Supercritical fluid extraction device for sitagliptin phosphate intermediate

By designing a supercritical fluid extraction device including a separation mechanism and a guide mechanism, the defects of the existing device in temperature control, kettle body structure, and separation system are solved, and efficient extraction of sitagliptin phosphate intermediates and recycling of finished products are achieved, improving the stability and purity of the extraction process.

CN120189729APending Publication Date: 2025-06-24YANCHENG DAFENG AREA TIANSHENG JOINT PHARM CO LTD
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Patent Information

Application Number
CN202510370466.9
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-03-27
Publication Date
2025-06-24

AI Technical Summary

Technical Problem

The existing supercritical fluid extraction device for sitagliptin phosphate intermediate has defects in temperature control, kettle body structure, and separation system, resulting in low extraction efficiency, difficult to guarantee purity, and lack of centralized treatment of residues and rapid separation structure of finished products.

Method used

A supercritical fluid extraction device including a separation mechanism and a guide mechanism is designed. The separation mechanism realizes the extraction of the sitagliptin phosphate intermediate and the separation and discharge of residues through the coordination of the transmission component, the reaction component, the discharge component and the buffer component. The guide mechanism realizes the circulating conveying of raw materials and centralized treatment of impurities through the coordination of the feeding assembly, the guide assembly, the backtracking assembly and the return assembly.

Benefits of technology

The extraction efficiency of the sitagliptin phosphate intermediate and the recovery stability of the finished product are improved, centralized treatment of residues and rapid separation of the finished product are achieved, and the overall stability and purity of the extraction process are improved.

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Abstract

The invention relates to the technical field of extraction, in particular to a sitagliptin phosphate intermediate supercritical fluid extraction device which comprises a separation mechanism and a guide mechanism, the guide mechanism is arranged on the inner side of the separation mechanism, and the separation mechanism comprises a transmission assembly, a reaction assembly, a discharge assembly and a buffer assembly. The reaction assembly is fixedly connected to the top of the transmission assembly, the discharge assembly is rotatably connected to the inner side of the transmission assembly, and the buffer assembly is fixedly connected to the bottom of the transmission assembly. The invention provides a supercritical fluid extraction device for a sitagliptin phosphate intermediate, which is provided with a structure for centrally guiding residues everywhere in the device in the extraction process, so that the residues can be centrally treated, the efficiency in the extraction process of the sitagliptin phosphate intermediate is improved, and a structure for separating the residues from finished products is arranged, so that the extraction efficiency is improved. Therefore, the residue can be quickly separated from the finished product, and the recovery stability of the sitagliptin phosphate intermediate finished product after extraction is improved.
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Description

Technical Field

[0001] The present invention relates to the technical field of extraction, and specifically to a supercritical fluid extraction device for sitagliptin phosphate intermediate. Background Art

[0002] As is well known, in pharmaceutical synthesis, the extraction of sitagliptin phosphate intermediate is crucial. Traditional extraction technologies, such as liquid-liquid and solid-liquid extraction, have problems such as environmental pollution, solvent residue, low efficiency, and difficulty in ensuring purity. The supercritical fluid extraction technology uses a fluid with both gas and liquid advantages to efficiently extract the intermediate. However, the existing devices have defects in temperature control, kettle body structure, and separation system. Therefore, the research and development of a new device is of great significance for efficient and high-purity extraction.

[0003] After retrieval, the Chinese patent discloses a double-kettle flipping supercritical fluid extraction device, and its application publication number is: CN106833883B. This patent includes a motor arranged on a first support, a transmission shaft arranged on the power output shaft of the motor, a second support and a third support arranged on the transmission shaft. A fixed disk is fixed on the upper part of the second support, and a traveling mechanism is arranged at the bottom. The transmission shaft passes through the fixed disk, and a rotating disk and an extraction kettle support rod are sequentially fixed on the transmission shaft. The two ends of the extraction kettle support rod are respectively fixed with a left extraction kettle and a right extraction kettle. One port of a fifth three-way valve arranged on the rotating disk is connected to the liquid inlet hole on the fixed disk through a pipeline, and the other two ports are respectively connected to the left extraction kettle and the right extraction kettle through pipelines. One port of a sixth three-way valve arranged on the rotating disk is connected to the liquid outlet hole on the fixed disk, and the other two ports are respectively connected to the left extraction kettle and the right extraction kettle through pipelines.

[0004] When using supercritical fluid to extract sitagliptin phosphate intermediate, residues will be generated everywhere in the extraction equipment during the extraction process, which will reduce the quality during extraction. The problems existing in the prior art are: due to the lack of a structure for centrally guiding the residues everywhere in the equipment during the extraction process, the residues cannot be centrally processed, which reduces the efficiency during the extraction process of sitagliptin phosphate intermediate, and due to the lack of a structure for separating the residues and the finished product, the residues and the finished product cannot be quickly separated, which reduces the stability of the recovery of the sitagliptin phosphate intermediate finished product after extraction. Summary of the Invention

[0005] (I) Technical Problems to be Solved

[0006] In view of the deficiencies of the prior art, the present invention provides a supercritical fluid extraction device for sitagliptin phosphate intermediates, which has a structure for centrally guiding residues at various parts inside the equipment during the extraction process. Therefore, the residues can be centrally processed, improving the efficiency of the extraction process of sitagliptin phosphate intermediates. And it has a structure for separating residues and finished products. Therefore, the residues and finished products can be quickly separated, improving the recovery stability of the sitagliptin phosphate intermediate finished product after extraction.

[0007] (2) Technical solution

[0008] The above technical objectives of the present invention are achieved through the following technical solutions: A supercritical fluid extraction device for sitagliptin phosphate intermediates includes a separation mechanism and a guiding mechanism. The guiding mechanism is arranged inside the separation mechanism. The separation mechanism includes a transmission component, a reaction component, a discharge component, and a buffer component. The reaction component is fixedly connected to the top of the transmission component. The discharge component is rotatably connected to the inside of the transmission component. The buffer component is fixedly connected to the bottom of the transmission component. The guiding mechanism includes a feeding component, a guiding component, a backtracking component, a reflux component, and a supply component. The feeding component is fixedly connected to the top inside the reaction component. The guiding component is fixedly connected to the surface of the feeding component. The backtracking component is fixedly connected to the bottom of the feeding component. The reflux component is fixedly connected to the inside of the guiding component. The supply component is communicated with the bottom of the feeding component. The bottom of the supply component is fixedly connected to the top of the discharge component.

[0009] By adopting the above technical solutions, through the setting of the separation mechanism and the guiding mechanism, the separation mechanism can separate the residues generated during the supercritical fluid extraction of sitagliptin phosphate intermediates and discharge the finished products after the supercritical fluid extraction of sitagliptin phosphate intermediates. The guiding mechanism can reciprocally circulate and transport the sitagliptin phosphate intermediate raw materials and can centrally transport the residues generated during the extraction to the separation mechanism.

[0010] The present invention is further set as: The transmission component includes a positioning ring seat, a support plate, and a transmission servo motor. The support plate is fixedly connected to the bottom of the positioning ring seat. The transmission servo motor is fixedly connected to the inside of the support plate.

[0011] By adopting the above technical solutions, through the setting of the transmission component, the positioning ring seat can cooperate with the support plate and the transmission servo motor. By supporting the support plate through the positioning ring seat, the transmission servo motor can be supported, increasing the structural stability of the transmission servo motor. At the same time, it can form a sealed environment with the reaction component and the discharge component. The transmission servo motor can provide power for the supply component, so that the overall structure of the guiding mechanism can operate.

[0012] The present invention is further configured such that: the reaction assembly includes a reaction kettle, an interception mesh cover, and a positioning cover. The reaction kettle is fixedly connected to the top of the positioning ring seat. The interception mesh cover is fixedly connected to the bottom inside the reaction kettle. The positioning cover is snap - connected to the top of the reaction kettle.

[0013] With the above - mentioned technical solution, by setting the reaction assembly, the reaction kettle can cooperate with the interception mesh cover and the positioning cover. By forming a sealed environment with the positioning ring seat and the discharge assembly, it can provide space for the supercritical fluid extraction operation of the sitagliptin phosphate intermediate. The interception mesh cover can intercept the impurities generated during extraction and separate the finished product of the sitagliptin phosphate intermediate after extraction into the reaction kettle, so as to facilitate the removal of the finished product. The positioning cover can facilitate the opening of the reaction kettle to maintain the internal structure or add reaction materials.

[0014] The present invention is further configured such that: the discharge assembly includes a conduction ring, a guiding cone barrel, a discharge valve, and a conduction rotating rod. The conduction ring is fixedly connected to the inside of the positioning ring seat. The guiding cone barrel is fixedly connected to the inside of the conduction ring. The discharge valve is communicated with the bottom of the guiding cone barrel. The conduction rotating rod is rotatably connected to the top of the guiding cone barrel. The bottom of the conduction rotating rod is fixedly connected to the output end of the top of the driving servo motor.

[0015] With the above - mentioned technical solution, by setting the discharge assembly, the conduction ring can cooperate with the guiding cone barrel, the discharge valve, and the conduction rotating rod. By limiting the guiding cone barrel through the conduction ring, the guiding cone barrel can guide the impurities generated during extraction to the discharge valve. The discharge valve can discharge the impurities. The conduction rotating rod can drive the supply assembly to rotate along with the drive of the driving servo motor, thereby providing power for the operation of the guiding mechanism.

[0016] The present invention is further configured such that: the buffer assembly includes a support seat, a gas spring rod, and a guiding telescopic rod. The support seat is fixedly connected to the bottom of the positioning ring seat. The gas spring rod is fixedly connected to the bottom of the support seat. The guiding telescopic rod is fixedly connected to the side of the support seat away from the gas spring rod.

[0017] With the above - mentioned technical solution, by setting the buffer assembly, the support seat can cooperate with the gas spring rod and the guiding telescopic rod. By limiting the gas spring rod through the support seat, the gas spring rod can buffer the vibration generated during the operation of the guiding mechanism through its own elasticity. The guiding telescopic rod can reinforce the support seat and further increase the stability of the gas spring rod during buffering.

[0018] The present invention is further configured such that: the feeding assembly includes a feeding pump, a guiding rotating plate, and a receiving pipe. The feeding pump is communicated with the bottom of the positioning cover. The guiding rotating plate is rotatably connected to the bottom of the feeding pump. The receiving pipe is communicated with the top of the feeding pump. The top of the receiving pipe penetrates through the top of the positioning cover and is communicated with the positioning cover.

[0019] With the above technical solution, by setting up the feeding component, the feeding pump can cooperate with the guiding rotating plate and the material receiving pipe. The feeding pump can convey the sitagliptin phosphate intermediate raw material to the supply component. The guiding rotating plate can drive the guiding component, the backtracking component and the reflux component to rotate together with the rotation of the supply component, so as to provide guidance for the power required for centralized conveying of impurities. The material receiving pipe can be externally connected to the sitagliptin phosphate intermediate raw material conveying equipment to convey the sitagliptin phosphate intermediate raw material to the feeding pump.

[0020] The present invention is further configured as: the guiding component includes a drainage cone barrel, a transmission ring and a traction sleeve. The drainage cone barrel is fixedly connected to the surface of the guiding rotating plate. The transmission ring is fixedly connected to the bottom of the drainage cone barrel. The traction sleeve is welded to the inner side of the transmission ring.

[0021] With the above technical solution, by setting up the guiding component, the drainage cone barrel can cooperate with the transmission ring and the traction sleeve. The impurities generated during extraction can be guided by the drainage cone barrel, and the impurities can be further concentrated at the backtracking component, so that the backtracking component can guide the impurities to the guiding cone barrel for easy recovery of the impurities. Moreover, the drainage cone barrel can drive the transmission ring to rotate together with the guiding rotating plate, and can also drive the backtracking component to rotate. The transmission ring can drive the traction sleeve to rotate together with the drainage cone barrel, so that the traction sleeve can drive the reflux component to rotate together.

[0022] The present invention is further configured as: the backtracking component includes a backtracking drainage pipe, a backtracking drainage tube and a backtracking diversion opening. The backtracking drainage pipe is fixedly connected to the bottom of the guiding rotating plate. The backtracking drainage tube is communicated with the bottom of the backtracking drainage pipe. The backtracking diversion openings are respectively opened on the surface of the backtracking drainage pipe and the bottom of the surface of the backtracking drainage tube.

[0023] With the above technical solution, by setting up the backtracking component, the backtracking drainage pipe can cooperate with the backtracking drainage tube and the backtracking diversion opening. The impurities can be guided from the backtracking drainage pipe to the backtracking drainage tube through the backtracking diversion opening, and the backtracking drainage tube can centrally discharge the impurities from the backtracking diversion opening to the guiding cone barrel through centrifugal force.

[0024] The present invention is further configured as: the reflux component includes a reflux drainage pipe, a reflux drainage tube and a reflux diversion opening. The reflux drainage pipe is clamped inside the traction sleeve. The reflux drainage tube is communicated with the bottom of the reflux drainage pipe. The reflux diversion openings are respectively opened on the surface of the reflux drainage pipe and the bottom of the surface of the reflux drainage tube.

[0025] With the above technical solution, by setting up a reflux assembly, the reflux drain pipe can cooperate with the reflux drainage pipe and the reflux diversion port. The impurities can be transported from the reflux diversion port to the reflux drain pipe by the reflux drainage pipe using centrifugal force, enabling the reflux drain pipe to centrally transport the impurities generated during the extraction process to the drainage cone bucket, and the drainage cone bucket transports the impurities to the backtracking assembly.

[0026] The present invention is further configured as follows: The supply assembly includes a feed pipe, a positioning rod, and a spiral conveyor plate. The feed pipe is connected to the bottom of the feed pump, the bottom of the feed pipe is fixedly connected to the top of the conduction rotating rod, the positioning rod is fixedly connected to the inner side of the feed pipe, and the spiral conveyor plate is fixedly connected to the surface of the positioning rod.

[0027] With the above technical solution, by setting up a supply assembly, the feed pipe can cooperate with the positioning rod and the spiral conveyor plate. The sitagliptin phosphate intermediate raw material can be transported to the spiral conveyor plate through the feed pipe. When the positioning rod rotates with the feed pipe, it can drive the spiral conveyor plate to rotate together, and evenly transport the sitagliptin phosphate intermediate raw material to each part of the feed pipe through the spiral conveyor plate, so that the feed pipe can evenly transport the sitagliptin phosphate intermediate raw material into the reaction kettle for extraction treatment through the holes on its own surface.

[0028] (III) Beneficial effects

[0029] Compared with the prior art, the present invention provides a supercritical fluid extraction device for sitagliptin phosphate intermediate, which has the following beneficial effects:

[0030] For the supercritical fluid extraction device for sitagliptin phosphate intermediate, by setting up a separation mechanism, the transmission assembly can cooperate with the reaction assembly, the discharge assembly, and the buffer assembly. By forming a sealed structure between the transmission assembly and the reaction assembly and the discharge assembly, the transmission assembly can drive the guiding mechanism to operate for extracting the supercritical fluid of sitagliptin phosphate intermediate. The reaction assembly can intercept the residues generated during extraction and separate the finished products. The discharge assembly can centrally store the residues and can centrally discharge the residues. The buffer assembly can buffer the vibration of the entire separation mechanism driven by the guiding mechanism during operation, which can improve the stability of the separation mechanism during extraction;

[0031] The supercritical fluid extraction device for sitagliptin phosphate intermediate can cooperate with the guiding component, the backtracking component, the reflux component and the supply component by setting up the guiding mechanism. By connecting the feeding component to the raw material conveying equipment of sitagliptin phosphate intermediate, the raw material can be conveyed to the supply component. The supply component can drive the feeding component to rotate together with the transmission of the separation mechanism, so that the feeding component drives the guiding component, the backtracking component and the reflux component to rotate together, and evenly conveys the raw material into the separation mechanism for extraction by supercritical fluid. When the guiding component, the backtracking component and the reflux component rotate, the impurities generated during extraction can be conveyed to the guiding component through the reflux component, centrally conveyed to the backtracking component through the guiding component, and finally centrally conveyed to the separation mechanism through the backtracking component to achieve the effect of centralized impurity treatment. Description of the Drawings

[0032] Figure 1 Schematic diagram of the overall structure in the present invention;

[0033] Figure 2 Schematic diagram of the connection between the separation mechanism and the guiding mechanism in the present invention;

[0034] Figure 3 Schematic diagram of the structure of the separation mechanism in the present invention;

[0035] Figure 4 Schematic diagram of the structure of the buffer component and the reaction component in the present invention;

[0036] Figure 5 Schematic diagram of the structure of the discharge component and the buffer component in the present invention;

[0037] Figure 6 Schematic diagram of the structure of the guiding mechanism in the present invention;

[0038] Figure 7 Schematic diagram of the structure of the transmission component and the guiding component in the present invention;

[0039] Figure 8 Schematic diagram of the structure of the backtracking component in the present invention;

[0040] Figure 9 Schematic diagram of the structure of the reflux component in the present invention;

[0041] Figure 10 Schematic diagram of the structure of the supply component in the present invention.

[0042] In the figure: 1. Separation mechanism; 11. Transmission component; 111. Positioning ring seat; 112. Support plate; 113. Transmission servo motor; 12. Reaction component; 121. Reaction kettle; 122. Intercepting mesh cover; 123. Positioning cover; 13. Discharge component; 131. Conduction ring; 132. Guide cone; 133. Discharge valve; 134. Conduction rotating rod; 14. Buffer component; 141. Support seat; 142. Gas spring rod; 143. Guide telescopic rod; 2. Guide mechanism; 21. Feeding component; 211. Feed pump; 212. Guide rotating plate; 213. Material receiving pipe; 22. Guide component; 221. Drainage cone; 222. Transmission ring; 223. Traction sleeve; 23. Backtracking component; 231. Backtracking drainage pipe; 232. Backtracking drainage tube; 233. Backtracking diversion port; 24. Return component; 241. Return drainage pipe; 242. Return drainage tube; 243. Return diversion port; 25. Supply component; 251. Feed pipe; 252. Positioning rod; 253. Screw conveyor plate. Detailed implementation manners

[0043] Next, the technical solutions in the embodiments of the present invention will be clearly and completely described in conjunction with the accompanying drawings in the embodiments of the present invention. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative efforts shall fall within the protection scope of the present invention.

[0044] Embodiment 1

[0045] Please refer to Figure 1-5 , a supercritical fluid extraction device for sitagliptin phosphate intermediate, including a separation mechanism 1. The separation mechanism 1 includes a transmission component 11, a reaction component 12, a discharge component 13, and a buffer component 14. The reaction component 12 is fixedly connected to the top of the transmission component 11. The discharge component 13 is rotatably connected to the inside of the transmission component 11. The buffer component 14 is fixedly connected to the bottom of the transmission component 11. By setting the separation mechanism 1, the transmission component 11 can cooperate with the reaction component 12, the discharge component 13, and the buffer component 14. A sealing structure can be formed between the transmission component 11 and the reaction component 12 and the discharge component 13, so that the transmission component 11 can drive the guide mechanism 2 to operate to extract the supercritical fluid of the sitagliptin phosphate intermediate. The reaction component 12 can intercept the residues generated during extraction and separate the finished products. The discharge component 13 can concentrate and store the residues and can discharge the residues centrally. The buffer component 14 can buffer the vibration of the entire separation mechanism 1 driven by the operation of the guide mechanism 2, which can improve the stability of the separation mechanism 1 during extraction.

[0046] Among them, the transmission assembly 11 includes a positioning ring seat 111, a support plate 112, and a transmission servo motor 113. The support plate 112 is fixedly connected to the bottom of the positioning ring seat 111, and the transmission servo motor 113 is fixedly connected to the inner side of the support plate 112. By setting the transmission assembly 11, the positioning ring seat 111 can cooperate with the support plate 112 and the transmission servo motor 113. By supporting the support plate 112 through the positioning ring seat 111, the transmission servo motor 113 can be supported, increasing the structural stability of the transmission servo motor 113. At the same time, a closed environment can be formed with the reaction assembly 12 and the discharge assembly 13. The transmission servo motor 113 can provide power for the supply assembly 25, so that the overall structure of the guiding mechanism 2 can operate.

[0047] Among them, the reaction assembly 12 includes a reaction kettle 121, an interception mesh cover 122, and a positioning cover 123. The reaction kettle 121 is fixedly connected to the top of the positioning ring seat 111, the interception mesh cover 122 is fixedly connected to the bottom inside the reaction kettle 121, and the positioning cover 123 is snap-connected to the top of the reaction kettle 121. By setting the reaction assembly 12, the reaction kettle 121 can cooperate with the interception mesh cover 122 and the positioning cover 123. By forming a closed environment with the positioning ring seat 111 and the discharge assembly 13 through the reaction kettle 121, a space can be provided for the supercritical fluid extraction operation of the sitagliptin phosphate intermediate. The interception mesh cover 122 can intercept the impurities generated during extraction and separate the finished product of the sitagliptin phosphate intermediate after extraction into the reaction kettle 121, so that the finished product can be easily taken out. The positioning cover 123 can facilitate the opening of the reaction kettle 121, so as to maintain the internal structure or add reaction materials.

[0048] Among them, the discharge assembly 13 includes a conduction ring 131, a guiding cone barrel 132, a discharge valve 133, and a conduction rotating rod 134. The conduction ring 131 is fixedly connected to the inner side of the positioning ring seat 111, the guiding cone barrel 132 is fixedly connected to the inner side of the conduction ring 131, the discharge valve 133 is connected to the bottom of the guiding cone barrel 132, and the conduction rotating rod 134 is rotatably connected to the top of the guiding cone barrel 132. The bottom of the conduction rotating rod 134 is fixedly connected to the output end of the top of the transmission servo motor 113. By setting the discharge assembly 13, the conduction ring 131 can cooperate with the guiding cone barrel 132, the discharge valve 133, and the conduction rotating rod 134. By limiting the guiding cone barrel 132 through the conduction ring 131, the guiding cone barrel 132 can guide the impurities generated during extraction to the discharge valve 133. The discharge valve 133 can discharge the impurities. The conduction rotating rod 134 can drive the supply assembly 25 to rotate along with the transmission of the transmission servo motor 113, so as to provide power for the operation of the guiding mechanism 2.

[0049] Among them, the buffer assembly 14 includes a support base 141, a gas spring rod 142, and a guiding telescopic rod 143. The support base 141 is fixedly connected to the bottom of the positioning ring base 111. The gas spring rod 142 is fixedly connected to the bottom of the support base 141. The guiding telescopic rod 143 is fixedly connected to the side of the support base 141 away from the gas spring rod 142. By setting the buffer assembly 14, the support base 141 can cooperate with the gas spring rod 142 and the guiding telescopic rod 143. By limiting the gas spring rod 142 through the support base 141, the gas spring rod 142 can buffer the vibration generated during the operation of the guiding mechanism 2 through its own elasticity. The guiding telescopic rod 143 can reinforce the support base 141, and can further increase the stability of the gas spring rod 142 during buffering.

[0050] Working principle of this embodiment: First, the driving servo motor 113 drives the conduction rotating rod 134 to rotate the guiding mechanism 2, so that the guiding mechanism 2 conveys the raw materials into the reaction kettle 121. The guiding mechanism 2 will extract the raw materials. Then, the gas spring rod 142 will buffer the vibration generated during the extraction of the guiding mechanism 2. After that, when the guiding mechanism 2 extracts the raw materials and concentrates the impurities, the intercepting mesh cover 122 will intercept the impurities in the guiding cone 132. Then, the guiding cone 132 will concentrate and guide the impurities to the discharge valve 133. Finally, the impurities can be discharged through the discharge valve 133.

[0051] Embodiment 2

[0052] Reference Figure 6-10, A supercritical fluid extraction device for sitagliptin phosphate intermediate further includes a guiding mechanism 2. Among them, the guiding mechanism 2 includes a feeding component 21, a guiding component 22, a backtracking component 23, a reflux component 24, and a supply component 25. The feeding component 21 is fixedly connected to the top inside the reaction component 12. The guiding component 22 is fixedly connected to the surface of the feeding component 21. The backtracking component 23 is fixedly connected to the bottom of the feeding component 21. The reflux component 24 is fixedly connected to the inside of the guiding component 22. The supply component 25 is communicated with the bottom of the feeding component 21. The bottom of the supply component 25 is fixedly connected to the top of the discharge component 13. By setting the guiding mechanism 2, the feeding component 21 can cooperate with the guiding component 22, the backtracking component 23, the reflux component 24, and the supply component 25. By externally connecting the raw material conveying equipment for sitagliptin phosphate intermediate to the feeding component 21, the raw materials can be conveyed to the supply component 25. The supply component 25 can drive the feeding component 21 to rotate together with the transmission of the separation mechanism 1, so that the feeding component 21 drives the guiding component 22, the backtracking component 23, and the reflux component 24 to rotate together, and uniformly conveys the raw materials into the separation mechanism 1 for extraction by supercritical fluid. When the guiding component 22, the backtracking component 23, and the reflux component 24 rotate, the impurities generated during extraction can be conveyed to the guiding component 22 through the reflux component 24, centrally conveyed to the backtracking component 23 through the guiding component 22, and finally centrally conveyed to the separation mechanism 1 through the backtracking component 23 to achieve the effect of centralized impurity treatment.

[0053] Among them, the feeding component 21 includes a feeding pump 211, a guiding rotating plate 212, and a material receiving pipe 213. The feeding pump 211 is communicated with the bottom of the positioning cover 123. The guiding rotating plate 212 is rotatably connected to the bottom of the feeding pump 211. The material receiving pipe 213 is communicated with the top of the feeding pump 211. The top of the material receiving pipe 213 penetrates through the top of the positioning cover 123 and is communicated with the positioning cover 123. By setting the feeding component 21, the feeding pump 211 can cooperate with the guiding rotating plate 212 and the material receiving pipe 213. The feeding pump 211 can convey the sitagliptin phosphate intermediate raw materials to the supply component 25. The guiding rotating plate 212 can drive the guiding component 22, the backtracking component 23, and the reflux component 24 to rotate together with the rotation of the supply component 25, so as to provide guidance for the power required for centralized impurity conveyance. The material receiving pipe 213 can be externally connected to the raw material conveying equipment for sitagliptin phosphate intermediate to convey the sitagliptin phosphate intermediate raw materials to the feeding pump 211.

[0054] Among them, the guiding component 22 includes a drainage cone 221, a transmission ring 222, and a traction sleeve 223. The drainage cone 221 is fixedly connected to the surface of the guiding rotating plate 212. The transmission ring 222 is fixedly connected to the bottom of the drainage cone 221. The traction sleeve 223 is welded to the inner side of the transmission ring 222. By setting the guiding component 22, the drainage cone 221 can cooperate with the transmission ring 222 and the traction sleeve 223. The drainage cone 221 can guide the impurities generated during extraction, and further concentrate the impurities at the backtracking component 23, so that the backtracking component 23 can guide the impurities to the guiding cone 132 for impurity recovery. Moreover, the drainage cone 221 can drive the transmission ring 222 to rotate together with the guiding rotating plate 212, and can also drive the backtracking component 23 to rotate together. The transmission ring 222 can drive the traction sleeve 223 to rotate together with the drainage cone 221, so that the traction sleeve 223 can drive the reflux component 24 to rotate together.

[0055] Among them, the backtracking component 23 includes a backtracking drainage pipe 231, a backtracking drainage tube 232, and a backtracking diversion port 233. The backtracking drainage pipe 231 is fixedly connected to the bottom of the guiding rotating plate 212. The backtracking drainage tube 232 is connected to the bottom of the backtracking drainage pipe 231. The backtracking diversion ports 233 are respectively opened on the surface of the backtracking drainage pipe 231 and the bottom of the surface of the backtracking drainage tube 232. By setting the backtracking component 23, the backtracking drainage pipe 231 can cooperate with the backtracking drainage tube 232 and the backtracking diversion ports 233. The impurities can be guided from the backtracking drainage pipe 231 to the backtracking drainage tube 232 through the backtracking diversion ports 233, and the backtracking drainage tube 232 can concentrate and discharge the impurities from the backtracking diversion ports 233 to the guiding cone 132 by centrifugal force.

[0056] Among them, the reflux component 24 includes a reflux drainage pipe 241, a reflux drainage tube 242, and a reflux diversion port 243. The reflux drainage pipe 241 is clamped inside the traction sleeve 223. The reflux drainage tube 242 is connected to the bottom of the reflux drainage pipe 241. The reflux diversion ports 243 are respectively opened on the surface of the reflux drainage pipe 241 and the bottom of the surface of the reflux drainage tube 242. By setting the reflux component 24, the reflux drainage pipe 241 can cooperate with the reflux drainage tube 242 and the reflux diversion ports 243. The impurities can be transported from the reflux diversion ports 243 to the reflux drainage pipe 241 by the reflux drainage tube 242 using centrifugal force. The reflux drainage pipe 241 can concentrate and transport the impurities generated during the extraction process to the drainage cone 221, and the drainage cone 221 can transport the impurities to the backtracking component 23.

[0057] Among them, the supply component 25 includes a supply pipe 251, a positioning rod 252 and a spiral conveying plate 253. The supply pipe 251 is connected to the bottom of the feed pump 211, the bottom of the supply pipe 251 is fixedly connected to the top of the conductive rotating rod 134, the positioning rod 252 is fixedly connected to the inner side of the supply pipe 251, and the spiral conveying plate 253 is fixedly connected to the surface of the positioning rod 252. By setting the supply component 25, the supply pipe 251 can cooperate with the positioning rod 252 and the spiral conveying plate 253, and the intermediate raw material of sitagliptin phosphate is transported to the spiral conveying plate 253 through the supply pipe 251. The positioning rod 252 can drive the spiral conveying plate 253 to rotate with the rotation of the supply pipe 251, and the intermediate raw material of sitagliptin phosphate is evenly transported to each part of the supply pipe 251 through the spiral conveying plate 253, so that the supply pipe 251 can evenly transport the intermediate raw material of sitagliptin phosphate to the reactor 121 through the holes on its surface for extraction treatment.

[0058] The working principle of this embodiment is as follows: first, the receiving pipe 213 is connected to the raw material conveying equipment, and then the raw material is conveyed to the feed pipe 251 through the feed pump 211. After that, the feed pipe 251 will drive the positioning rod 252 and the guide rotating plate 212 to rotate with the rotation of the separation mechanism 1. When the positioning rod 252 rotates, it will drive the spiral conveying plate 253 to evenly convey the raw material to various places in the feed pipe 251, and then discharge it into the supercritical fluid through the feed pipe 251. Then, the guide rotating plate 212 will drive the drainage cone barrel 221, the backflow drainage pipe 231 and the reflux drainage pipe 241 to rotate. The reflux drainage pipe 242 will remove the impurities generated in the extraction through the reflux drainage pipe 241 when it rotates. The reflux guide port 243 is transported to the reflux drainage pipe 241, and then discharged into the drainage cone barrel 221 through the reflux guide port 243 at the reflux drainage pipe 241. The drainage cone barrel 221 will guide the impurities to the tracing guide port 233, and rotate the traction sleeve 223 through the transmission ring 222. The traction sleeve 223 will drive the tracing drainage pipe 231 to rotate, and then the tracing drainage pipe 231 will drive the tracing drainage pipe 232 to move together. The tracing drainage pipe 232 will transport the impurities to the tracing guide port 233 at the tracing drainage pipe 232 when moving, and finally discharge them to the discharge port of the separation mechanism 1 through the tracing guide port 233.

[0059] This specific embodiment is only an explanation of the present invention, and it is not a limitation of the present invention. After reading this specification, those skilled in the art can make non-creative modifications to the present embodiment as needed. Although the embodiments of the present invention have been shown and described, it is understandable to those of ordinary skill in the art that various changes, modifications, substitutions and variations can be made to these embodiments without departing from the principle and spirit of the present invention. The scope of the present invention is defined by the appended claims and their equivalents.

Claims

1. A supercritical fluid extraction device for sitagliptin phosphate intermediates, comprising a separation mechanism (1) and a guide mechanism (2), characterized in that: The guide mechanism (2) is arranged on the inner side of the separation mechanism (1); the separation mechanism (1) comprises a transmission component (11), a reaction component (12), a discharge component (13) and a buffer component (14); the reaction component (12) is fixedly connected to the top of the transmission component (11); the discharge component (13) is rotatably connected to the inner side of the transmission component (11); the buffer component (14) is fixedly connected to the bottom of the transmission component (11); the guide mechanism (2) comprises a feeding component (21), a guide component (22), a backtracking component (21); 3), a reflux component (24) and a supply component (25), wherein the feed component (21) is fixedly connected to the top of the inner side of the reaction component (12), the guide component (22) is fixedly connected to the surface of the feed component (21), the tracing component (23) is fixedly connected to the bottom of the feed component (21), the reflux component (24) is fixedly connected to the inner side of the guide component (22), the supply component (25) is connected to the bottom of the feed component (21), and the bottom of the supply component (25) is fixedly connected to the top of the discharge component (13).

2. A supercritical fluid extraction device for sitagliptin phosphate intermediate according to claim 1, characterized in that: The transmission assembly (11) comprises a positioning ring seat (111), a support plate (112) and a transmission servo motor (113); the support plate (112) is fixedly connected to the bottom of the positioning ring seat (111); and the transmission servo motor (113) is fixedly connected to the inner side of the support plate (112).

3. A supercritical fluid extraction device for sitagliptin phosphate intermediate according to claim 2, characterized in that: The reaction assembly (12) comprises a reaction kettle (121), an intercepting mesh cover (122) and a positioning cover (123); the reaction kettle (121) is fixedly connected to the top of the positioning ring seat (111); the intercepting mesh cover (122) is fixedly connected to the bottom of the inner side of the reaction kettle (121); and the positioning cover (123) is clamped on the top of the reaction kettle (121).

4. A supercritical fluid extraction device for sitagliptin phosphate intermediate according to claim 2, characterized in that: The discharge assembly (13) comprises a conduction ring (131), a guide cone barrel (132), a discharge valve (133) and a conduction rotating rod (134); the conduction ring (131) is fixedly connected to the inner side of the positioning ring seat (111); the guide cone barrel (132) is fixedly connected to the inner side of the conduction ring (131); the discharge valve (133) is connected to the bottom of the guide cone barrel (132); the conduction rotating rod (134) is rotatably connected to the top of the guide cone barrel (132); and the bottom of the conduction rotating rod (134) is fixedly connected to the output end of the top of the transmission servo motor (113).

5. A supercritical fluid extraction device for sitagliptin phosphate intermediate according to claim 2, characterized in that: The buffer assembly (14) comprises a support seat (141), a gas spring rod (142) and a guide telescopic rod (143); the support seat (141) is fixedly connected to the bottom of the positioning ring seat (111); the gas spring rod (142) is fixedly connected to the bottom of the support seat (141); and the guide telescopic rod (143) is fixedly connected to a side of the support seat (141) away from the gas spring rod (142).

6. A supercritical fluid extraction device for sitagliptin phosphate intermediate according to claim 3, characterized in that: The feeding assembly (21) comprises a feeding pump (211), a guide rotating plate (212) and a material receiving pipe (213); the feeding pump (211) is connected to the bottom of the positioning cover (123); the guide rotating plate (212) is rotatably connected to the bottom of the feeding pump (211); the material receiving pipe (213) is connected to the top of the feeding pump (211); and the top of the material receiving pipe (213) passes through the top of the positioning cover (123) and is connected to the positioning cover (123).

7. A supercritical fluid extraction device for sitagliptin phosphate intermediate according to claim 6, characterized in that: The guide assembly (22) comprises a drainage cone barrel (221), a transmission ring (222) and a traction sleeve (223); the drainage cone barrel (221) is fixedly connected to the surface of the guide rotating plate (212); the transmission ring (222) is fixedly connected to the bottom of the drainage cone barrel (221); and the traction sleeve (223) is welded to the inner side of the transmission ring (222).

8. The supercritical fluid extraction device for sitagliptin phosphate intermediate according to claim 6, characterized in that: The tracing back assembly (23) comprises a tracing back drainage pipe (231), a tracing back drainage pipe (232) and a tracing back flow guide port (233); the tracing back drainage pipe (231) is fixedly connected to the bottom of the guide rotating plate (212); the tracing back drainage pipe (232) is connected to the bottom of the tracing back drainage pipe (231); and the tracing back flow guide port (233) is respectively provided on the surface of the tracing back drainage pipe (231) and the bottom of the surface of the tracing back drainage pipe (232).

9. A supercritical fluid extraction device for sitagliptin phosphate intermediate according to claim 7, characterized in that: The reflux assembly (24) comprises a reflux drainage pipe (241), a reflux drainage pipe (242) and a reflux guide port (243); the reflux drainage pipe (241) is clamped on the inner side of the traction sleeve (223); the reflux drainage pipe (242) is connected to the bottom of the reflux drainage pipe (241); and the reflux guide port (243) is respectively provided on the surface of the reflux drainage pipe (241) and the bottom of the surface of the reflux drainage pipe (242).

10. A supercritical fluid extraction device for sitagliptin phosphate intermediate according to claim 6, characterized in that: The supply assembly (25) includes a supply pipe (251), a positioning rod (252) and a spiral conveying plate (253); the supply pipe (251) is connected to the bottom of the feed pump (211); the bottom of the supply pipe (251) is fixedly connected to the top of the conductive rotating rod (134); the positioning rod (252) is fixedly connected to the inner side of the supply pipe (251); and the spiral conveying plate (253) is fixedly connected to the surface of the positioning rod (252).

Citation Information

Patent Citations

  • Double-bottle tilting supercritical fluid extraction unit

    CN106833883B