Filtering device for everolimus impurity synthesis

Abstract

The utility model relates to the technical field of medicine production filtering technologies, in particular to a filtering device for everolimus impurity synthesis. Comprising two groups of charging barrels and a group of liquid storage barrels which are arranged side by side, the charging barrels are used for storing mobile phases, the bottom ends of the charging barrels are detachably connected with filter barrels for containing silica gel, the bottom ends of the filter barrels are provided with liquid outlet pipes, the liquid outlet pipes are provided with liquid outlet valves, the bottom ends of the liquid storage barrels are provided with liquid transfer pipes, and the liquid outlet pipes are communicated with the liquid transfer pipes through connecting pipes. A liquid discharging pipe is arranged on the connecting pipe, a liquid discharging valve is arranged on the liquid discharging pipe, and the liquid storage cylinder is connected with a vacuumizing mechanism. The filtering efficiency in the synthesis process of the everolimus impurities is improved.

Description

Technical Field

[0001] This utility model relates to the field of pharmaceutical production filtration technology, and in particular to a filtration device for the synthesis of everolimus impurities. Background Technology

[0002] In the synthesis process of everolimus impurities, purification and filtration devices are required to filter the catalyst, remove additional impurity particles, separate unreacted raw materials, and other impurities.

[0003] In existing technologies, silica gel column chromatography is commonly used in the synthesis of everolimus impurities. Silica gel is used as the stationary phase, and the components are separated based on their different partition coefficients between the stationary and mobile phases. Everolimus impurities and the target product have different adsorption capacities on the silica gel surface. When a suitable eluent is used as the mobile phase, different substances will move at different speeds within the column with the eluent, thereby separating the everolimus impurities from other components and achieving the purpose of impurity filtration.

[0004] To improve filtration speed, existing technologies typically use pressurized mobile phase at the top of the silica gel column or negative pressure at the tail end to extract the mobile phase. Pressurization usually uses inert gas, but it's not possible to simultaneously pressurize and replenish the mobile phase. Negative pressure is usually achieved by drawing negative pressure from the tail end to elute the mobile phase within the silica gel column. However, negative pressure is only suitable for small-scale column chromatography in the laboratory, the mobile phase cannot be monitored in real time, and backflow can easily occur, causing chromatography failure. In addition, silica gel columns require regeneration and cleaning maintenance after a period of use, making them inconvenient to use. Utility Model Content

[0005] To address the issue of improving filtration efficiency in the synthesis process of everolimus impurities, this invention provides a filtration device for the synthesis of everolimus impurities.

[0006] This utility model provides a filtration device for the synthesis of everolimus impurities, comprising two sets of material cylinders arranged side by side and a set of liquid storage cylinders. The material cylinders are used to store the mobile phase. The bottom end of each material cylinder is detachably connected to a filter cylinder containing silica gel. The bottom end of each filter cylinder is provided with a liquid outlet pipe and a liquid outlet valve. The bottom end of the liquid storage cylinder is provided with a transfer pipe. The liquid outlet pipe and the transfer pipe are connected by a connecting pipe. The connecting pipe is provided with a drain pipe and a drain valve. The liquid storage cylinder is connected to a vacuum mechanism.

[0007] Furthermore, the feed cylinder is equipped with a liquid inlet pipe, and the liquid inlet pipe is equipped with a liquid inlet valve. The two sets of liquid inlet pipes on the feed cylinder are connected by a T-connector.

[0008] Furthermore, the vacuuming mechanism includes a suction pipe disposed on the upper part of the liquid storage cylinder and a vacuum pump connected to the suction pipe.

[0009] Further, the filter cartridge is connected with the inner cavity.

[0010] Further, the filter cartridge comprises a closed cover at the top end and a cylinder body, the closed cover is connected with the cylinder body through bolts, the filter cartridge is provided with a chromatographic cartridge containing silica gel, and a limiting rib is arranged on the inner wall of the filter cartridge.

[0011] Further, the filter cartridge comprises a closed cover at the top end and a cylinder body, the closed cover is connected with the cylinder body through bolts, the filter cartridge is provided with a chromatographic cartridge containing silica gel, and a limiting rib is arranged on the inner wall of the filter cartridge.

[0012] Further, the filter cartridge comprises a closed cover at the top end and a cylinder body, the closed cover is connected with the cylinder body through bolts, the filter cartridge is provided with a chromatographic cartridge containing silica gel, and a limiting rib is arranged on the inner wall of the filter cartridge.

[0013] Further, the filter cartridge comprises a closed cover at the top end and a cylinder body, the closed cover is connected with the cylinder body through bolts, the filter cartridge is provided with a chromatographic cartridge containing silica gel, and a limiting rib is arranged on the inner wall of the filter cartridge.

[0014] Further, the filter cartridge comprises a closed cover at the top end and a cylinder body, the closed cover is connected with the cylinder body through bolts, the filter cartridge is provided with a chromatographic cartridge containing silica gel, and a limiting rib is arranged on the inner wall of the filter cartridge.

[0015] Further, the filter cartridge comprises a closed cover at the top end and a cylinder body, the closed cover is connected with the cylinder body through bolts, the filter cartridge is provided with a chromatographic cartridge containing silica gel, and a limiting rib is arranged on the inner wall of the filter cartridge.

[0016] The utility model has the advantages of the following beneficial technical effects:

[0017] 1. The utility model provides a kind of filter device for synthesis of everolimus impurity, two groups of side-by-side cartridge are provided, can be alternately used, when the filter cartridge of one cartridge is regenerated and cleaned and other maintenance operations, another cartridge can continue to work, effectively improve the filtration efficiency, inlet tube is equipped on cartridge, and the inlet tube of two groups of cartridge is connected by tee pipe, it is convenient to switch the flow phase of different cartridge for subsequent chromatography filtration.

[0018] 2. The utility model provides a kind of filter device for synthesis of everolimus impurity, liquid storage cylinder connects vacuumizing mechanism, utilizes negative pressure to drive flow phase to pass through filter cartridge, realizes high-efficiency filtration.

[0019] 3.The utility model provides a kind of filtering device for synthesis of everolimus impurity, annular connecting wall of filter cartridge top end is equipped with the channel for connecting column embedding, this connection mode is convenient and fast, it is convenient to replace filter cartridge and maintain.Perforated backing plate is equipped at chromatographic cartridge bottom end, top end is equipped with anti-impact screen, and perforated backing plate can uniformly receive mobile phase, prevent silica gel leakage, and anti-impact screen can prevent mobile phase impact from causing silica gel layer to collapse, observation window is equipped on liquid storage cylinder, and the collection condition of liquid in liquid storage cylinder can be monitored at any time. BRIEF DESCRIPTION OF DRAWINGS

[0020] Figure 1 It is a kind of filtering device for synthesis of everolimus impurity of the utility model embodiment structure schematic diagram.

[0021] Figure 2 It is the structure schematic diagram of cartridge of the utility model embodiment.

[0022] Figure 3 It is the structure schematic diagram of filter cartridge of the utility model embodiment.

[0023] Figure 4 It is the sectional view of front view of filter cartridge of the utility model embodiment.

[0024] Among them, 1, cartridge;101, liquid inlet pipe;102, liquid inlet valve;103, tee pipe;104, inner cavity;105, outer cavity;1041, filter screen;106, connecting convex part;107, connecting column;2, filter cartridge;201, liquid outlet pipe;202, liquid outlet valve;203, annular connecting wall;204, channel;205, closure cover;206, barrel;207, bolt;208, limiting rib;209, sealing element one;210, support frame;211, sealing element two;3, liquid storage cylinder;301, liquid transfer pipe;302, check valve;303, observation window;4, connecting pipe;401, liquid discharge pipe;402, liquid discharge valve;5, vacuum extraction mechanism;501, air extraction pipe;502, vacuum pump;6, chromatographic cartridge;601, perforated backing plate;602, anti-impact screen. DETAILED DESCRIPTION

[0025] The utility model is further explained in detail in connection with drawings.

[0026] Embodiment 1

[0027] Refer to Figure 1The embodiment of the application discloses a filtering device for synthesizing everolimus impurities, which comprises two groups of material cylinders 1 arranged side by side, a group of liquid storage cylinders 3, the material cylinder 1 is used for storing a mobile phase, a filter cylinder 2 containing silica gel is detachably connected to the bottom end of the material cylinder 1, a liquid outlet pipe 201 is arranged at the bottom end of the filter cylinder 2, a liquid outlet valve 202 is arranged on the liquid outlet pipe 201, a liquid transfer pipe 301 is arranged at the bottom end of the liquid storage cylinder 3, the liquid outlet pipe 201 and the liquid transfer pipe 301 are communicated through a connecting pipe 4, a liquid discharge pipe 401 is arranged on the connecting pipe 4, a liquid discharge valve 402 is arranged on the liquid discharge pipe 401, and the liquid storage cylinder 3 is connected with a vacuum pumping mechanism 5.

[0028] With reference to Figure 1 A liquid inlet pipe 101 is arranged on the material cylinder 1, a liquid inlet valve 102 is arranged on the liquid inlet pipe 101, and the liquid inlet pipes 101 on the two groups of material cylinders 1 are connected through a three-way pipe 103.

[0029] The two groups of material cylinders 1 arranged side by side can store mobile phases respectively, the liquid inlet pipes 101 are connected through the three-way pipe 103, the same liquid inlet pipe can be connected, the mixed liquid to be separated can flow into the mixed liquid to be separated through the same liquid inlet pipe, and the liquid inlet valve 102 can change the flow direction of the mixed liquid.

[0030] With reference to Figure 1 The vacuum pumping mechanism 5 comprises a suction pipe 501 arranged on the upper portion of the liquid storage cylinder 3 and a vacuum pump 502 connected with the suction pipe 501.

[0031] The vacuum pumping mechanism 5 connected with the liquid storage cylinder 3 can draw the liquid storage cylinder 3 to a negative pressure state, a pressure difference generated by the negative pressure drives the mobile phase to quickly pass through the filter cylinder 2, and the filtering speed is improved. The check valve 302 can prevent the liquid in the liquid storage cylinder 3 from being sucked back to the filter cylinder 2, and ensures the smooth progress of the filtering process.

[0032] With reference to Figure 2 A filter screen 1041 is arranged in the material cylinder 1, the filter screen 1041 divides the material cylinder 1 into an inner cavity 104 and an outer cavity 105, the liquid inlet pipe 101 is communicated with the outer cavity 105, and the filter cylinder 2 is communicated with the inner cavity 104.

[0033] With reference to Figure 2 And Figure 3 A connecting convex part 106 is formed at the bottom end of the material cylinder 1, a connecting column 107 is arranged on the side wall of the connecting convex part 106, a ring-shaped connecting wall 203 matched with the connecting convex part 106 is arranged at the top end of the filter cylinder 2, and a groove 204, in which the connecting column 107 is embedded, is arranged on the connecting wall.

[0034] With reference to Figure 3The filter cartridge 2 comprises a closed cover 205 at the top end and a cartridge body 206, the closed cover 205 is connected with the cartridge body 206 through a bolt 207, a chromatographic cartridge 6 containing silica gel is arranged in the filter cartridge 2, and a limiting rib 208 is arranged on the inner wall of the filter cartridge 2, and the limiting rib 208 is used for limiting the chromatographic cartridge 6.

[0035] The filter cartridge 1 and the filter cartridge 2 are detachably connected in a mode that the connecting column 107 is embedded into the groove 204 through cooperation of the connecting convex part 106 and the annular connecting wall 203, and the closed cover 205 of the filter cartridge 2 is connected with the cartridge body 206 through the bolt 207, so that the closed cover 205 is convenient to open, and the chromatographic cartridge 6 and the silica gel inside are convenient to replace and maintain. The limiting rib 208 can easily take out and put in the chromatographic cartridge 6, and the maintenance efficiency is improved.

[0036] With reference to Figure 3 The chromatographic cartridge 6 is provided with a porous supporting plate 601 at the bottom end, and is provided with an anti-impact screen plate 602 at the top end.

[0037] With reference to Figure 3 The closed cover 205 is provided with a sealing element one 209 between the closed cover 205 and the chromatographic cartridge 6, the sealing element one 209 is a circular annular elastic rubber ring, the filter cartridge is a cylinder, and the diameter of the sealing element one 209 is the same as the diameter of the cross section of the filter cartridge 2.

[0038] With reference to Figure 4 The cartridge body 206 of the filter cartridge 2 is provided with a supporting frame 210 at the bottom, and the supporting frame 210 is provided with a sealing element two 211, the sealing element two 211 is a circular annular elastic rubber ring, and the diameter of the sealing element two 211 is the same as the diameter of the cross section of the filter cartridge 2.

[0039] The silica gel in the filter cartridge 2 serves as a stationary phase, and the difference in adsorption capacity of everolimus impurities and target products on the surface of silica gel is utilized, when the mobile phase carries the sample through the silica gel layer, different substances move at different speeds, so that the separation of each component is realized. The porous supporting plate 601 makes the mobile phase uniformly enter the silica gel layer, the anti-impact screen plate 602 ensures the stability of the silica gel layer under the impact of the mobile phase, and the separation effect is improved. The sealing element one 209 and the sealing element two 211 make the chromatographic cartridge 6 in a relatively sealed structure, and the negative pressure effect is improved.

[0040] The connecting part of the liquid transfer pipe 301 and the liquid storage cylinder 3 is provided with a check valve 302, and the liquid storage cylinder 3 is provided with an observation window 303. The lower end of the liquid storage cylinder 3 is provided with a pipeline connected with the next stage processing work.

[0041] Working: the mobile phase is injected into the inner cavity 104 of the two barrels 1 through the inlet pipe 101, the impurity mixture of the evirolimus to be filtered enters the outer cavity 105, and then enters the inner cavity 104 after being filtered by the filter screen 1041. The silica gel is filled in the chromatographic cartridge 6, the chromatographic cartridge 6 is placed in the filter cartridge 2, and then the sealing cover 205 is installed, the bolt 207 is tightened, and the sealing is ensured.

[0042] Filtering stage: open the liquid outlet valve 202 at the bottom end of the filter cartridge 2 of one barrel 1, and start the vacuum pump 502 of the liquid storage cartridge 3 at the same time, so that the liquid storage cartridge 3 is pumped to a negative pressure state. Under the action of negative pressure, the mobile phase in the barrel 1 passes through the silica gel layer in the filter cartridge 2, and the evirolimus impurities and the target product are separated under the action of the silica gel. The separated liquid enters the liquid storage cartridge 3 through the liquid outlet pipe 201, the connecting pipe 4 and the liquid transfer pipe 301. The separation condition is observed, and the remaining mobile phase not containing the target product is discharged through the liquid discharge pipe 401.

[0043] Switching and maintenance stage: when the working filter cartridge 2 needs to be regenerated or cleaned, the liquid outlet valve 202 thereof is closed, and the liquid outlet valve 202 of the other barrel 1 is opened, so as to switch to the other filter cartridge 2. The filter cartridge 2 to be maintained is disassembled from the barrel 1, the sealing cover 205 is opened, and the chromatographic cartridge 6 is taken out for maintenance operation such as silica gel replacement and cleaning.

[0044] Monitoring the mobile phase: the operator can observe the collection condition of the liquid in the liquid storage cartridge 3 through the observation window 303 at any time, and adjust the suction of the vacuum pump 502.

[0045] The above are preferred embodiments of the present application, and are not limited to the protection scope of the present application, so that: any equivalent changes made according to the structure, shape and principle of the present application should be covered in the protection scope of the present application.

Claims

1. A filtering device for synthesizing an everolimus impurity, characterized by, The application relates to a liquid storage device, which comprises two groups of liquid containers (1) arranged side by side, a group of liquid storage containers (3), the liquid containers (1) are used for storing mobile phases, the bottom end of the liquid containers (1) is detachably connected with a filter container (2) containing silica gel, the bottom end of the filter container (2) is provided with a liquid outlet pipe (201), the liquid outlet pipe (201) is provided with a liquid outlet valve (202), the bottom end of the liquid storage container (3) is provided with a liquid transfer pipe (301), the liquid outlet pipe (201) and the liquid transfer pipe (301) are communicated through a connecting pipe (4), the connecting pipe (4) is provided with a liquid discharge pipe (401), the liquid discharge pipe (401) is provided with a liquid discharge valve (402), and the liquid storage container (3) is connected with a vacuum pumping mechanism (5).

2. The filtration device for synthesis of everolimus impurities according to claim 1, characterized in that, The liquid containers (1) are provided with liquid inlet pipes (101), the liquid inlet pipes (101) are provided with liquid inlet valves (102), and the liquid inlet pipes (101) of the two groups of liquid containers (1) are connected through a three-way pipe (103).

3. The filtration device for synthesis of everolimus impurities according to claim 2, characterized in that, The vacuum pumping mechanism (5) comprises an air suction pipe (501) arranged on the upper portion of the liquid storage container (3) and a vacuum pump (502) connected with the air suction pipe (501).

4. The filtration device for synthesis of everolimus impurities according to claim 3, characterized in that, The liquid containers (1) are provided with filter screens (1041), the filter screens (1041) divide the liquid containers (1) into inner cavities (104) and outer cavities (105), the liquid inlet pipes (101) are communicated with the outer cavities (105), and the filter containers (2) are communicated with the inner cavities (104).

5. The filtration device for synthesis of everolimus impurities according to claim 4, characterized in that, The bottom end of the liquid containers (1) is formed with a connecting convex portion (106), the side wall of the connecting convex portion (106) is provided with a connecting column (107), the top end of the filter container (2) is provided with an annular connecting wall (203) matched with the connecting convex portion (106), and the connecting wall is provided with a groove (204) for embedding the connecting column (107).

6. The filtration device for synthesis of everolimus impurities according to claim 5, characterized by, The filter container (2) comprises a closed cover (205) at the top end and a container body (206), the closed cover (205) is connected with the container body (206) through bolts (207), the filter container (2) is provided with a chromatographic container (6) containing silica gel, and the inner wall of the filter container (2) is provided with limiting ribs (208) for limiting the chromatographic container (6).

7. The filtration device for synthesis of everolimus impurities according to claim 6, characterized by, The bottom end of the chromatographic container (6) is provided with a porous supporting plate (601), and the top end of the chromatographic container (6) is provided with an anti-collapse sieve plate (602).

8. The filtration device for synthesis of everolimus impurities according to claim 7, characterized by, The closed cover (205) and the chromatographic container (6) are provided with a sealing member I (209), the sealing member I (209) is a circular elastic rubber ring, the filter container (2) is cylindrical, and the diameter of the sealing member I (209) is the same as the diameter of the cross section of the filter container (2).

9. The filtration device for synthesis of everolimus impurities according to claim 8, characterized by, The bottom portion of the container body (206) of the filter container (2) is provided with a supporting frame (210), and the supporting frame (210) is provided with a sealing member II (211), the sealing member II (211) is a circular elastic rubber ring, and the diameter of the sealing member II (211) is the same as the diameter of the cross section of the filter container (2).

10. The filtration device for synthesis of everolimus impurities according to claim 9, characterized by, The connecting position of the liquid transfer pipe (301) and the liquid storage container (3) is provided with a check valve (302), and the liquid storage container (3) is provided with an observation window (303).

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