029] The o-sulfonic acid separation equipment based on cooling crystallization provided by this invention uses a cooling crystallization plate 3 for cooling crystallization. The cooling crystallization plate 3 can slide periodically along the horizontal guide groove 201 of the annular clamping block 2. When the plate slides into the vessel, its low-temperature surface induces the o-sulfonic acid in the liquid to crystallize and precipitate. When the plate slides outward, the elastic scrapers 203 on both sides of the cleaning opening 202 automatically scrape off the crystals adhering to the plate surface to prevent scaling. The cooling speed can be adjusted by sliding and adjusting the volume and area of ​​the cooling crystallization plate 3 inside the annular crystallization chamber 101. The dynamic sliding temperature control of the cooling crystallization plate 3 and the self-cleaning of the elastic scrapers 203 solve the problems of lagging temperature control and scaling on the cooling surface in traditional equipment. Combined with turbine forced circulation, it achieves efficient, continuous and low-consumption operation of the o-sulfonic acid crystallization process, greatly improving product purity and production efficiency.

[0030] Those skilled in the art should understand that the discussion of any of the above embodiments is merely exemplary and is not intended to imply that the scope of the invention is limited to these examples; within the framework of the invention, the technical features of the above embodiments or different embodiments can also be combined, the steps can be implemented in any order, and there are many other variations of the different aspects of the invention as described above, which are not provided in detail for the sake of brevity. Any omissions, modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the invention should be included within the scope of protection of the invention.

Claims

1. A sulfonic acid separation device based on cooling crystallization, comprising a crystallization separation vessel (1), wherein the crystallization separation vessel (1) is provided with an annular crystallization chamber (101), characterized in that, Also includes: A ring-shaped clamping block (2) is arranged around the outside of the side wall of the crystallization separation vessel (1). The middle of the ring-shaped clamping block (2) is uniformly provided with a plurality of horizontal guide grooves (201) in a circular shape. The inner end of the horizontal guide groove (201) penetrates the side wall of the crystallization separation vessel (1) and is provided with a cleaning opening (202). Elastic scrapers (203) are symmetrically arranged on the left and right sides of the cleaning opening (202). The cooling crystallization plate (3) is fitted and slidably disposed inside the horizontal guide groove (201). The cooling crystallization plate (3) is provided with a hollow flow guide chamber (301). The upper and lower sides of the outer end of the hollow flow guide chamber (301) are respectively connected to a cooling inlet (304) and a cooling outlet (305). A central conveying cylinder (102) is vertically arranged at the center of the annular crystallization chamber (101). The bottom and top of the side wall of the central conveying cylinder (102) are respectively provided with an input opening (103) and an output opening (104). A conveying turbine (105) is fitted and rotated at the center of the interior of the central conveying cylinder (102). A ring-shaped circulating filter plate (901) is fitted and slidably disposed outside the input opening (103) at the bottom of the central conveying cylinder (102). A central discharge cylinder (8) is connected to the bottom of the central conveying cylinder (102). A separation discharge port (801) is provided on the side wall of the central discharge cylinder (8). A sliding sealing plate (804) is fitted and slidably disposed in the middle of the central discharge cylinder (8). The hollow flow guide chamber (301) has multiple conveying baffles (302) arranged evenly and parallel in the vertical direction inside. Conveying openings (303) are provided on the opposite side of adjacent conveying baffles (302). The outer ends of the cooling inlet (304) and cooling outlet (305) are connected to horizontal telescopic pipes (5). The outer ends of the cooling inlet (304) and cooling outlet (305) are connected to the annular cooler (6) through the horizontal telescopic pipes (5). The annular cooler (6) has a plurality of cooling fins (605) arranged evenly and parallel in the vertical direction in the middle. A plurality of vertical conveying pipes (604) are embedded in the middle of the cooling fins (605). Annular input pipes (601) and annular output pipes (602) are respectively provided at the upper and lower ends of the vertical conveying pipes (604). A circulating conveying pump (603) is provided in the middle of the annular input pipes (601). The outer ends of the cooling input port (304) and the cooling output port (305) are respectively connected to the annular input pipes (601) and the annular output pipes (602) through horizontal telescopic pipes (5). The horizontal telescopic tube (5) includes a fixed sleeve (502) and a sliding sleeve (501). The sliding sleeve (501) is fitted and slidably disposed inside the fixed sleeve (502). The inner end of the sliding sleeve (501) is connected to the cooling inlet (304) or the cooling outlet (305). The outer end of the fixed sleeve (502) is connected to the annular inlet pipe (601) or the annular outlet pipe (602). A sliding sealing ring (503) is arranged around the inner end opening of the fixed sleeve (502). An annular conveying chamber (504) is provided in the middle of the side wall of the fixed sleeve (502). A plurality of conveying openings (505) are evenly arranged in the horizontal direction in the middle of the inner wall of the fixed sleeve (502). The conveying openings (505) are connected to the annular inlet pipe (601) or the annular outlet pipe (602) through the annular conveying chamber (504).

2. The o-sulfonic acid separation device based on cooling crystallization according to claim 1, characterized in that, A horizontal adjustment frame (4) is provided above the cooling crystallization plate (3). A translation guide rail (403) is provided in the middle of the horizontal adjustment frame (4). A translation adjustment screw (404) is provided parallel to the outside of the translation guide rail (403). A translation adjustment motor (405) is connected to the shaft end of the translation adjustment screw (404). A horizontal traction slider (406) is slidably provided in the middle of the translation guide rail (403). An adjustment sleeve (408) is provided in the middle of the horizontal traction slider (406). The horizontal traction slider (406) is connected to the translation adjustment screw (404) through the adjustment sleeve (408). An adjustment traction frame (306) is provided at the outer end of the cooling crystallization plate (3). The horizontal traction slider (406) is connected to the adjustment traction frame (306).

3. The o-sulfonic acid separation device based on cooling crystallization according to claim 2, characterized in that, The horizontal guide groove (201) has symmetrical horizontal translation guide rods (204) on the left and right sides of its outer end. The adjustment traction frame (306) has symmetrical translation sliding sleeves (307) on its left and right sides. The adjustment traction frame (306) is slidably connected to the translation guide rods (204) through the translation sliding sleeves (307).

4. The o-sulfonic acid separation device based on cooling crystallization according to claim 3, characterized in that, The top of the annular clamping block (2) is surrounded by an annular guide rail (205). The horizontal adjustment frame (4) is slidably connected to the annular guide rail (205). The horizontal adjustment frame (4) is slidably rotated around the crystallization separation vessel (1) via the annular guide rail (205). A rotating traction block (407) is connected below the horizontal traction slider (406). A rotating traction slot (308) is provided in the middle of the top of the adjustment traction frame (306). The rotating traction slot (308) and the rotating traction block (407) are mutually engaged. A rotating adjustment motor (402) is provided at the bottom of the horizontal adjustment frame (4). A rotating adjustment gear (401) is connected to the shaft end of the rotating adjustment motor (402). An adjustment gear ring (206) is surrounded in the middle of the annular guide rail (205). The rotating adjustment gear (401) and the adjustment gear ring (206) are mutually meshed.

5. The o-sulfonic acid separation device based on cooling crystallization according to claim 1, characterized in that, A vertical washing pipe (7) is vertically arranged on the inner side of the elastic scraper (203). Multiple washing nozzles (701) are evenly arranged on the side wall of the vertical washing pipe (7) in the vertical direction. An annular washing pipe (702) is connected to the outer end of the vertical washing pipe (7). A booster pump (703) is connected to the outer end of the annular washing pipe (702).

6. The o-sulfonic acid separation device based on cooling crystallization according to claim 1, characterized in that, The top surface of the sliding sealing plate (804) is a conical structure. A synchronous connecting frame (805) is connected to the center of the top surface of the sliding sealing plate (804). A sliding filter plate (806) is connected to the top of the synchronous connecting frame (805). The sliding filter plate (806) is fitted and slidably disposed inside the central conveying cylinder (102). A first hydraulic telescopic rod (807) is connected to the bottom of the sliding sealing plate (804). The telescopic end and the fixed end of the first hydraulic telescopic rod (807) are respectively connected to the sliding sealing plate (804) and the central discharge cylinder (8).

7. The o-sulfonic acid separation device based on cooling crystallization according to claim 6, characterized in that, An annular washing filter plate (9) is nested and slidably arranged on the outer side of the central discharge cylinder (8). A lateral adjustment rod (902) is connected to the top of the annular washing filter plate (9). The top of the lateral adjustment rod (902) is connected to the annular circulating filter plate (901). A second hydraulic telescopic rod (904) is connected to the outer side of the lateral adjustment rod (902). The telescopic end and the fixed end of the second hydraulic telescopic rod (904) are connected to the sliding sealing plate (804) and the central discharge cylinder (8) respectively. The second hydraulic telescopic rod (904) drives the annular washing filter plate (9) and the annular circulating filter plate (901) to slide up and down synchronously through the lateral adjustment rod (902).

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