Long carbon chain dibasic acid crystallization and separation integrated device

Abstract

The application discloses a long-carbon-chain binary acid crystallization and separation integrated equipment, and relates to the field of crystallization and separation equipment, which comprises a crystallization tower, and further comprises a separation pipe and a plurality of groups of crystallization pipes which are distributed in the circumferential direction of the crystallization tower; a plurality of groups of crystallization attachment rods which are detachably arranged in the separation pipe and the crystallization pipe and have outer surfaces which are modified for crystallization promotion; a support frame which is arranged in the crystallization tower and is used for temporarily storing idle crystallization attachment rods; a solution circulation system which is used for conveying solution into the crystallization pipe and making the solution flow in the crystallization pipe in a circulating manner; a cooling part which is arranged in the crystallization pipe and is used for cooling the solution entering the crystallization pipe; a heating part which is arranged on the separation pipe and is used for heating the crystallization attachment rod entering the separation pipe, and a discharge pipe which is communicated with the lower end of the separation pipe; and a carrying assembly which is arranged in the crystallization tower and is used for carrying the crystallization attachment rod between the separation pipe and the crystallization pipe. The application has the effects of realizing the continuous crystallization and separation process and improving the production efficiency.

Description

Technical Field

[0001] This invention relates to the field of crystallization and separation equipment, and in particular to an integrated equipment for the crystallization and separation of long-chain dicarboxylic acids. Background Technology

[0002] Long-chain dicarboxylic acids (such as DC12-DC18) are important raw materials for synthesizing high-performance nylon, hot melt adhesives, fragrances, and other chemical products. Currently, the mainstream production process is bio-fermentation. After extraction, the fermentation broth needs to undergo multiple processes such as crystallization, centrifugation, washing, and drying to obtain the finished product.

[0003] Related technology can be found in Chinese patent application CN118681260A, which discloses a continuous crystallization separation device. This device, from top to bottom, includes a cooling crystallization section, a crystallization precipitation section, and a crystallization separation section. The cooling crystallization section includes a heat exchange device used to cool the flowing solution, causing it to transition from an unsaturated state to a saturated state, forming crystalline crystals. The crystallization precipitation section is connected to the cooling crystallization section and is used to enrich the crystalline crystals and precipitate them as a solid product. The crystallization separation section is connected to the crystallization precipitation section and is used to separate the solid product from the solution. This method enables the continuous crystallization preparation of lithium hexafluorophosphate, significantly improving the production efficiency of lithium hexafluorophosphate.

[0004] Regarding the aforementioned technologies, the crystals remain mixed with the solution during the crystallization separation stage. During crystal discharge, some solution remains mixed within the crystals. Therefore, further solid-liquid separation, washing, and drying are required to obtain crystals of higher purity. When higher purity crystals are needed and the use of organic solvents must be avoided, layer crystallization can be employed. This involves allowing crystals to adhere to a solid wall and form a crystalline layer, which is then processed through sweating, washing, and peeling off the crystal layer. However, in layer crystallization, processing the crystalline layer takes time, during which the crystallization separation equipment cannot continue crystallization, making continuous production difficult. Summary of the Invention

[0005] In order to obtain high-purity crystalline products while achieving continuous production of crystallization and separation, this application provides an integrated equipment for the crystallization and separation of long-chain dicarboxylic acids.

[0006] This application provides an integrated device for crystallization and separation of long-chain dicarboxylic acids, employing the following technical solution: An integrated device for crystallization and separation of long-chain dicarboxylic acids, comprising a crystallization tower, and further comprising: The separation tube and several sets of crystallizing tubes are evenly distributed around the circumference of the crystallization tower, and both the separation tube and the crystallizing tube are designed to inhibit crystallization and modify the crystallization. Several sets of crystallization attachment rods are provided, corresponding to the separation tube and the crystallization tube. The outer circular surface of the crystallization attachment rods is modified to promote crystallization, which facilitates the adhesion of the crystallization layer. The upper ends of the crystallization tube and the separation tube are provided with openings along the axial direction for the crystallization attachment rods to enter and exit. The solution circulation system includes a solution storage section, an outlet pipe, and an inlet pipe. The solution storage section is located below the crystallization tower and is used to store the solution. Both the outlet pipe and the inlet pipe are connected to the solution storage section. The outlet pipe is connected to the upper end of the crystallization tower and is used to transport the solution into the crystallization tower. The inlet pipe is connected to the lower end of the crystallization tower and is used to recover the solution flowing to the bottom of the crystallization tower back to the solution storage section. A cooling element, installed inside the crystallization tube, is used to cool the solution entering the crystallization tube; A heating element, installed on the separation tube, is used to heat the crystallizing rods that enter the separation tube. A discharge pipe is connected to the lower end of the separation tube. A transport assembly, located inside the crystallization tower, is used to transport the crystallization attachment rod between the separation tube and the crystallization tube; A support frame, installed inside the crystallization tower, is used to temporarily store and support idle crystal attachment rods.

[0007] By adopting the above technical solution, in the initial state, the crystallizing rod in the working state is located inside the crystallization tube, and the idle crystallizing rod is placed on the support frame. The solution circulation system delivers a high-temperature saturated solution to the upper end of the crystallization tube through the outlet pipe, causing the solution to flow along the outer surface of the crystallizing rod. During this process, the solution is cooled by the cooling component, causing crystals to precipitate and adhere to the outer surface of the crystallizing rod. After the solution flows to the lower end of the crystallization tube, it is then recovered to the solution storage section by the inlet pipe. The solution circulates. When the thickness of the crystal layer outside the crystallizing rod reaches the required level, the crystallizing rod is pulled out of the crystallization tube by the transport component and placed into the separation tube through the opening. The heating component slowly heats up the crystal layer to make it sweat. After the sweating process is completed, the temperature continues to rise, causing the crystal layer to melt and be discharged and collected through the discharge pipe. During the heating and sweating process, the transport component places the idle crystallizing rod on the support frame into the idle separation tube to continue the crystallization work. The crystallization and separation work are carried out simultaneously, which is beneficial to maintaining the purity of the crystals while improving the efficiency and convenience of crystallization and separation production.

[0008] Optionally, the upper end of the crystallizing tube is provided with a flow passage cavity along the circumference, the flow passage cavity is arranged around the crystallizing tube, and a number of nozzles connected to the flow passage cavity are arranged circumferentially inside the crystallizing tube. When the crystallizing attachment rod is located inside the crystallizing tube, it is located between all the nozzles. The crystallizing tower is provided with a medium conveying system for conveying cleaning medium to the flow passage cavity.

[0009] By adopting the above technical solution, while the crystallizing rod is being extracted from the crystallization tube, a cleaning medium, such as a gas that does not react with crystallization, is conveyed into the flow chamber through the medium conveying system. The cleaning medium is sprayed from the nozzle onto the outer surface of the crystallizing rod and blows the residual solution on the outer surface of the crystallizing rod into the crystallization tube for collection, thereby reducing the probability of the solution on the surface of the crystallizing rod contaminating the equipment during the handling of the crystallizing rod.

[0010] Optionally, the cooling component includes a flow tube, a support tube, and a medium circulation system. The support tube is coaxially disposed inside the crystallization tube and fixed to the crystallization tower. The flow tube is coaxially fixed inside the support tube and extends along the length of the crystallization tube. A heat-conducting cavity is opened at the lower end of the crystallization attachment rod along the axial direction. The inner diameter of the heat-conducting cavity is larger than the outer diameter of the flow tube. When the crystallization attachment rod is located inside the crystallization tube and is in working condition, the upper end of the support tube is in contact with the crystallization attachment rod. The support tube has a recovery hole that communicates with the heat-conducting cavity in a vertical direction. At this time, the flow tube is located inside the heat-conducting cavity and does not contact the inner wall of the heat-conducting cavity. The medium circulation system is used to transport the cooling medium. It is provided with a medium input end and a recovery end. The input end is connected to the lower end of the flow tube, and the recovery end is connected to the recovery hole.

[0011] By adopting the above technical solution, the support tube provides support for the flow tube. During the crystallization process, the flow tube is located in the heat conduction cavity. At this time, the medium circulation system delivers cooling medium to the flow tube through the input end. The cooling medium flows into the cooling cavity along the flow tube, thereby cooling the crystal attachment rod, so that the crystals adhere to the outer surface of the crystal attachment rod. The cooling medium that has completed the heat exchange passes through the recovery hole and flows back to the medium circulation system from the recovery end, so as to realize the continuous circulation of the cooling medium.

[0012] Optionally, in the same group of crystallization tubes, there are multiple crystallization tubes. A support cylinder is fixed inside the crystallization tower. All crystallization tubes in the same group are located inside the support cylinder. The upper ends of all crystallization attachment rods in the same group are fixed to the same mounting plate. When the transport component is working, it drives all the corresponding crystallization attachment rods to move through the mounting plate. A sealing plate is fixed at the upper end of the support cylinder. The sealing plate has a through hole that matches the crystallization attachment rod along the vertical direction. When the crystallization attachment rod is located inside the crystallization tube and is in working condition, the lower end face of the mounting plate is attached to the upper end face of the sealing plate and blocks the through hole.

[0013] By adopting the above technical solution, the diameter of the crystallization tube and the crystallization attachment rod is reduced, thereby increasing the contact area between the crystallization attachment rod and the solution and improving the crystallization efficiency. The support cylinder protects all crystallization tubes in the same group. During the crystallization process, the mounting plate is supported by the sealing plate, and the inside of the support cylinder is kept in a sealed state.

[0014] Optionally, the upper end of the crystallization tube is slidably connected to two semi-ring blocks. The two semi-ring blocks are arranged opposite each other with respect to the crystallization tube axis and move in a direction that approaches or moves away from each other. The support cylinder is provided with a power component for driving the semi-ring blocks to open and close. When the crystallization attachment rod is located inside the crystallization tube, it is located between the two semi-ring blocks and fits against the semi-ring blocks. The semi-ring blocks have a buffer cavity inside that communicates with the liquid outlet pipe. The liquid outlet pipe communicates with the buffer cavity. The lower end of the semi-ring blocks has a drain port that communicates with the buffer cavity. The drain port is arc-shaped and surrounds the crystallization attachment rod.

[0015] By adopting the above technical solution, in the initial state, the two semi-ring blocks are far apart from each other, thus avoiding the crystallization attachment rod. When the crystallization attachment rod enters the crystallization tube, the power component drives the two semi-ring blocks to approach each other and close together, thereby positioning the crystallization attachment rod. The outlet pipe transports the solution to the buffer chamber. After entering the buffer chamber, the solution is discharged along the drain port to the crystallization attachment rod and sprayed onto the outside of the crystallization attachment rod, thereby making the solution evenly distributed on the outer circle of the crystallization attachment rod and improving the uniformity of the crystallization layer.

[0016] Optionally, the semi-ring block is provided with a pressure valve plate at the drain port. The pressure valve plate blocks the drain port in its natural state. When the outlet pipe delivers solution into the buffer chamber, the pressure valve plate opens under the pressure of the solution and guides the solution to flow towards the crystal adhesion rod.

[0017] By adopting the above technical solution, when the solution is stopped being supplied to the buffer chamber, the pressure valve plate blocks the drain port, thereby reducing the probability of solution leakage from the drain port.

[0018] Optionally, the heating element includes a heating ring and a heating rod. The separation tube has a cavity along the axial direction, the heating ring is disposed in the cavity and extends along the axial direction of the separation tube, and a heat-conducting layer is provided on the inner wall of the separation tube to guide the heat of the heating ring to radiate to the crystallization attachment rod. The heating rod is fixed on the crystallization tower and coaxially disposed on the inner side of the separation tube. The outer diameter of the heating rod is smaller than the inner diameter of the heat-conducting cavity.

[0019] By adopting the above technical solution, the heating ring and heating rod can work synchronously to heat the crystal layer from both the inside and outside, or they can be started separately to heat the crystal layer from the inside or outside.

[0020] Optionally, the upper end of the separation tube has a cleaning chamber opened in the circumferential direction, and the inner wall of the separation tube is provided with a number of nozzles II that communicate with the cleaning chamber in the circumferential direction. When the crystallization attachment rod is located inside the separation tube, it is located between all the nozzles II, and the nozzles II are inclined from top to bottom toward the axis of the separation tube. The crystallization tower is provided with a medium conveying system II for conveying the cleaning medium to the cleaning chamber.

[0021] By adopting the above technical solution, after the thermal melting separation of the crystallized layer is completed, the cleaning medium is transported through the two-way cleaning chamber of the medium conveying system, so that the cleaning medium is sprayed out along the second nozzle onto the crystallized attachment rod, thereby cleaning the crystallized attachment rod.

[0022] In summary, this application includes at least one of the following beneficial technical effects: 1. In the initial state, the crystallizing rod in the working state is inside the crystallization tube, and the idle crystallizing rod is placed on the support frame. The solution circulation system delivers a high-temperature saturated solution to the upper end of the crystallization tube through the liquid outlet pipe, causing the solution to flow along the outer surface of the crystallizing rod. During this process, the solution is cooled by the cooling component, causing crystals to precipitate and adhere to the outer surface of the crystallizing rod. After the solution flows to the lower end of the crystallization tube, it is then recovered to the solution storage section by the liquid inlet pipe. The solution circulates. When the thickness of the crystal layer outside the crystallizing rod reaches the required level, the crystallizing rod is pulled out of the crystallization tube by the transport component and placed into the separation tube through the open end. The heating component slowly heats up the crystal layer to make it sweat. After the sweating process is completed, the temperature continues to rise, causing the crystal layer to melt and be discharged and collected through the discharge pipe. During the heating and sweating process, the transport component places the idle crystallizing rod on the support frame into the idle separation tube to continue the crystallization work. The crystallization and separation work are carried out simultaneously, which helps to maintain the purity of the crystals while improving the efficiency and convenience of crystallization and separation production. 2. While the crystallizing rod is being removed from the crystallization tube, a cleaning medium, such as a gas that does not react with crystallization, is being transported into the flow chamber through a media delivery system. The cleaning medium is sprayed from a nozzle onto the outer surface of the crystallizing rod and blows the residual solution on the outer surface of the crystallizing rod into the crystallization tube for collection, thereby reducing the probability of the solution on the surface of the crystallizing rod contaminating the equipment during the handling of the crystallizing rod. Attached Figure Description

[0023] Figure 1 This is a schematic diagram of the external structure of the crystallization tower.

[0024] Figure 2 This is a schematic diagram of the internal structure of a crystallization tower.

[0025] Figure 3 This is a schematic diagram designed to highlight the internal structure of the support cylinder.

[0026] Figure 4 yes Figure 3 An enlarged schematic diagram of part A in the middle.

[0027] Figure 5 This is a schematic diagram designed to highlight the position of the semi-circular block.

[0028] Figure 6 This is a schematic diagram designed to highlight the internal structure of the separator.

[0029] Explanation of reference numerals in the attached drawings: 1. Crystallization tower; 11. Support cylinder; 111. Sealing plate; 121. Guide plate; 122. Moving block; 123. Power unit; 124. Guide groove; 13. Support frame; 2. Separation pipe; 21. Discharge pipe; 22. Cleaning chamber; 23. Nozzle two; 3. Crystallization tube; 31. Flow chamber; 32. Nozzle one; 33. Semi-ring block; 331. Buffer chamber; 332. Drain port; 333. Pressure valve plate; 3 34. Round rod; 4. Crystallization adhesion rod; 41. Heat conduction cavity; 42. Mounting plate; 421. Clamping rod; 51. Solution storage section; 52. Liquid outlet pipe; 53. Liquid inlet pipe; 6. Cooling component; 61. Flow pipe; 62. Support pipe; 621. Recovery hole; 7. Heating component; 71. Heating ring; 72. Heating rod; 8. Transport assembly; 81. Vertical moving part; 82. Lateral moving part; 83. Rotating part; 84. Clamping part. Detailed Implementation

[0030] The present application will be further described in detail below with reference to all the accompanying drawings.

[0031] This application discloses an integrated device for crystallization and separation of long-chain dicarboxylic acids. Example

[0032] Reference Figure 1 , Figure 2 and Figure 3 An integrated crystallization and separation device for long-chain dicarboxylic acids includes a crystallization tower 1. Inside the crystallization tower 1, multiple sets of crystallization tubes 3 and a set of separation tubes 2 are evenly distributed along the circumference. Both the crystallization tubes 3 and the separation tubes 2 are hollow, and the upper ends of both the crystallization tubes 3 and the separation tubes 2 are open. The lower end of the crystallization tower 1 is fixed with a base, and the crystallization tubes 3 and the separation tubes 2 are installed on the base and kept in a vertical state.

[0033] Reference Figure 2 and Figure 3 It also includes multiple sets of crystallization attachment rods 4, the number of which corresponds to the total number of crystallization tubes 3 and separation tubes 2. In the initial state, the crystallization attachment rods 4 are located inside the corresponding crystallization tube 3 or separation tube 2, and the outer surface of the crystallization attachment rods 4 does not contact the corresponding crystallization tube 3 or separation tube 2. All crystallization tubes 3 in the same set are provided with the same support cylinder 11 on their outer side. A sealing plate 111 is fixedly connected to the upper end of the support cylinder 11. The sealing plate 111 has through holes that correspond one-to-one with the crystallization attachment rods 4 along its vertical direction. The upper end of the crystallization attachment rods 4 passes through the through holes and is fixedly connected to the same mounting plate 42. Under the action of gravity, the lower end of the mounting plate 42 is in contact with the upper end face of the sealing plate 111. At this time, the mounting plate 42 blocks the through holes, so that the support cylinder 11 is in a sealed state.

[0034] Reference Figure 2 and Figure 3The crystallization tower 1 is equipped with a conveying assembly 8 for conveying the crystallization attachment rod 4 between the separation tube 2 and the crystallization tube 3. Two semi-ring blocks 33 are slidably connected to the upper end of the crystallization tube 3 along the support cylinder 11. The two semi-ring blocks 33 are arranged opposite each other with the axis of the crystallization tube 3 as the center. Both semi-ring blocks 33 are slidably connected to the support cylinder 11 in a direction close to or away from the axis of the crystallization tube 3. The support cylinder 11 is fixed with a guide rod for guiding the movement of the semi-ring blocks 33.

[0035] Reference Figure 3 and Figure 4 The semi-ring block 33 has a buffer cavity 331 inside, and a drain port 332 is provided at the lower end of the semi-ring block 33. The drain port 332 is arc-shaped and inclined from top to bottom toward the axis of the crystallizing tube 3. A pressure valve plate 333 is slidably connected to the lower end of the semi-ring block 33. A spring is provided between the semi-ring block 33 and the pressure valve plate 333. In its natural state, the spring applies a pushing force to the pressure valve plate 333, so that the pressure valve plate 333 is located in the drain port 332 and blocks the drain port 332.

[0036] Reference Figure 3 and Figure 5 The support cylinder 11 is provided with a power component for driving two semi-ring blocks 33 of the same group to move closer or further apart. The power component includes a guide plate 121, a moving block 122 and a power unit 123. The guide plate 121 is slidably connected to the support cylinder 11 in the vertical direction. Both semi-ring blocks 33 are fixedly connected to round rods 334 in the horizontal direction. The guide plate 121 has two guide grooves 124 that are adapted to the round rods 334 in the vertical direction from top to bottom. The two guide grooves 124 gradually move further apart from bottom to top.

[0037] Reference Figure 3 and Figure 5 The round rod 334 is located within the corresponding guide groove 124 and fits against the inner wall of the guide groove 124. All guide plates 121 within the same support cylinder 11 are fixedly connected to the moving block 122. The power unit 123 is located inside the support cylinder 11 and is used to drive the moving block 122 to move vertically. Specifically, the power unit 123 uses a motor screw mechanism, which is existing technology and will not be described in detail here.

[0038] Reference Figure 3 and Figure 5In the initial state, the guide plate 121 is in an upward state. At this time, the round rod 334 is located at the lower end of the guide groove 124, and the two semi-annular blocks 33 are close to each other and cover the outside of the crystallizing attachment rod 4. The drain port 332 faces the outer surface of the crystallizing attachment rod 4. When the power unit 123 drives the moving block 122 to move down, the guide plate 121 descends synchronously with the moving block 122, thereby pushing the two round rods 334 away from each other through the inner wall of the guide groove 124, so that the two semi-annular blocks 33 are away from each other, so as to avoid the crystallizing attachment rod 4 during the transportation of the crystallizing attachment rod 4.

[0039] Reference Figure 2 and Figure 3 The crystallization tower 1 is also equipped with a solution circulation system, which includes a solution storage section 51, an outlet pipe 52, and an inlet pipe 53. The solution storage section 51 is installed at the lower end of the crystallization tower 1 and is connected to an external liquid supply system, which supplies saturated solution to the solution storage section 51. Both the outlet pipe 52 and the inlet pipe 53 are connected to the solution storage section 51, and the end of the outlet pipe 52 away from the solution storage section 51 is connected to a branch pipe, which is fixedly connected to the semi-ring block 33 and connected to the buffer chamber 331.

[0040] Reference Figure 3 and Figure 4 An infusion pump is installed on the outlet pipe 52. When the infusion pump is working, it drives the solution in the solution storage section 51 to flow along the outlet pipe 52 to the branch pipe. The solution enters the corresponding buffer chamber 331 along the branch pipe and pushes the pressure valve plate 333 away from the drain port 332. Under the guidance of the pressure valve plate 333 and the drain port 332, the solution is sprayed out onto the outer surface of the crystallizing attachment rod 4 and flows along the outer surface of the crystallizing attachment rod 4. The drain port 332 is arc-shaped, so that the solution is evenly distributed on the outer circle of the crystallizing attachment rod 4. After the solution flows to the lower end of the crystallizing tube 3, it is collected back into the solution storage section 51 by the inlet pipe 53.

[0041] Reference Figure 3 and Figure 4 The support cylinder 11 is also equipped with a cooling component 6, which includes a flow pipe 61, a support pipe 62, and a medium circulation system. The support pipe 62 is located inside the crystallizing tube 3 and is coaxially arranged with the crystallizing tube 3. The flow pipe 61 is located inside the support pipe 62 and is fixed coaxially with the support pipe 62. A recovery hole 621 is provided between the support pipe 62 and the flow pipe 61. The support pipe 62 is fixedly connected to the support cylinder 11 and supports the flow pipe 61.

[0042] Reference Figure 3 and Figure 4A heat-conducting cavity 41 is provided on the inner side of the crystallization attachment rod 4, and an opening is provided at its lower end. The flow pipe 61 extends along the opening into the heat-conducting cavity 41 of the crystallization attachment rod 4, and the outer circle of the crystallization attachment rod 4 does not contact the inner wall of the heat-conducting cavity 41. The medium circulation system is provided at the lower end of the crystallization tower 1, including a storage chamber and a circulation pump. The storage chamber is fixedly connected to the crystallization tower 1, and the storage chamber contains cooling medium. The storage chamber is provided with an input end and an output end. The input end is connected to the lower end of the flow pipe, and the circulation pump is installed on the input end. When working, it drives the cooling medium in the storage chamber to flow from the input end to the flow pipe.

[0043] Reference Figure 2 and Figure 3 The cooling medium flows into the heat-conducting cavity 41 along the flow pipe and comes into contact with the crystallization attachment rod 4. Heat exchange occurs between the rod and the solution, causing crystals to precipitate on the outer surface of the rod. The outer surface of the rod is modified to promote crystallization, facilitating crystal adhesion and growth. Furthermore, both the crystallization tube 3 and the separation tube 2 are modified to inhibit crystallization, with smooth surfaces coated with a hydrophobic layer to reduce the probability of crystal adhesion. The output end is installed at the lower end of the support tube 62 and communicates with the recovery hole 621. The cooling medium flows along the heat-conducting cavity 41 to the lower end of the crystallization tube 3, passes through the recovery hole 621, and enters the output end, ultimately being recovered from the output end into the storage chamber.

[0044] Reference Figure 2 and Figure 3 The conveying assembly 8 includes a vertical moving part 81, a horizontal moving part 82, a rotating part 83, and a clamping part 84. The vertical moving part 81 is slidably connected to the crystallization tower 1 in the vertical direction. The crystallization tower 1 is equipped with a first moving part for driving the vertical moving part 81 to move. The horizontal moving part 82 is slidably connected to the vertical moving part 81 in the radial direction of the crystallization tower 1. When the vertical moving part 81 moves, it drives the horizontal moving part 82 to move. The vertical moving part 81 is equipped with a second moving part for driving the horizontal moving part 82 to move. Both the first moving part and the second moving part are commonly used mechanisms in the prior art. In this embodiment, both the first moving part and the second moving part are motor screw mechanisms, which are prior art and will not be described in detail here.

[0045] Reference Figure 2 and Figure 3 The rotating part 83 is located on the side of the lateral moving part 82 away from the vertical moving part 81, and is rotatably connected to the lateral moving part 82 in the lateral direction. When the lateral moving part 82 moves, it drives the rotating part 83 to move synchronously. The lateral moving part 82 is equipped with a rotary motor for driving the rotating part 83 to rotate. The clamping part 84 is installed at the end of the rotating part 83 away from the lateral moving part 82 and moves synchronously with the rotating part 83. It adopts a commonly used electrically controlled gripper structure in the art. The upper end of the mounting plate 42 is fixedly connected to a clamping rod 421 for clamping by the clamping part 84.

[0046] Reference Figure 2 and Figure 3 A support frame 13 is also provided inside the crystallization tower 1. The support frame 13 is located in the middle of all crystallization tubes 3 and separation tubes 2, and the upper end of the support frame 13 is provided with a support ring adapted to the mounting surface. When the crystallization layer on the outer surface of the crystallization attachment rod 4 reaches the preset thickness, the crystallization layer needs to be peeled off. In the initial state, the vertical moving part 81 is located above the crystallization tower 1. By controlling the moving part 2 and the rotary motor to adjust the position of the rotating part 83, the clamping part 84 is located directly above the separation tube 2 assembly. The moving part 1 drives the vertical moving part 81 to move down until the clamping part 84 clamps the clamping rod 421 corresponding to the crystallization attachment rod 4 in the separation tube 2.

[0047] Reference Figure 2 and Figure 3 After clamping is completed, the vertical moving part 81 moves upward and removes the idle crystallization attachment rod 4 from the separation tube 2, and places the removed crystallization attachment rod 4 on the support frame 13, so that the support frame 13 supports and temporarily stores the crystallization attachment rod 4. After temporarily storing the crystallization attachment rod 4, the position of the clamping part 84 is adjusted again so that the clamping part 84 clamps the clamping rod 421 corresponding to the crystallization attachment rod 4 that needs to be peeled off, and the crystallization attachment rod 4 is removed from the corresponding separation tube 2. During this process, the liquid outlet pipe 52 stops supplying solution to the corresponding semi-ring block 33, and all the remaining solution in the corresponding separation tube 2 is recovered into the solution storage part 51 through the liquid inlet pipe 53.

[0048] Reference Figure 2 and Figure 4 The upper end of the crystallizing tube 3 is provided with a flow passage cavity 31. The flow passage cavity 31 is annular and arranged around the circumference of the crystallizing tube 3. Multiple nozzles 32 are arranged around the inner wall of the crystallizing tube 3. All nozzles 32 are connected to the flow passage cavity 31. When the crystallizing attachment rod 4 is inside the crystallizing tube 3, it is located between all the nozzles 32. The nozzles 32 are arranged at an angle from top to bottom from the outer circumference of the crystallizing tube 3 towards the axis.

[0049] Reference Figure 2 and Figure 4 The crystallization tower 1 is also equipped with a medium conveying system, which can be a gas cylinder or a blower. The medium conveying system is connected to a conveying pipe and, during operation, conveys the cleaning medium to the flow chamber 31 through the conveying pipe. The cleaning medium is a gas that does not react with crystallization, such as nitrogen. After entering the flow chamber 31, the gas is sprayed out along the nozzle 32 onto the crystallization attachment rod 4. During the process of the crystallization attachment rod 4 being drawn out of the crystallization tube 3, the gas blows off the residual solution on the outside of the crystallization attachment rod 4, leaving the solution inside the crystallization tube 3.

[0050] Reference Figure 2 and Figure 6After the crystallization rod 4 with the crystallization layer is removed from the crystallization tube 3, it is placed in the empty separation tube 2. The separation tube 2 is equipped with a heating element 7, which includes a heating ring 71 and a heating rod 72. The tube wall of the separation tube 2 is hollow, the heating ring 71 is located in the tube wall of the separation tube 2, and the inner wall of the separation tube 2 is provided with a heat-conducting layer. After the crystallization rod 4 enters the separation tube 2, the crystallization layer and the heat-conducting layer do not come into contact with each other.

[0051] Reference Figure 2 and Figure 6 The crystallization tower 1 is equipped with a discharge pipe 21. The lower end of the separation pipe 2 is connected to the discharge pipe 21. The heating rod 72 is located inside the separation pipe 2 and is coaxial with the separation pipe 2. The diameter of the heating rod 72 is smaller than the inner diameter of the heat conduction cavity 41. When the crystal attachment rod 4 enters the separation pipe 2, the heating rod 72 enters the heat conduction cavity 41 through the opening of the crystal attachment rod 4. The heating ring 71 and the heating rod 72 slowly heat up, thereby heating the crystal layer from both the inside and outside to perform sweating treatment. During this process, the molten impurities are discharged through the discharge pipe 21 and collected.

[0052] Reference Figure 2 and Figure 6 After sweating is complete, the heating rod 72 and heating ring 71 continue to heat up until the crystallized layer melts and drips down the outer wall of the crystallization attachment rod 4 to the bottom of the separation tube 2, and is then discharged again through the discharge pipe 21. During the sweating and heating-based crystallization process, the idle crystallization attachment rod 4 on the support frame 13 is placed into an idle crystallization tube 3 by the transport assembly 8 to continue the crystallization process. The crystallization and separation processes are carried out simultaneously, which helps to improve the crystallization production efficiency, and multiple crystallization tubes 3 are crystallized sequentially, making the crystallization and separation process continuous.

[0053] Reference Figure 2 and Figure 6 The upper end of the separation tube 2 has a cleaning chamber 22 circumferentially formed, and multiple nozzles 23 are fixedly connected to the inner wall of the separation tube 2 circumferentially. All nozzles 23 are connected to the cleaning chamber 22. When the crystallizing rod 4 is inside the separation tube 2, it is located between all the separation tubes 2. The crystallization tower 1 is also equipped with a media conveying system 2, which can be the same as the media conveying system 1. When the idle crystallizing rod 4 with the crystallized layer peeled off is extracted from the separation tube 2, the cleaning medium is conveyed to the cleaning chamber 22 through the media conveying system 2, so that the cleaning medium is sprayed out from the nozzles 23 and cleans the crystallizing rod 4. Furthermore, the crystallization tower 1 is also connected to an exhaust mechanism to discharge the cleaning medium entering the crystallization tower 1 in order to balance the air pressure inside the crystallization tower 1.

[0054] The implementation principle of the integrated crystallization and separation equipment for long-chain dicarboxylic acids in this application embodiment is as follows: A crystallization attachment rod 4 is placed in a crystallization tube 3, allowing the solution to flow between the crystallization tube 3 and the crystallization attachment rod 4. A cooling medium is supplied to the crystallization attachment rod 4 through a flow pipe 61, causing crystals to adhere to the outer wall of the crystallization attachment rod 4 and gradually grow and thicken. When the crystallization layer thickness reaches the preset requirement, the crystallization attachment rod 4 is extracted from the crystallization tube 3 by a transport component 8 and transported to a separation tube 2 for sweating and melt stripping treatment of the crystallization layer. During this process, another idle crystallization attachment rod 4 is placed in the crystallization tube 3 to continue crystallization processing, thereby facilitating the synchronous execution of the crystallization and separation processes. By adjusting the number of crystallization tubes 3 and separation tubes 2, it is helpful to achieve continuous crystallization and separation processes and improve crystallization production efficiency.

[0055] The above are all preferred embodiments of this application, and are not intended to limit the scope of protection of this application. Therefore, all equivalent changes made in accordance with the structure, shape and principle of this application should be covered within the scope of protection of this application.

Claims

1. An integrated crystallization and separation device for long-chain dicarboxylic acids, comprising a crystallization tower (1), characterized in that, Also includes: Separation tube (2) and several sets of crystallization tubes (3) are uniformly distributed around the crystallization tower (1). Separation tube (2) and crystallization tubes (3) are both set to inhibit crystallization and modify crystallization. Several sets of crystallization attachment rods (4) are provided, corresponding to the separation tube (2) and the crystallization tube (3). The outer circular surface of the crystallization attachment rod (4) is modified to promote crystallization, which facilitates the adhesion of the crystallization layer. The upper ends of the crystallization tube (3) and the separation tube (2) are provided with openings along the axial direction for the crystallization attachment rods (4) to enter and exit. The solution circulation system includes a solution storage section (51), an outlet pipe (52), and an inlet pipe (53). The solution storage section (51) is located below the crystallization tower (1) and is used to store the solution. The outlet pipe (52) and the inlet pipe (53) are both connected to the solution storage section (51). The outlet pipe (52) is connected to the upper end of the crystallization tube (3) and is used to transport the solution into the crystallization tube (3). The inlet pipe (53) is connected to the lower end of the crystallization tube (3) and is used to recover the solution flowing to the bottom of the crystallization tube (3) back to the solution storage section (51). Cooling component (6) is installed inside crystallization tube (3) and is used to cool the solution entering crystallization tube (3); A heating element (7) is installed on the separation tube (2) to heat the crystallization attachment rod (4) that enters the separation tube (2). The lower end of the separation tube (2) is connected to a discharge pipe (21). A conveying assembly (8) is provided inside the crystallization tower (1) for conveying the crystallization attachment rod (4) between the separation tube (2) and the crystallization tube (3); A support frame (13) is installed inside the crystallization tower (1) to temporarily store and support idle crystal attachment rods (4).

2. The integrated crystallization and separation equipment for long-chain dicarboxylic acids according to claim 1, characterized in that: The upper end of the crystallizing tube (3) is provided with a flow passage cavity (31) along the circumference. The flow passage cavity (31) is arranged around the crystallizing tube (3). Several nozzles (32) communicating with the flow passage cavity (31) are arranged in the circumference inside the crystallizing tube (3). When the crystallizing attachment rod (4) is located inside the crystallizing tube (3), it is located between all the nozzles (32). The crystallizing tower (1) is provided with a medium conveying system for conveying cleaning medium to the flow passage cavity (31).

3. The integrated crystallization and separation equipment for long-chain dicarboxylic acids according to claim 1, characterized in that: The cooling component (6) includes a flow pipe (61), a support pipe (62), and a medium circulation system. The support pipe (62) is coaxially arranged inside the crystallization tube (3) and fixed to the crystallization tower (1). The flow pipe (61) is coaxially fixed inside the support pipe (62) and extends along the length of the crystallization tube (3). A heat-conducting cavity (41) is opened at the lower end of the crystallization attachment rod (4) along the axial direction. The inner diameter of the heat-conducting cavity (41) is larger than the outer diameter of the flow pipe (61). The crystallization attachment rod (4) is located on the crystallization tube. (3) When the support tube (62) is in working condition, the upper end of the support tube (62) is attached to the crystal attachment rod (4). The support tube (62) has a recovery hole (621) that communicates with the heat conduction cavity (41) in the vertical direction. At this time, the flow tube (61) is located in the heat conduction cavity (41) and does not contact the inner wall of the heat conduction cavity (41). The medium circulation system is used to transport the cooling medium. It is provided with a medium input end and a recovery end. The input end is connected to the lower end of the flow tube (61), and the recovery end is connected to the recovery hole (621).

4. The integrated crystallization and separation equipment for long-chain dicarboxylic acids according to claim 1, characterized in that: In the same group of crystallization tubes (3), there are multiple crystallization tubes (3). A support cylinder (11) is fixed inside the crystallization tower (1). All crystallization tubes (3) in the same group are located inside the support cylinder (11). The upper ends of all crystallization attachment rods (4) in the same group are fixed with the same mounting plate (42). When the transport component (8) is working, it drives all the corresponding crystallization attachment rods (4) to move through the mounting plate (42). A sealing plate (111) is fixed at the upper end of the support cylinder (11). The sealing plate (111) has a through hole that is adapted to the crystallization attachment rod (4) in the vertical direction. When the crystallization attachment rod (4) is located inside the crystallization tube (3) and is in working condition, the lower end face of the mounting plate (42) is attached to the upper end face of the sealing plate (111) and the through hole is blocked.

5. The integrated crystallization and separation equipment for long-chain dicarboxylic acids according to claim 4, characterized in that: The upper end of the crystallizing tube (3) is slidably connected to two semi-ring blocks (33). The two semi-ring blocks (33) are arranged opposite each other with respect to the axis of the crystallizing tube (3) and move in the direction of approaching or moving away from each other. The support cylinder (11) is provided with a power component for driving the semi-ring blocks (33) to open and close. When the crystallizing attachment rod (4) is located inside the crystallizing tube (3), it is between the two semi-ring blocks (33) and fits against the semi-ring blocks (33). The semi-ring blocks (33) have a buffer cavity (331) that communicates with the liquid outlet pipe (52). The liquid outlet pipe (52) communicates with the buffer cavity (331). The lower end of the semi-ring blocks (33) has a drain port (332) that communicates with the buffer cavity (331). The drain port (332) is arc-shaped and surrounds the crystallizing attachment rod (4).

6. The integrated crystallization and separation equipment for long-chain dicarboxylic acids according to claim 5, characterized in that: The semi-ring block (33) is provided with a pressure valve plate (333) at the drain port (332). The pressure valve plate (333) blocks the drain port (332) in its natural state. When the outlet pipe (52) delivers the solution into the buffer chamber (331), the pressure valve plate (333) opens under the pressure of the solution and guides the solution to flow towards the crystal adhesion rod (4).

7. The integrated crystallization and separation equipment for long-chain dicarboxylic acids according to claim 3, characterized in that: The heating element (7) includes a heating ring (71) and a heating rod (72). The separation tube (2) has a cavity along the axial direction. The heating ring (71) is placed in the cavity and extends along the axial direction of the separation tube (2). The inner wall of the separation tube (2) is provided with a heat-conducting layer to guide the heat of the heating ring (71) to radiate to the crystallization attachment rod (4). The heating rod (72) is fixed on the crystallization tower (1) and coaxially arranged inside the separation tube (2). The outer diameter of the heating rod (72) is smaller than the inner diameter of the heat-conducting cavity (41).

8. The integrated crystallization and separation equipment for long-chain dicarboxylic acids according to claim 1, characterized in that: The upper end of the separation tube (2) has a cleaning chamber (22) circumferentially open, and the inner wall of the separation tube (2) is provided with a number of nozzles (23) communicating with the cleaning chamber (22) circumferentially. When the crystallization attachment rod (4) is located inside the separation tube (2), it is located between all the nozzles (23), and the nozzles (23) are inclined from top to bottom towards the axis of the separation tube (2). The crystallization tower (1) is provided with a medium conveying system (2) for conveying the cleaning medium to the cleaning chamber (22).

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