Preparation process, equipment and method of alogliptin
The novel preparation device and process for alogliptin addresses the complexities of traditional methods by integrating a reactor, distillation tower, condenser, and collector with mixing and centrifugal screening structures, enhancing efficiency and product quality while facilitating easy maintenance.
Patent Information
- Application Number
- CN202411094080.1
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-08-09
- Publication Date
- 2024-12-17
- Estimated Expiration
- Not applicable · inactive patent
AI Technical Summary
The traditional preparation method of alogliptin faces issues of complex equipment, cumbersome operation, high energy consumption, and unstable product quality.
A novel preparation device and process involving a reactor, distillation tower, condenser, and collector, equipped with a mixing structure, centrifugal screening structure, and limiting structure, which ensures efficient mixing, centrifugal screening, and stable operation, while allowing for easy disassembly and cleaning.
The process achieves efficient, economical, and environmentally friendly preparation of alogliptin with improved product quality and production efficiency through automation and continuity, ensuring uniform mixing and high purity of the product.
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Figure CN119140037A_ABST
Abstract
Description
Technical Field
[0001] The present invention relates to the technical field of chemical synthesis, and more specifically, to a preparation process of alogliptin and a device and method thereof. Background Art
[0002] As the number of diabetic patients continues to increase, the demand for drugs to treat diabetes is also growing. As an effective drug for the treatment of type II diabetes, alogliptin has an increasingly strong market demand.
[0003] According to patent document CN105777709A, the present invention discloses a preparation process of alogliptin. The process comprises the following steps: 1) 2-(6-chloro-3-methyl-2,4-dioxo-3,4-dihydro-2H-pyrimidin-1-ylmethyl)-benzonitrile (IV) and (R)-3-Boc-aminopiperidine undergo substitution reaction in the presence of a base and in an alcohol solvent to obtain compound IX, 2) removing the protecting group of the tert-butyloxycarbonyl group of the compound IX with an acid to obtain alogliptin (V), and the synthesis route thereof is as follows: characterized in that the base used in step 1) is selected from an inorganic base, the alcohol solvent used is selected from a hindered alcohol; and the acid used in step 2) is selected from a carboxylic acid. The advantages of the present invention are that, in the process of converting compound (IV) to compound (V), a hindered alcohol is selected as the solvent, which can effectively avoid the reaction of the α-Cl position of the allylic position with the solvent to generate impurities; an organic carboxylic acid with a weaker acidity is selected to remove the Boc protecting group, which does not damage the structure of the compound and avoids the use of p-toluenesulfonic acid, which may introduce genotoxic impurities when a lower alcohol is used as a solvent.
[0004] The traditional method for preparing alogliptin has problems such as complex equipment, cumbersome operation, high energy consumption and unstable product quality. Therefore, it is of great significance to develop an efficient, economical and environmentally friendly alogliptin preparation process and equipment.
[0005] The present invention aims at solving the above problems and provides a novel alogliptin preparation process and equipment and method thereof. By optimizing reaction conditions and improving equipment structure, efficient, economical and environmentally friendly preparation of alogliptin is achieved, and product quality and production efficiency are improved. Summary of the invention
[0006] In order to overcome the above-mentioned defects of the prior art, the present invention provides a preparation device and process of alogliptin. The technical problem to be solved by the present invention is that the traditional preparation method of alogliptin has the problems of complex equipment, cumbersome operation, high energy consumption and unstable product quality. Therefore, it is of great significance to develop an efficient, economical and environmentally friendly preparation process and equipment of alogliptin.
[0007] To achieve the above-mentioned purpose, the present invention provides the following technical scheme: comprising a reactor, wherein the outer wall of the reactor is fixedly connected with a connecting pipe 1, the other end of the connecting pipe 1 is fixedly connected with a distillation tower, the outer wall of the distillation tower is fixedly connected with a connecting pipe 2, the other end of the connecting pipe 2 is fixedly connected with a condenser, the outer wall of the condenser is fixedly connected with a connecting pipe 3, the other end of the connecting pipe 3 is fixedly connected with a collector, the end of the connecting pipe 3 away from the condenser penetrates into the interior of the collector, the interior of the reactor is provided with a mixing structure, the interior of the collector is provided with a limiting structure, the interior of the limiting structure is movably connected with a screening tank, the bottom of the screening tank is fixedly connected with a centrifugal screening structure, the top of the reactor is fixedly connected with a feed inlet, the upper part of the outer wall of the condenser is fixedly connected with a cold water inlet, the bottom of the collector is fixedly connected with a discharge port, the front side of the collector is fixedly connected with a control panel, and the lower part of the outer wall of the reactor is fixedly connected with a heating mechanism;
[0008] The mixing structure includes a stepper motor 1, the bottom of which is fixedly connected to a support platform, the bottom of which is fixedly connected to the top of the reactor, the output end of the stepper motor 1 is fixedly connected to a gear 1, the outer wall of the gear 1 is meshingly connected to a toothed disc 1, and the bottom of the toothed disc 1 is fixedly connected to a stirring assembly.
[0009] As a further solution of the present invention: the top of the toothed disc 1 is meshingly connected with a gear 2, the right end of the gear 2 is fixedly connected with a rotating rod 1, the outer wall of the rotating rod 1 is movably connected with a supporting sleeve 1, and the bottom of the supporting sleeve 1 is fixedly connected to the top of the reactor.
[0010] As a further scheme of the present invention: the other end of the rotating rod one is fixedly connected to a cross universal joint one, and the other end of the cross universal joint one is fixedly connected to a rotating rod two, and the rotating rod two is movably connected to a support sleeve two near the outer wall of the cross universal joint one, and the bottom of the support sleeve two is fixedly connected to the top of the reactor, and the rotating rod two is movably connected to a support sleeve three away from the outer wall of the cross universal joint one, and the bottom of the support sleeve three is fixedly connected to the outer wall of the reactor. The other end of the rotating rod two is fixedly connected to the cross universal joint two, and the other end of the cross universal joint two is fixedly connected to the rotating rod three, and the rotating rod three is movably connected to a support sleeve four near the outer wall of the cross universal joint two, one side of the support sleeve four is fixedly connected to the outer wall of the reactor, and the bottom of the outer wall of the rotating rod three is movably connected to a support sleeve five, and one side of the support sleeve five is fixedly connected to a fixing sleeve, and the inner wall of the fixing sleeve is fixedly connected to the support column at the bottom of the reactor.
[0011] As a further solution of the present invention: a limiting ring is arranged below the toothed disc, a gear sleeve is fixedly connected to the bottom of the limiting ring, a circular movable hole is opened on the top of the reactor and penetrates into the interior, and the outer wall of the limiting ring is fixedly connected to the inner wall of the circular movable hole.
[0012] As a further solution of the present invention: the stirring assembly includes a fixed rod 1, the top of the fixed rod 1 is fixedly connected to the bottom of the toothed disc 1, the upper part of the outer wall of the fixed rod 1 is fixedly connected to the inner wall of the limiting ring 1, the lower part of the outer wall of the fixed rod 1 is fixedly connected to the inner wall of the gear sleeve 1, the bottom of the fixed rod 1 is fixedly connected with a three-pronged plate, the tops of the three forked plates of the three-pronged plate are each provided with a circular movable hole 2 that penetrates to the bottom, the inner wall of the circular movable hole 2 is movably connected to a limiting rod 1, the upper and lower ends of the limiting rod 1 are fixedly connected with gears 3, and the outer walls of the three upper gears 3 are meshed with the outer wall of the gear sleeve 1.
[0013] As a further scheme of the present invention: the three forked plates of the three-pronged plate are provided with a circular movable hole three extending to the bottom away from the top of the fixed rod one, the inner wall of the circular movable hole three is movably connected to the limiting rod two, a gear sleeve two is fixedly connected below the outer wall of the limiting rod two, the outer wall of the gear sleeve two is meshed and connected with the outer wall of the gear three below, the bottom of the limiting rod two is fixedly connected with a connecting plate, the connecting plate is provided with a circular movable hole four extending to the bottom away from the top of the limiting rod two, the inner wall of the circular movable hole four is fixedly connected to the fixing rod two, the bottom of the fixing rod two is fixedly connected with a stirring blade, the three forked plates of the three-pronged plate are fixedly connected with an arc plate on one side away from the fixing rod one, the bottom of the arc plate is fixedly connected with a scraper, and the outer wall of the scraper is movably connected to the inner wall of the reactor.
[0014] As a further solution of the present invention: the centrifugal screening structure includes a conical tooth 1, the top of the conical tooth 1 is fixedly connected to the bottom of the rotating rod 3, the outer wall of the conical tooth 1 is meshedly connected with the conical tooth 2, the right end of the conical tooth 2 is fixedly connected with the rotating rod 4, the outer wall of the rotating rod 4 close to the conical tooth 2 is movably connected with a support sleeve 6, one side of the support sleeve 6 is fixedly connected to the left side of the collector, the outer wall of the rotating rod 4 is movably connected with a support sleeve 7, one side of the support sleeve 7 is fixedly connected to the bottom of the collector, and the other end of the rotating rod 4 is fixedly connected There is a conical tooth three, the outer wall of which is meshed with a conical tooth four, the rear end of which is fixedly connected to a rotating rod five, the outer wall of which is movably connected to a supporting sleeve eight, one side of which is fixedly connected to the bottom of the collector, the rear end of the rotating rod five is fixedly connected to a gear four, the outer wall of which is meshed with a toothed disc two, the top of which is fixedly connected to a connecting shaft, the bottom of the collector is provided with a circular movable hole five which passes through the interior, and the upper part of the outer wall of the connecting shaft is movably connected to the inner wall of the circular movable hole five.
[0015] As a further solution of the present invention: the screening tank includes a tank body, the bottom of the tank body is fixedly connected to the top of the connecting shaft, a limiting ring 2 is fixedly connected to the middle position of the outer wall of the tank body, a plurality of circular movable holes 6 penetrating to the interior are opened on the upper and lower sides of the outer wall of the tank body, a filter is fixedly connected to the inner wall of the circular movable hole 6, a circular through hole penetrating to the interior is opened on the top of the tank body, and the inner wall of the circular through hole is movably connected to the outer wall of the connecting pipe 3.
[0016] As a further solution of the present invention: the limiting structure includes an installation groove 1, the inner wall of the installation groove 1 is fixedly connected with a separation sleeve, the inner wall of the separation sleeve is movably connected with a rotating shaft, the left end of the rotating shaft is fixedly connected with a stepping motor 2, the top of the separation sleeve is fixedly connected with a protective cover, the right end of the rotating shaft is fixedly connected with a bidirectional threaded rod, the middle position of the outer wall of the bidirectional threaded rod is movably connected with a support sleeve 9, the outer wall of the support sleeve 9 is fixedly connected to the inner wall of the installation groove 1, the right end of the bidirectional threaded rod is rotatably connected to the inner wall of the installation groove 1, the outer wall of the bidirectional threaded rod is threadedly connected with two symmetrical sliders, the tops of the two sliders are fixedly connected with two symmetrical L-shaped blocks, and the front sides of the L-shaped blocks in the vertical direction are fixedly connected A telescopic block is fixedly connected, and two symmetrical arc-edge trapezoidal blocks are fixedly connected on the front and rear sides of one side where the two telescopic blocks are close to each other, and the inclined surface of the arc-edge trapezoidal block is provided with two rectangular grooves, and the upper and lower sides of the inner wall of the rectangular groove are rotatably connected with rollers, and the tops of the two L-shaped blocks are fixedly connected to the sides where they are close to each other, and the inner walls of the two sliding sleeves are movably connected with sliding rods, and the left and right ends of the sliding rods are fixedly connected with mounting groove 2, and the front sides of mounting groove 2 and mounting groove 1 are fixedly connected to the rear side of the collector, and rectangular movable holes that penetrate into the interior are provided on the left and right sides of the inner wall of the collector, and the outer wall of the telescopic block is movably connected to the inner wall of the rectangular movable hole, and the outer wall of the roller is movably connected to the outer wall of limit ring 2.
[0017] In addition, the present invention also relates to a preparation process of alogliptin and equipment thereof, comprising the following steps:
[0018] Step 1: Add the required raw materials into the reactor through the feed port, and close the feed port to ensure the airtightness of the reactor. At the same time, start the heating mechanism to provide the required reaction temperature for the raw materials in the reactor.
[0019] Step 2:
[0020] When the temperature in the reactor reaches the preset value, the stepper motor 1 is started, and the stepper motor 1 drives the gear 1 to rotate, and then the gear 1 is meshed with the gear disc 1 to drive the gear disc 1 and the stirring assembly at the bottom to rotate. During the rotation process, the three-pronged plate and the stirring blades in the stirring assembly effectively mix and stir the raw materials in the reactor to ensure the uniformity and efficiency of the reaction.
[0021] Step 3:
[0022] As the reaction proceeds, gas is generated in the reactor. The gas enters the distillation tower through connecting pipe one for distillation separation. The distilled gas enters the condenser through connecting pipe two. In the condenser, the cold water introduced through the cold water inlet cools the gas to condense it into liquid. The condensed liquid enters the collector through connecting pipe three.
[0023] Step 4:
[0024] In the collector, the liquid enters the screening tank, which is connected to the centrifugal screening structure through a connecting shaft. The centrifugal screening structure is meshed and connected through rotating rod three and gear four. When the stirring assembly rotates, the centrifugal screening structure also rotates, driving the screening tank for centrifugal screening. The screened liquid enters the bottom of the collector through the filter screen, while the solid impurities are intercepted by the filter screen in the screening tank.
[0025] Step 5:
[0026] During the centrifugal screening process, the limiting structure plays the role of fixing the screening tank. The stepper motor 2 drives the rotating shaft to rotate, which in turn drives the bidirectional threaded rod to rotate. The two sliders on the bidirectional threaded rod move toward or away from each other under the drive of the thread, thereby driving the telescopic block and the arc-edge trapezoidal block to fix or loosen the screening tank. The roller rolls on the outer wall of the limiting ring 2 to ensure the stability of the screening tank during rotation and facilitate disassembly and cleaning.
[0027] Step 6:
[0028] The liquid after centrifugal screening is discharged through the discharge port at the bottom of the collector, collected and stored. At the same time, the equipment is monitored and adjusted through the control panel to ensure the smooth progress of the entire preparation process.
[0029] The beneficial effects of the present invention are:
[0030] 1. The present invention realizes automation and continuity in the preparation process of alogliptin by providing a preparation equipment consisting of a reaction kettle, a distillation tower, a condenser and a collector, thereby greatly improving the preparation efficiency. At the same time, through the coordination of a stirring component and a centrifugal screening structure, sufficient mixing of raw materials and purity of the product are ensured, effectively solving the problems of complex equipment, cumbersome operation, high energy consumption and unstable product quality in the traditional preparation method.
[0031] 2. The present invention realizes stable fixation of the screening tank during operation through the design of the limiting structure, and at the same time has the effect of convenient disassembly, which is convenient for cleaning and maintenance of the equipment, and further improves the practicability and service life of the equipment. BRIEF DESCRIPTION OF THE DRAWINGS
[0032] Figure 1 It is a structural schematic diagram of the present invention;
[0033] Figure 2 It is a schematic diagram of the structural cross section of the present invention;
[0034] Figure 3 It is a schematic diagram of the structural cross section of the present invention;
[0035] Figure 4 It is a schematic diagram of the structural cross section of the hybrid structure of the present invention;
[0036] Figure 5 It is a schematic diagram of the structural cross section of the stirring assembly of the present invention;
[0037] Figure 6 It is a structural schematic diagram of the centrifugal screening structure of the present invention;
[0038] Figure 7 It is a structural schematic diagram of the screening tank of the present invention;
[0039] Figure 8 It is a schematic diagram of the structural cross-section of the limiting structure of the present invention.
[0040] In the figure: 1, reactor; 2, distillation tower; 3, condenser; 4, collector; 5, mixing structure; 6, centrifugal screening structure; 7, limit structure; 8, screening tank; 9, feed port; 10, connecting pipe 1; 11, connecting pipe 2; 12, cold water inlet; 13, connecting pipe 3; 14, discharge port; 15, control panel; 16, heating mechanism; 51, stepping motor 1; 52, support platform; 53, gear 1; 54, gear disc 1; 55 , stirring assembly; 56, gear two; 57, rotating rod one; 58, support sleeve one; 59, cross universal joint one; 50, rotating rod two; 501, support sleeve two; 502, support sleeve three; 503, cross universal joint two; 504, rotating rod three; 505, support sleeve four; 506, support sleeve five; 507, fixed sleeve; 508, limit ring one; 509, gear sleeve one; 551, fixed rod one; 552, three-prong plate; 553, limit rod one; 554, gear three; 555, limit rod two; 556, gear sleeve two; 557, connecting plate; 558, fixed rod two; 559, stirring blade; 550, arc plate; 5501, scraper; 61, cone tooth one; 62, cone tooth two; 63, rotating rod four; 64, support sleeve six; 65, support sleeve seven; 66, cone tooth three; 67, cone tooth four; 68, rotating rod five; 69, support sleeve eight; 60, gear four; 601, toothed disc two ; 602, connecting shaft; 81, tank body; 82, limit ring 2; 83, filter; 84, circular through hole; 71, mounting slot 1; 72, separation sleeve; 73, rotating shaft; 74, stepping motor 2; 75, protective cover; 76, bidirectional threaded rod; 77, support sleeve 9; 78, slider; 79, L-shaped block; 70, telescopic block; 701, arc-edged trapezoidal block; 702, roller; 703, sliding sleeve; 704, sliding rod; 705, mounting slot 2. DETAILED DESCRIPTION
[0041] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.
[0042] like Figure 1-3 As shown, the present invention provides a preparation device for alogliptin, comprising a reactor 1, an outer wall of the reactor 1 is fixedly connected with a connecting pipe 10, the other end of the connecting pipe 10 is fixedly connected with a distillation tower 2, an outer wall of the distillation tower 2 is fixedly connected with a connecting pipe 2 11, the other end of the connecting pipe 2 11 is fixedly connected with a condenser 3, an outer wall of the condenser 3 is fixedly connected with a connecting pipe 3 13, the other end of the connecting pipe 3 13 is fixedly connected with a collector 4, one end of the connecting pipe 3 13 away from the condenser 3 penetrates into the collector 4, a mixing structure 5 is arranged inside the reactor 1, a limiting structure 7 is arranged inside the collector 4, a screening tank 8 is movably connected inside the limiting structure 7, a centrifugal screening structure 6 is fixedly connected to the bottom of the screening tank 8, a feed inlet 9 is fixedly connected to the top of the reactor 1, a cold water inlet 12 is fixedly connected to the top of the outer wall of the condenser 3, a discharge port 14 is fixedly connected to the bottom of the collector 4, a control panel 15 is fixedly connected to the front side of the collector 4, and a heating mechanism 16 is fixedly connected to the bottom of the outer wall of the reactor 1;
[0043] like Figure 4-7As shown, the mixing structure 5 includes a stepper motor 51, the bottom of the stepper motor 51 is fixedly connected to a support platform 52, the bottom of the support platform 52 is fixedly connected to the top of the reactor 1, the output end of the stepper motor 51 is fixedly connected to a gear 53, the outer wall of the gear 53 is meshingly connected to a toothed disc 54, the bottom of the toothed disc 54 is fixedly connected to a stirring assembly 55, the top of the toothed disc 54 is meshingly connected to a gear 2 56, the right end of the gear 2 56 is fixedly connected to a rotating rod 1 57, the outer wall of the rotating rod 57 is movably connected to a supporting sleeve 1 58, the bottom of the supporting sleeve 58 is fixedly connected to the top of the reactor 1, the other end of the rotating rod 57 is fixedly connected to a cross universal joint 1 59, and the other end of the cross universal joint 1 59 is fixedly connected to the rotating rod 2 50, the outer wall of the rotating rod 2 50 near the cross universal joint 1 59 is movably connected with the supporting sleeve 2 501, the bottom of the supporting sleeve 2 501 is fixedly connected to the top of the reactor 1, the outer wall of the rotating rod 2 50 away from the cross universal joint 1 59 is movably connected with the supporting sleeve 3 502, the bottom of the supporting sleeve 3 502 is fixedly connected to the outer wall of the reactor 1, the other end of the rotating rod 2 50 is fixedly connected with the cross universal joint 2 503, the other end of the cross universal joint 2 503 is fixedly connected with the rotating rod 3 504, the outer wall of the rotating rod 3 504 near the cross universal joint 2 503 is movably connected with the supporting sleeve 4 505, one side of the supporting sleeve 4 505 is fixedly connected to the outer wall of the reactor 1, the outer wall bottom of the rotating rod 3 504 is movably connected with the supporting sleeve 5 506, the supporting sleeve 5 A fixing sleeve 507 is fixedly connected to one side of 506, and the inner wall of the fixing sleeve 507 is fixedly connected to the support column at the bottom of the reactor 1. A limiting ring 508 is arranged below the toothed disc 54, and a toothed sleeve 509 is fixedly connected to the bottom of the limiting ring 508. A circular movable hole 1 penetrating to the inside is provided on the top of the reactor 1, and the outer wall of the limiting ring 508 is fixedly connected to the inner wall of the circular movable hole 1. The stirring assembly 55 includes a fixing rod 551, and the top of the fixing rod 551 is fixedly connected to the bottom of the toothed disc 54, the upper part of the outer wall of the fixing rod 551 is fixedly connected to the inner wall of the limiting ring 508, the lower part of the outer wall of the fixing rod 551 is fixedly connected to the inner wall of the toothed sleeve 509, and the bottom of the fixing rod 551 is fixedly connected to a three-pronged Plate 552, the tops of the three forked plates of the three-pronged plate 552 are all provided with circular movable holes 2 that penetrate to the bottom, the inner wall of the circular movable hole 2 is movably connected to the limiting rod 1 553, the upper and lower ends of the limiting rod 1 553 are fixedly connected with gear 3 554, the outer walls of the three upper gears 3 554 are meshed and connected with the outer wall of the gear sleeve 1 509, the tops of the three forked plates of the three-pronged plate 552 away from the fixed rod 1 551 are provided with circular movable holes 3 that penetrate to the bottom, the inner wall of the circular movable hole 3 is movably connected to the limiting rod 2 555, the lower part of the outer wall of the limiting rod 2 555 is fixedly connected with the gear sleeve 2 556, the outer wall of the gear sleeve 2 556 is meshed and connected with the outer wall of the lower gear 3 554, the lower part of the limiting rod 2 555 is fixedly connected with the connecting plate 557,A circular movable hole 4 is provided at the top of the connecting plate 557 away from the limiting rod 2 555 and extends to the bottom. The inner wall of the circular movable hole 4 is fixedly connected to the fixing rod 2 558. The bottom of the fixing rod 2 558 is fixedly connected to the stirring blade 559. The three forked plates of the three-fork plate 552 are fixedly connected to the arc plate 550 on one side away from the fixing rod 1 551. The bottom of the arc plate 550 is fixedly connected to the scraper 5501. The outer wall of the scraper 5501 is movably connected to the inner wall of the reactor 1. The centrifugal screening structure 6 includes a conical tooth 1 61. The top of the conical tooth 1 61 is fixedly connected to the bottom of the rotating rod 3 504, the outer wall of the conical tooth 1 61 is meshedly connected with the conical tooth 2 62, the right end of the conical tooth 2 62 is fixedly connected with the rotating rod 4 63, the outer wall of the rotating rod 4 63 close to the conical tooth 2 62 is movably connected with the support sleeve 6 64, one side of the support sleeve 64 is fixedly connected to the left side of the collector 4, the outer wall of the rotating rod 4 63 is movably connected with the support sleeve 7 65, one side of the support sleeve 7 65 is fixedly connected to the bottom of the collector 4, and the other end of the rotating rod 4 63 is fixedly connected with the conical tooth The outer wall of the conical tooth three 66 is meshedly connected with the conical tooth four 67, the rear end of the conical tooth four 67 is fixedly connected with the rotating rod five 68, the outer wall of the rotating rod five 68 is movably connected with the supporting sleeve eight 69, one side of the supporting sleeve eight 69 is fixedly connected to the bottom of the collector 4, the rear end of the rotating rod five 68 is fixedly connected with the gear four 60, the outer wall of the gear four 60 is meshedly connected with the toothed disc two 601, the top of the toothed disc two 601 is fixedly connected with the connecting shaft 602, the bottom of the collector 4 is provided with a circular movable hole five that penetrates to the inside, and the connecting shaft 602 is fixedly connected to the outer wall of the conical tooth three 66. The top of the outer wall of the tank body 81 is movably connected to the inner wall of the circular movable hole 5, the screening tank 8 includes a tank body 81, the bottom of the tank body 81 is fixedly connected to the top of the connecting shaft 602, the middle position of the outer wall of the tank body 81 is fixedly connected to the limiting ring 2 82, the upper and lower sides of the outer wall of the tank body 81 are provided with a plurality of circular movable holes 6 penetrating to the inside, the inner wall of the circular movable hole 6 is fixedly connected with a filter screen 83, the top of the tank body 81 is provided with a circular through hole 84 penetrating to the inside, the inner wall of the circular through hole 84 is movably connected to the outer wall of the connecting pipe 3 13;
[0044] The required raw materials are added into the reactor 1 through the feed port 9, and the feed port 9 is closed. Then, the heating mechanism 16 is started through the control panel 15 to start heating the reactor 1. As the temperature gradually rises, the raw materials in the reactor 1 begin to undergo a chemical reaction. At the same time, the stepper motor 1 51 starts to work, driving the gear 1 53 to rotate. The gear 1 53 drives the toothed disc 1 54 to rotate through meshing transmission, thereby starting the stirring assembly 55. The tripod plate 552 is driven by the toothed disc 1 54 to rotate around the fixed rod 1 551. At the same time, due to the meshing relationship between the gear 3 554 thereon and the gear sleeve 1 509 and the gear sleeve 2 556, the stirring assembly 55 starts to work. The limiting rod 1 553 and the limiting rod 2 555 also generate corresponding movements, driving the stirring blade 559 to perform complex stirring actions to ensure that the raw materials in the reactor 1 can be fully mixed and the reaction is more uniform. As the reaction proceeds, the generated gas enters the distillation tower 2 through the connecting pipe 10. In the distillation tower 2, the gas is separated by distillation to obtain the desired product gas. These product gases then enter the condenser 3 through the connecting pipe 2 11. In the condenser 3, cold water enters through the cold water inlet 12 to perform heat exchange with the product gas, so that the product gas is condensed into liquid. The condensed liquid enters the collector 4 through the connecting pipe 3 13. In the collector 4, The operation of stepper motor 1 51 starts the centrifugal screening structure 6. The rotation of toothed disc 1 54 drives gear 2 56 to rotate the rotating rod 1 57, and then the rotating rod 2 50 is rotated under the action of cross universal joint 1 59, and the rotating rod 3 504 is rotated under the action of cross universal joint 2 503, so that the conical gear 1 61 is rotated, driving the conical gear 2 62, the rotating rod 4 63 and other components to rotate in sequence. The meshing relationship between gear 4 60 on the rotating rod 5 68 and toothed disc 2 601 makes the connecting shaft 602 drive the screening tank 8 to rotate. During the rotation of the screening tank 8, the liquid inside it passes through the filter screen 8 under the action of centrifugal force. 3 is screened to separate the desired pure product. After screening, the pure product accumulates at the bottom of the inner wall of the collector 4. When the product accumulates to a certain extent, the control panel 15 can be operated to stop the rotation of the screening tank 8, and the product is discharged from the collector 4 through the discharge port 14. During the whole preparation process, the temperature, pressure and other parameters of the reactor 1 can be monitored in real time through the control panel 15, and the heating power of the heating mechanism 16 can be adjusted as needed to ensure the smooth progress of the reaction. At the same time, the control panel 15 can also control the rotation speed of the stepping motor 51, thereby adjusting the stirring speed of the stirring component 55 to meet the needs of different raw materials and reaction conditions.
[0045] like Figure 8As shown, the limiting structure 7 includes a mounting groove 1 71, a separation sleeve 72 is fixedly connected to the inner wall of the mounting groove 1 71, a rotating shaft 73 is movably connected to the inner wall of the separation sleeve 72, a stepping motor 2 74 is fixedly connected to the left end of the rotating shaft 73, a protective cover 75 is fixedly connected to the top of the separation sleeve 72, a bidirectional threaded rod 76 is fixedly connected to the right end of the rotating shaft 73, a support sleeve 9 77 is movably connected to the middle position of the outer wall of the bidirectional threaded rod 76, the outer wall of the support sleeve 9 77 is fixedly connected to the inner wall of the mounting groove 1 71, the right end of the bidirectional threaded rod 76 is rotatably connected to the inner wall of the mounting groove 1 71, the outer wall of the bidirectional threaded rod 76 is threadedly connected to two symmetrical sliders 78, the tops of the two sliders 78 are fixedly connected to two symmetrical L-shaped blocks 79, and the front side of the L-shaped block 79 in the vertical direction is fixedly connected to a telescopic Block 70, two symmetrical arc-edge trapezoidal blocks 701 are fixedly connected to the front and rear sides of the side where the two telescopic blocks 70 are close to each other, and the inclined surface of the arc-edge trapezoidal block 701 is provided with two rectangular grooves, and the upper and lower sides of the inner wall of the rectangular groove are rotatably connected with rollers 702, and the tops of the two L-shaped blocks 79 are fixedly connected to the side where the two L-shaped blocks 79 are close to each other, and the inner walls of the two sliding sleeves 703 are movably connected with sliding rods 704, and the left and right ends of the sliding rods 704 are fixedly connected with mounting groove 2 705, and the front sides of mounting groove 2 705 and mounting groove 1 71 are fixedly connected to the rear side of the collector 4, and the left and right sides of the inner wall of the collector 4 are provided with rectangular movable holes that penetrate to the inside, the outer wall of the telescopic block 70 is movably connected to the inner wall of the rectangular movable hole, and the outer wall of the roller 702 is movably connected to the outer wall of the limiting ring 2 82;
[0046] When it is necessary to limit or release the limit of the screening tank 8, the control panel 15 can be used to control the start or stop of the stepper motor 2 74. The start of the stepper motor 2 74 will drive the rotation of the shaft 73, thereby causing the bidirectional threaded rod 76 to start rotating. Due to the threaded connection between the bidirectional threaded rod 76 and the two sliders 78, the two sliders 78 move relative to or away from each other along the outer wall of the bidirectional threaded rod 76 under the rotation of the bidirectional threaded rod 76. This movement will drive the two L-shaped blocks 79 to move accordingly, thereby changing the distance between the two telescopic blocks 70. As the telescopic block 70 moves, the inclined surface of the arc-edge trapezoidal block 701 moves away from the outer wall of the limiting ring 2 82, and the tank body 81 is released from the limit. The roller 702 rolls on the outer wall of the limiting ring 2 82, making the tank body 81 more stable during operation. The telescopic block 70 is moved in the rectangular movable hole The movement enables the telescopic block 70 to move smoothly along the inner wall of the rectangular movable hole. At the same time, the movable connection of the sliding sleeve 703 on the sliding rod 704 ensures the stability of the telescopic block 70 during the movement. When the two telescopic blocks 70 are close to each other, they will clamp the limiting ring 2 82 of the screening tank 8, thereby limiting the screening tank 8 to prevent it from shaking or shifting during the centrifugal screening process. When it is necessary to release the limitation of the screening tank 8, it is only necessary to control the stepper motor 2 74 to rotate in the opposite direction to make the two telescopic blocks 70 move away from each other, and the screening tank 8 can be easily taken out from the limiting structure. This not only ensures the stability of the screening tank 8 during the centrifugal screening process, but also improves the automation degree and operation convenience of the entire preparation process. At the same time, combined with the real-time monitoring and adjustment functions of the control panel 15, the entire preparation process is more accurate, efficient and safe.
[0047] In addition, the present invention also relates to a preparation process of alogliptin and equipment thereof, comprising the following steps:
[0048] Step 1: Add the required raw materials into the reactor 1 through the feed port 9, and close the feed port 9 to ensure the airtightness of the reactor 1. At the same time, start the heating mechanism 16 to provide the required reaction temperature for the raw materials in the reactor 1.
[0049] Step 2:
[0050] When the temperature in the reactor 1 reaches a preset value, the stepper motor 51 is started, and the stepper motor 51 drives the gear 53 to rotate, and then the gear 53 is meshed with the toothed disc 54 to drive the toothed disc 54 and the stirring component 55 at the bottom thereof to rotate. During the rotation process, the tripod plate 552 and the stirring blade 559 in the stirring component 55 effectively mix and stir the raw materials in the reactor 1 to ensure the uniformity and efficiency of the reaction.
[0051] Step 3:
[0052] As the reaction proceeds, gas is generated in the reactor 1. The gas enters the distillation tower 2 through the connecting pipe 10 for distillation and separation. The distilled gas enters the condenser 3 through the connecting pipe 2 11. In the condenser 3, the cold water introduced through the cold water inlet 12 cools the gas to condense it into liquid. The condensed liquid enters the collector 4 through the connecting pipe 3 13.
[0053] Step 4:
[0054] In the collector 4, the liquid enters the screening tank 8, and the screening tank 8 is connected to the centrifugal screening structure 6 through the connecting shaft 602. The centrifugal screening structure 6 is meshed and connected through the rotating rod three 504 and the gear four 60. When the stirring assembly 55 rotates, the centrifugal screening structure 6 also rotates, driving the screening tank 8 to perform centrifugal screening. The screened liquid enters the bottom of the collector 4 through the filter screen 83, and the solid impurities are intercepted by the filter screen 83 in the screening tank 8.
[0055] Step 5:
[0056] During the centrifugal screening process, the limiting structure 7 plays the role of fixing the screening tank 8. The stepper motor 2 74 drives the rotating shaft 73 to rotate, thereby driving the bidirectional threaded rod 76 to rotate. The two sliders 78 on the bidirectional threaded rod 76 move toward or away from each other under the drive of the thread, thereby driving the telescopic block 70 and the arc-edge trapezoidal block 701 to fix or loosen the screening tank 8. The roller 702 rolls on the outer wall of the limiting ring 2 82 to ensure the stability of the screening tank 8 during rotation and facilitate disassembly and cleaning.
[0057] Step 6:
[0058] The liquid after centrifugal screening is discharged through the discharge port 14 at the bottom of the collector 4, collected and stored. At the same time, the equipment is monitored and adjusted through the control panel 15 to ensure the smooth progress of the entire preparation process.
[0059] The working principle of the present invention is as follows: the required raw materials are added into the reactor 1 through the feed port 9, and the feed port 9 is closed. Then, the heating mechanism 16 is started through the control panel 15 to start heating the reactor 1. As the temperature gradually rises, the raw materials in the reactor 1 begin to undergo a chemical reaction. At the same time, the stepping motor 1 51 starts to work, driving the gear 1 53 to rotate. The gear 1 53 drives the toothed disc 1 54 to rotate through meshing transmission, thereby starting the stirring assembly 55. The tripod plate 552 is driven by the toothed disc 1 54 to rotate around the fixed rod 1 551. At the same time, due to the meshing of the gear 3 554 thereon with the gear sleeve 1 509 and the gear sleeve 2 556, the stirring assembly 55 starts to work. The combination relationship makes the limit rod 1 553 and the limit rod 2 555 also produce corresponding movement, driving the stirring blade 559 to perform complex stirring actions, ensuring that the raw materials in the reactor 1 can be fully mixed and the reaction is more uniform. As the reaction proceeds, the generated gas enters the distillation tower 2 through the connecting pipe 10. In the distillation tower 2, the gas is distilled and separated to obtain the desired product gas. The product gas then enters the condenser 3 through the connecting pipe 2 11. In the condenser 3, cold water enters through the cold water inlet 12 to perform heat exchange with the product gas, so that the product gas is condensed into liquid. The condensed liquid enters the collector 4 through the connecting pipe 3 13. In the collector 4 In the embodiment, the centrifugal screening structure 6 starts to work by operating the stepper motor 1 51, the rotation of the toothed disc 1 54 drives the gear 2 56 to rotate the rotating rod 1 57, and then the rotating rod 2 50 is rotated under the action of the cross universal joint 1 59, and then the rotating rod 3 504 is rotated under the action of the cross universal joint 2 503, so that the conical gear 1 61 is rotated, driving the conical gear 2 62, the rotating rod 4 63 and other components to rotate in sequence, the meshing relationship between the gear 4 60 on the rotating rod 5 68 and the toothed disc 2 601 makes the connecting shaft 602 drive the screening tank 8 to rotate, and during the rotation of the screening tank 8, the liquid inside the screening tank is filtered by the centrifugal force. The net 83 is used for screening to separate the desired pure product. After screening, the pure product accumulates at the bottom of the inner wall of the collector 4. When the product accumulates to a certain extent, the control panel 15 can be operated to stop the rotation of the screening tank 8, and the product can be discharged from the collector 4 through the discharge port 14. During the entire preparation process, the temperature, pressure and other parameters of the reactor 1 can be monitored in real time through the control panel 15, and the heating power of the heating mechanism 16 can be adjusted as needed to ensure the smooth progress of the reaction. At the same time, the control panel 15 can also control the rotation speed of the stepper motor 51, thereby adjusting the stirring speed of the stirring component 55 to meet the needs of different raw materials and reaction conditions.
[0060] When it is necessary to limit or release the limit of the screening tank 8, the control panel 15 can be used to control the start or stop of the stepper motor 2 74. The start of the stepper motor 2 74 will drive the rotation of the shaft 73, thereby causing the bidirectional threaded rod 76 to start rotating. Due to the threaded connection between the bidirectional threaded rod 76 and the two sliders 78, the two sliders 78 move relative to or away from each other along the outer wall of the bidirectional threaded rod 76 under the rotation of the bidirectional threaded rod 76. This movement will drive the two L-shaped blocks 79 to move accordingly, thereby changing the distance between the two telescopic blocks 70. As the telescopic block 70 moves, the inclined surface of the arc-edge trapezoidal block 701 moves away from the outer wall of the limiting ring 2 82, and the tank body 81 is released from the limit. The roller 702 rolls on the outer wall of the limiting ring 2 82, making the tank body 81 more stable during operation. The telescopic block 70 is moved in the rectangular movable hole The movement enables the telescopic block 70 to move smoothly along the inner wall of the rectangular movable hole. At the same time, the movable connection of the sliding sleeve 703 on the sliding rod 704 ensures the stability of the telescopic block 70 during the movement. When the two telescopic blocks 70 are close to each other, they will clamp the limiting ring 2 82 of the screening tank 8, thereby limiting the screening tank 8 to prevent it from shaking or shifting during the centrifugal screening process. When it is necessary to release the limitation of the screening tank 8, it is only necessary to control the stepper motor 2 74 to rotate in the opposite direction to make the two telescopic blocks 70 move away from each other, and the screening tank 8 can be easily taken out from the limiting structure. This not only ensures the stability of the screening tank 8 during the centrifugal screening process, but also improves the automation degree and operation convenience of the entire preparation process. At the same time, combined with the real-time monitoring and adjustment functions of the control panel 15, the entire preparation process is more accurate, efficient and safe.
[0061] Finally, a few points should be explained: First, in the description of this application, it should be noted that, unless otherwise specified and limited, the terms "installed", "connected" and "connected" should be understood in a broad sense, which can be a mechanical connection or an electrical connection, or the internal communication of two components, or a direct connection. "upper", "lower", "left" and "right" are only used to indicate relative positional relationships. When the absolute position of the object being described changes, the relative positional relationship may change;
[0062] Secondly: In the drawings of the embodiments disclosed in the present invention, only the structures related to the embodiments disclosed in the present invention are involved, and other structures can refer to the general design. In the absence of conflict, the same embodiment and different embodiments of the present invention can be combined with each other;
[0063] The above description is only a preferred specific implementation manner of the present invention, but the protection scope of the present invention is not limited thereto. Any technician familiar with the technical field can make equivalent replacements or changes according to the technical scheme and inventive concept of the present invention within the technical scope disclosed by the present invention, which should be covered by the protection scope of the present invention.
Claims
1. A preparation device for alogliptin, comprising a reaction kettle (1), characterized in that: The outer wall of the reactor (1) is fixedly connected to a connecting pipe 1 (10), the other end of the connecting pipe 1 (10) is fixedly connected to a distillation tower (2), the outer wall of the distillation tower (2) is fixedly connected to a connecting pipe 2 (11), the other end of the connecting pipe 2 (11) is fixedly connected to a condenser (3), the outer wall of the condenser (3) is fixedly connected to a connecting pipe 3 (13), the other end of the connecting pipe 3 (13) is fixedly connected to a collector (4), the end of the connecting pipe 3 (13) away from the condenser (3) penetrates into the interior of the collector (4), and a mixing structure is arranged inside the reactor (1). The collector (4) is provided with a limiting structure (7) inside, the limiting structure (7) is movably connected to a screening tank (8) inside, the bottom of the screening tank (8) is fixedly connected to a centrifugal screening structure (6), the top of the reactor (1) is fixedly connected to a feed port (9), the upper part of the outer wall of the condenser (3) is fixedly connected to a cold water inlet (12), the bottom of the collector (4) is fixedly connected to a discharge port (14), the front side of the collector (4) is fixedly connected to a control panel (15), and the lower part of the outer wall of the reactor (1) is fixedly connected to a heating mechanism (16); The mixing structure (5) comprises a stepper motor (51), the bottom of the stepper motor (51) is fixedly connected to a support platform (52), the bottom of the support platform (52) is fixedly connected to the top of the reaction kettle (1), the output end of the stepper motor (51) is fixedly connected to a gear (53), the outer wall of the gear (53) is meshingly connected to a toothed disc (54), and the bottom of the toothed disc (54) is fixedly connected to a stirring assembly (55).
2. The preparation device of alogliptin according to claim 1, characterized in that: The top of the toothed disc 1 (54) is meshingly connected with a gear 2 (56), the right end of the gear 2 (56) is fixedly connected with a rotating rod 1 (57), the outer wall of the rotating rod 1 (57) is movably connected with a supporting sleeve 1 (58), and the bottom of the supporting sleeve 1 (58) is fixedly connected to the top of the reaction kettle (1).
3. The preparation device of alogliptin according to claim 2, characterized in that: The other end of the rotating rod 1 (57) is fixedly connected to a cross universal joint 1 (59), and the other end of the cross universal joint 1 (59) is fixedly connected to a rotating rod 2 (50). The rotating rod 2 (50) is movably connected to a support sleeve 2 (501) near the outer wall of the cross universal joint 1 (59), and the bottom of the support sleeve 2 (501) is fixedly connected to the top of the reaction kettle (1). The rotating rod 2 (50) is movably connected to a support sleeve 3 (502) away from the outer wall of the cross universal joint 1 (59), and the bottom of the support sleeve 3 (502) is fixedly connected to the outer wall of the reaction kettle (1). The other end of the rotating rod 2 (50) A cross universal joint 2 (503) is fixedly connected, and the other end of the cross universal joint 2 (503) is fixedly connected to a rotating rod 3 (504), and the rotating rod 3 (504) is movably connected to a supporting sleeve 4 (505) near the outer wall of the cross universal joint 2 (503), and one side of the supporting sleeve 4 (505) is fixedly connected to the outer wall of the reactor (1), and the bottom of the outer wall of the rotating rod 3 (504) is movably connected to a supporting sleeve 5 (506), and one side of the supporting sleeve 5 (506) is fixedly connected to a fixing sleeve (507), and the inner wall of the fixing sleeve (507) is fixedly connected to the supporting column at the bottom of the reactor (1).
4. The preparation device of alogliptin according to claim 1, characterized in that: A limiting ring (508) is provided below the toothed disc (54), and a gear sleeve (509) is fixedly connected to the bottom of the limiting ring (508). A circular movable hole (509) is provided on the top of the reactor (1) and penetrates into the interior, and the outer wall of the limiting ring (508) is fixedly connected to the inner wall of the circular movable hole (509).
5. The preparation device of alogliptin according to claim 1, characterized in that: The stirring assembly (55) comprises a fixing rod 1 (551), the top of which is fixedly connected to the bottom of a toothed disc 1 (54), the upper part of the outer wall of the fixing rod 1 (551) is fixedly connected to the inner wall of a limiting ring 1 (508), the lower part of the outer wall of the fixing rod 1 (551) is fixedly connected to the inner wall of a gear sleeve 1 (509), the bottom of the fixing rod 1 (551) is fixedly connected to a three-pronged plate (552), the tops of the three forked plates of the three-pronged plate (552) are each provided with a circular movable hole 2 extending through the bottom, the inner wall of the circular movable hole 2 is movably connected to a limiting rod 1 (553), the upper and lower ends of the limiting rod 1 (553) are fixedly connected to a gear 3 (554), and the outer walls of the three upper gears 3 (554) are meshedly connected to the outer wall of the gear sleeve 1 (509).
6. The preparation device of alogliptin according to claim 5, characterized in that: The three forked plates of the three-pronged plate (552) are provided with a circular movable hole three extending from the top to the bottom away from the fixed rod one (551); the inner wall of the circular movable hole three is movably connected to the limiting rod two (555); the lower part of the outer wall of the limiting rod two (555) is fixedly connected to the gear sleeve two (556); the outer wall of the gear sleeve two (556) is meshedly connected to the outer wall of the gear three (554) below; the lower part of the limiting rod two (555) is fixedly connected to the connecting plate (557); the connecting plate (557) is far away from the limiting rod two. A circular movable hole four is provided at the top of (555) and extends through the bottom. The inner wall of the circular movable hole four is fixedly connected to a fixed rod two (558). The bottom of the fixed rod two (558) is fixedly connected to a stirring blade (559). The three forked plates of the three-fork plate (552) are fixedly connected to an arc plate (550) on one side away from the fixed rod one (551). The bottom of the arc plate (550) is fixedly connected to a scraper (5501). The outer wall of the scraper (5501) is movably connected to the inner wall of the reaction kettle (1).
7. The preparation device of alogliptin according to claim 1, characterized in that: The centrifugal screening structure (6) comprises a conical tooth 1 (61), the top of the conical tooth 1 (61) is fixedly connected to the bottom of a rotating rod 3 (504), the outer wall of the conical tooth 1 (61) is meshingly connected with a conical tooth 2 (62), the right end of the conical tooth 2 (62) is fixedly connected with a rotating rod 4 (63), the rotating rod 4 (63) is movably connected with a support sleeve 6 (64) near the outer wall of the conical tooth 2 (62), one side of the support sleeve 6 (64) is fixedly connected to the left side of the collector (4), the outer wall of the rotating rod 4 (63) is movably connected with a support sleeve 7 (65), one side of the support sleeve 7 (65) is fixedly connected to the bottom of the collector (4), and the other end of the rotating rod 4 (63) is fixedly connected with the conical tooth 3 (64). 66), the outer wall of the conical tooth three (66) is meshedly connected with the conical tooth four (67), the rear end of the conical tooth four (67) is fixedly connected with the rotating rod five (68), the outer wall of the rotating rod five (68) is movably connected with the supporting sleeve eight (69), one side of the supporting sleeve eight (69) is fixedly connected to the bottom of the collector (4), the rear end of the rotating rod five (68) is fixedly connected with the gear four (60), the outer wall of the gear four (60) is meshedly connected with the toothed disc two (601), the top of the toothed disc two (601) is fixedly connected with the connecting shaft (602), the bottom of the collector (4) is provided with a circular movable hole five extending through the interior, and the upper part of the outer wall of the connecting shaft (602) is movably connected to the inner wall of the circular movable hole five.
8. The preparation device of alogliptin according to claim 1, characterized in that: The screening tank (8) comprises a tank body (81), the bottom of the tank body (81) is fixedly connected to the top of the connecting shaft (602), a limiting ring (82) is fixedly connected to the middle position of the outer wall of the tank body (81), a plurality of circular movable holes (6) penetrating to the interior are provided on the upper and lower sides of the outer wall of the tank body (81), a filter screen (83) is fixedly connected to the inner wall of the circular movable hole (6), a circular through hole (84) penetrating to the interior is provided on the top of the tank body (81), and the inner wall of the circular through hole (84) is movably connected to the outer wall of the connecting pipe (13).
9. The preparation device of alogliptin according to claim 1, characterized in that: The limiting structure (7) comprises a first installation groove (71), the inner wall of the first installation groove (71) is fixedly connected to a separation sleeve (72), the inner wall of the separation sleeve (72) is movably connected to a rotating shaft (73), the left end of the rotating shaft (73) is fixedly connected to a second stepping motor (74), the top of the separation sleeve (72) is fixedly connected to a protective cover (75), the right end of the rotating shaft (73) is fixedly connected to a bidirectional threaded rod (76), and the outer surface of the bidirectional threaded rod (76) is fixedly connected to the second stepping motor (74). A support sleeve 9 (77) is movably connected to the middle position of the wall, the outer wall of the support sleeve 9 (77) is fixedly connected to the inner wall of the installation groove 1 (71), the right end of the bidirectional threaded rod (76) is rotatably connected to the inner wall of the installation groove 1 (71), the outer wall of the bidirectional threaded rod (76) is threadedly connected to two symmetrical sliders (78), the tops of the two sliders (78) are fixedly connected to two symmetrical L-shaped blocks (79), the front sides of the L-shaped blocks (79) in the vertical direction are fixedly connected to a telescopic block (70), the front and rear sides of the two telescopic blocks (70) close to each other are fixedly connected to two symmetrical arc-edge trapezoidal blocks (701), the inclined surface of the arc-edge trapezoidal blocks (701) is provided with two rectangular grooves, the upper and lower sides of the inner wall of the rectangular groove are rotatably connected to rollers (702), the tops of the two L-shaped blocks (79) close to each other are fixedly connected to a sliding sleeve (703), the inner walls of the two sliding sleeves (703) are movably connected to Rod (704), the left and right ends of the sliding rod (704) are fixedly connected with mounting groove 2 (705), the front sides of mounting groove 2 (705) and mounting groove 1 (71) are fixedly connected with the rear side of the collector (4), the left and right sides of the inner wall of the collector (4) are both provided with rectangular movable holes penetrating into the interior, the outer wall of the telescopic block (70) is movably connected with the inner wall of the rectangular movable hole, and the outer wall of the roller (702) is movably connected with the outer wall of the second limiting ring (82).
10. A process for preparing alogliptin and an apparatus thereof according to any one of claims 1 to 9, comprising the following steps: Step 1: Add the required raw materials into the reactor (1) through the feed port (9), and close the feed port (9) to ensure the airtightness of the reactor (1). At the same time, start the heating mechanism (16) to provide the required reaction temperature for the raw materials in the reactor (1). Step 2: When the temperature in the reaction kettle (1) reaches a preset value, the stepper motor 1 (51) is started, and the stepper motor 1 (51) drives the gear 1 (53) to rotate, and then the gear 1 (53) is meshed with the gear disc 1 (54), driving the gear disc 1 (54) and the stirring component (55) at the bottom thereof to rotate. During the rotation process, the three-pronged plate (552) and the stirring blade (559) in the stirring component (55) effectively mix and stir the raw materials in the reaction kettle (1), thereby ensuring the uniformity and efficiency of the reaction. Step 3: As the reaction proceeds, gas is generated in the reactor (1). The gas enters the distillation tower (2) through the connecting pipe 1 (10) for distillation separation. The distilled gas enters the condenser (3) through the connecting pipe 2 (11). In the condenser (3), cold water introduced through the cold water inlet (12) cools the gas and condenses it into liquid. The condensed liquid enters the collector (4) through the connecting pipe 3 (13). Step 4: In the collector (4), liquid enters the screening tank (8), which is connected to the centrifugal screening structure (6) via a connecting shaft (602), and the centrifugal screening structure (6) is meshedly connected via a rotating rod three (504) and a gear four (60). When the stirring assembly (55) rotates, the centrifugal screening structure (6) also rotates, driving the screening tank (8) to perform centrifugal screening. The screened liquid passes through the filter screen (83) and enters the bottom of the collector (4), while solid impurities are intercepted by the filter screen (83) in the screening tank (8). Step 5: During the centrifugal screening process, the limiting structure (7) plays a role in fixing the screening tank (8). The second stepping motor (74) drives the rotating shaft (73) to rotate, thereby driving the bidirectional threaded rod (76) to rotate. The two sliders (78) on the bidirectional threaded rod (76) move towards or away from each other under the drive of the threads, thereby driving the telescopic block (70) and the arc-edge trapezoidal block (701) to fix or loosen the screening tank (8). The roller (702) rolls on the outer wall of the second limiting ring (82), thereby ensuring the stability of the screening tank (8) during the rotation process and facilitating disassembly and cleaning. Step 6: The liquid after centrifugal screening is discharged through the discharge port (14) at the bottom of the collector (4), collected and stored. At the same time, the equipment is monitored and adjusted through the control panel (15) to ensure the smooth progress of the entire preparation process.
Citation Information
Patent Citations
Preparation method of alogliptin
CN105777709A
