Low-temperature thickener

Abstract

The utility model provides a low-temperature concentrator, and aims to solve the technical problems that in the process of synthesizing fondaparinux sodium, a traditional rotary evaporator is adopted for concentration and separation, time consumption is long, and products have degradation risks. The concentration barrel is sequentially divided into a middle barrel body and an upper barrel body from bottom to top, and the inner spaces of the middle barrel body and the upper barrel body are mutually communicated. And the middle cylinder is provided with a heating unit. And a vacuum pipeline is arranged at the top of the upper cylinder body. The rotating unit is provided with a rotating table, the rotating table is arranged in the middle barrel, and a containing groove is formed in the rotating table from top to bottom. The turntable is connected with a motor. The liquid injection unit is matched with the rotary table and comprises a liquid pipeline and a liquid injection head. One end of the liquid pipeline penetrates through the side wall of the middle cylinder and then extends to the upper part of the rotary table. The liquid injection head is movably installed at one end of the liquid pipeline. A liquid injection hole set matched with the containing groove is formed in the bottom end of the liquid injection head and used for liquid injection of the containing groove. And through the matching effect between the rotary table and the liquid injection head provided with the liquid injection hole group, the liquid material is distributed into a liquid film in the accommodating groove, and the evaporation area is favorably increased.

Description

Technical Field

[0001] The present application relates to the field of concentrators, and in particular to a low-temperature concentrator. Background Art

[0002] Fondaparinux sodium is a synthetic heparin pentasaccharide drug that plays a particularly significant role in the prevention and treatment of thromboembolism and venous thrombotic diseases in orthopedic joint replacements. The synthetic route of Fondaparinux sodium is relatively long, with the number of reaction steps ranging from 50 to more than 70. Throughout the entire synthesis process, column purification is often involved many times to collect components, and then concentrate them on a rotary evaporator to separate the target product. During the operation, the technicians found that due to the large volume of the collected liquid obtained after multiple column purifications, it usually takes a long time to concentrate it on a rotary evaporator. Moreover, most of the target products are not tolerant to high temperatures, and there is a risk of degradation of the target products when separated by a rotary evaporator. Utility Model Content

[0003] The utility model provides a low-temperature concentrator to solve the problems raised in the above background technology.

[0004] A cryogenic concentrator, characterized in that: the cryogenic concentrator comprises:

[0005] The concentrating cylinder is divided into a middle cylinder body and an upper cylinder body from bottom to top, the cylinder spaces of which are interconnected; the middle cylinder body is provided with a heating unit; and the top of the upper cylinder body is provided with a vacuum pipe;

[0006] The rotating unit has a turntable; the turntable is arranged in the middle cylinder and has a receiving groove from top to bottom; the turntable is connected to a motor;

[0007] A liquid injection unit, matched with the turntable, comprising a liquid pipeline and a liquid injection head;

[0008] The liquid pipeline has one end that passes through the side wall of the middle cylinder and extends to the top of the turntable;

[0009] The injection head is movably mounted on one end of the liquid pipeline; a group of injection holes matching the receiving tank is provided at the bottom of the injection head for injecting liquid into the receiving tank.

[0010] Furthermore, the injection hole group has a plurality of injection holes; the plurality of injection holes are arranged in sequence along the circumference of the injection head at the bottom end of the injection head from the outer edge of the injection head to the center of the injection head, and the injection hole group is arranged densely outside and sparsely inside.

[0011] Furthermore, the concentrating cylinder further comprises a lower cylinder body, and the lower cylinder body and the middle cylinder body are not interconnected; the lower cylinder body is equipped with a motor.

[0012] Furthermore, the rotating unit also includes a rotating shaft; one end of the rotating shaft is connected to the movable end of the motor, and the other end passes through the top of the lower cylinder and is connected to the bottom end of the turntable; a sealing ring is provided at the connection between the rotating shaft and the lower cylinder.

[0013] Furthermore, a maintenance passage is provided on the side wall of the lower cylinder.

[0014] Furthermore, the heating unit is a heating jacket; the heating jacket is arranged on the side wall near the bottom end of the middle cylinder.

[0015] Furthermore, the liquid pipeline includes a horizontal pipe and a vertical pipe;

[0016] The transverse pipe penetrates the side wall of the middle cylinder from outside to inside and extends to the top of the turntable; the transverse pipe is threadedly connected to the side wall of the middle cylinder, and a regulating valve is provided at one end of the transverse pipe exposed from the middle cylinder;

[0017] One end of the vertical tube is connected to one end of the horizontal tube arranged in the middle cylinder body, and the other end is arranged toward the direction close to the containing groove and has the injection head movably installed thereon; the total length of the vertical tube and the injection head is arranged to match the inner space of the middle cylinder body.

[0018] Furthermore, a replacement channel is provided on the side wall of the upper cylinder; the replacement channel is sealed or opened by a flange.

[0019] Furthermore, the accommodating groove is a cylindrical structure.

[0020] Compared with the prior art, the beneficial effects of the utility model are:

[0021] (1) Through the cooperation between the turntable and the injection head provided with the injection hole group, the liquid material is distributed into a liquid film in the holding tank, thereby increasing the evaporation area, so that the liquid material can evaporate at a lower temperature, saving energy consumption while reducing the risk of decomposition of the target product. At the same time, it also greatly increases the evaporation rate of the liquid material, which is conducive to shortening the synthesis cycle of fondaparinux sodium.

[0022] (2) By rotating the liquid pipeline, the injection head is rotated to a position close to the upper cylinder, so that the technicians can replace the injection head through the replacement channel, thereby ensuring the normal operation of the cryogenic concentrator. BRIEF DESCRIPTION OF THE DRAWINGS

[0023] In order to more clearly illustrate the embodiments of the present application or the technical solutions in the prior art, the drawings required for use in the embodiments or the description of the prior art will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present application. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying creative work.

[0024] Figure 1 A schematic cross-sectional structure diagram of a cryogenic concentrator according to an embodiment of the present application;

[0025] Figure 2 This is a structural schematic diagram of a cryogenic concentrator according to an embodiment of the present application (the upper cylinder is not shown);

[0026] Figure 3 This is a top view of a liquid injection head of a low-temperature concentrator according to an embodiment of the present application.

[0027] Reference numerals:

[0028] 10. upper cylinder; 100. replacement channel; 11. middle cylinder; 12. lower cylinder; 13. vacuum pipe; 14. heating jacket;

[0029] 20. Turntable; 201. Accommodating slot; 21. Rotating shaft; 22. Motor;

[0030] 30. Liquid pipeline; 300. Horizontal pipe; 301. Vertical pipe; 31. Liquid injection head; 311. Liquid injection hole; 32. Regulating valve. DETAILED DESCRIPTION

[0031] In the following, only some exemplary embodiments are briefly described. As those skilled in the art will appreciate, the described embodiments may be modified in various ways without departing from the spirit or scope of the present invention. Therefore, the drawings and descriptions are considered to be exemplary and non-restrictive in nature.

[0032] In the description of the present utility model, it should be understood that the terms "center", "length", "thickness", "top", "top", "bottom", "inside", "outside", "clockwise", "counterclockwise", "circumferential" and the like indicate orientations or positional relationships based on the orientations or positional relationships shown in the accompanying drawings, or are the orientations or positional relationships conventionally placed when the product of the present utility model is used, or are the orientations or positional relationships conventionally understood by those skilled in the art. They are only for the convenience of describing the present utility model and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and therefore should not be understood as a limitation on the present utility model.

[0033] In addition, in the description of the present invention, “plurality” means two or more than two, unless otherwise clearly and specifically defined.

[0034] In the present invention, unless otherwise clearly specified and limited, the terms "installed", "connected", "connected" and the like should be understood in a broad sense, for example, it can be a fixed connection, a detachable connection, or an integral connection; it can be a mechanical connection, an electrical connection, or a communication; it can be a direct connection, or an indirect connection through an intermediate medium, it can be the internal connection of two elements or the interaction relationship between two elements. For ordinary technicians in this field, the specific meanings of the above terms in the present invention can be understood according to specific circumstances.

[0035] In the present utility model, unless otherwise clearly specified and limited, a first feature being "above" or "below" a second feature may include that the first and second features are in direct contact, or may include that the first and second features are not in direct contact but are in contact through another feature between them. Moreover, a first feature being "above", "above" and "above" a second feature includes that the first feature is directly above and obliquely above the second feature, or simply indicates that the first feature is higher in level than the second feature. A first feature being "below", "below" and "below" a second feature includes that the first feature is directly below and obliquely below the second feature, or simply indicates that the first feature is lower in level than the second feature.

[0036] The disclosure below provides many different embodiments or examples for realizing different structures of the present invention. In order to simplify the disclosure of the present invention, the components and settings of specific examples are described below. Of course, they are only examples, and the purpose is not to limit the present invention. In addition, the present invention may repeat reference numerals in different examples, and such repetition is for the purpose of simplification and clarity, and does not itself indicate the relationship between the various embodiments discussed.

[0037] The embodiments of the present utility model are described in detail below with reference to the accompanying drawings.

[0038] The present invention provides a cryogenic concentrator. Figure 1-Figure 3 The low-temperature concentrator can be applied to the production and preparation of fondaparinux sodium, and comprises a concentrating cylinder, a rotating unit and a liquid injection unit.

[0039] Specifically,

[0040] The concentrating cylinder is divided into a lower cylinder 12, a middle cylinder 11 and an upper cylinder 10 from bottom to top. The lower cylinder 12 and the middle cylinder 11 are not intercommunication, and the cylinder spaces of the middle cylinder 11 and the upper cylinder 10 are intercommunication. A heating jacket 14 is provided on the side wall near the bottom of the middle cylinder 11. A vacuum pipe 13 is provided on the top of the upper cylinder 10, and the vacuum pipe 13 is connected to a vacuum pump to suck out the steam in the concentrating cylinder. A replacement channel 100 is provided on the side wall of the upper cylinder 10, and the replacement channel 100 is sealed or opened by a flange.

[0041] The rotating unit includes a motor 22, a turntable 20 and a rotating shaft 21. The motor 22 is installed on the lower cylinder 12. In order to facilitate the maintenance of the motor 22, a maintenance channel is provided on the side wall of the lower cylinder 12. The turntable 20 is arranged in the middle cylinder 11 and is arranged close to the heating jacket 14. The turntable 20 can be heated by the heating jacket 14. The turntable 20 is provided with a receiving groove 201 from the top to the bottom. Preferably, the receiving groove 201 is a cylindrical structure as a whole. The rotating shaft 21, one end of which is connected to the movable end of the motor 22, and the other end passes through the top of the lower cylinder 12 and is connected to the turntable 21. The rotating shaft 21 is rotatably connected to the top of the lower cylinder 12, and a sealing ring is provided at the connection between the rotating shaft 21 and the lower cylinder 12. When the motor 22 is started, the rotating shaft 21 is driven to rotate clockwise / counterclockwise, thereby driving the turntable 20 to rotate clockwise / counterclockwise.

[0042] The liquid injection unit is matched with the turntable 20 , that is, the liquid injection unit can transfer liquid materials to the receiving tank 201 of the turntable 20 . The liquid injection unit includes a liquid pipeline 30 and a liquid injection head 31 .

[0043] The liquid pipeline 30, one end of which penetrates the side wall of the middle cylinder 11, extends to the top of the turntable 20. The liquid pipeline 30 includes a horizontal pipe 300 and a vertical pipe 301. The horizontal pipe 300 penetrates the side wall of the middle cylinder 11 from the outside to the inside, and extends to the top of the turntable 20. The horizontal pipe 300 is threadedly connected to the side wall of the middle cylinder 11, and a regulating valve 32 is provided at one end of the horizontal pipe 300 exposed in the middle cylinder 11. One end of the vertical pipe 301 is connected to one end of the horizontal pipe 300 provided in the middle cylinder 11, and the other end thereof is provided toward the receiving groove 201 close to the turntable 20.

[0044] The injection head 31 is movably mounted at the other end of the vertical pipe 301 and communicates with the liquid pipeline 30. The injection head 31 is matched with the receiving tank 201, that is, the cross-sectional shape of the bottom end of the injection head 31 is equal to the cross-sectional shape of the receiving tank 201, and the size of the cross-sectional shape of the bottom end of the injection head 31 is equal to or slightly smaller than the size of the cross-sectional shape of the receiving tank 201. A group of injection holes arranged along the circumference of the injection head 31 is opened at the bottom end of the injection head 31. The liquid material transmitted by the liquid pipeline 30 can be sent to the receiving tank 201 through the injection hole group of the injection head 31, and then the liquid material is distributed into a liquid film in the receiving tank 201 as the turntable 20 rotates, thereby increasing the evaporation area of ​​the liquid material.

[0045] In order to improve the uniformity of the thickness of the liquid film distributed at the bottom of the receiving tank 201, preferably, the multiple injection holes 311 of the injection hole group are arranged at the bottom of the injection head 31 along the circumference of the injection head 31 from the outer edge of the injection head 31 to the center of the injection head 31, and the injection hole 311 group is arranged in a dense outer and sparse inner manner. The total length of the vertical pipe 301 and the injection head 31 is set to match the inner space of the middle cylinder 11, that is, taking the vertical pipe 301, the injection head 31 and the middle cylinder 11 as coaxial, the total length of the vertical pipe 301 and the injection head 31 is smaller than the inner diameter of the middle cylinder 11, so that when the liquid pipeline 30 rotates, it can drive the injection head 31 to rotate to the vicinity of the upper cylinder 10. When the injection hole group is blocked, the liquid pipeline 30 is rotated to drive the injection head 31 to rotate toward the upper cylinder 10, so that the technician can replace the injection head 31 through the replacement channel 300.

[0046] Based on the above embodiments, the working principle of this application is as follows:

[0047] First, the turntable 20 is heated to about 40°C by the heating jacket 14, and then the transmission flow of the liquid pipeline 30 is adjusted by controlling the regulating valve 32, so that the liquid material passes through the liquid pipeline 30 and the injection head 31 in sequence and falls into the receiving tank 201 of the turntable 20. The motor 22 is started, and in the process of the motor 22 driving the turntable 20 to rotate, the liquid material is distributed into a liquid film in the receiving tank 201. The liquid film begins to evaporate under the heating condition, and the resulting vapor is extracted from the vacuum pipeline 13 through the vacuum pump, thereby realizing the rapid concentration and separation of the liquid material.

[0048] Based on the above embodiments, the advantages of this application are:

[0049] (1) Through the cooperation between the turntable 20 and the injection head 31 provided with the injection hole group, the liquid material is distributed into a liquid film in the containing tank 201, thereby increasing the evaporation area, so that the liquid material can evaporate at a relatively low temperature, saving energy consumption while reducing the risk of decomposition of the target product. At the same time, the evaporation rate of the liquid material is also greatly increased, which is conducive to shortening the synthesis cycle of fondaparinux sodium.

[0050] (2) By rotating the liquid pipeline 30, the injection head 31 is rotated to a position close to the upper cylinder 10, so that the technicians can replace the injection head 31 through the replacement channel 100, thereby ensuring the normal operation of the cryogenic concentrator.

Claims

1. A cryogenic concentrator, characterized in that: The cryogenic concentrator comprises: The concentrating cylinder is divided into a middle cylinder body and an upper cylinder body from bottom to top, the cylinder spaces of which are interconnected; the middle cylinder body is provided with a heating unit; and the top of the upper cylinder body is provided with a vacuum pipe; The rotating unit has a turntable; the turntable is arranged in the middle cylinder and has a receiving groove from top to bottom; the turntable is connected to a motor; A liquid injection unit, matched with the turntable, comprising a liquid pipeline and a liquid injection head; The liquid pipeline has one end that passes through the side wall of the middle cylinder and extends to the top of the turntable; The injection head is movably mounted on one end of the liquid pipeline; a group of injection holes matching the receiving tank is provided at the bottom of the injection head for injecting liquid into the receiving tank.

2. The cryogenic concentrator according to claim 1, characterized in that: The injection hole group has a plurality of injection holes; the plurality of injection holes are arranged in sequence along the circumference of the injection head at the bottom end of the injection head from the outer edge of the injection head to the center of the injection head, and the injection hole group is arranged in a dense outer and sparse inner manner.

3. The cryogenic concentrator according to claim 1, characterized in that: The concentrating cylinder further comprises a lower cylinder body, and the lower cylinder body and the middle cylinder body are not intercommunication; the lower cylinder body is equipped with a motor.

4. The cryogenic concentrator according to claim 3, characterized in that: The rotating unit also includes a rotating shaft; one end of the rotating shaft is connected to the movable end of the motor, and the other end passes through the top of the lower cylinder and is connected to the bottom of the turntable; a sealing ring is provided at the connection between the rotating shaft and the lower cylinder.

5. The cryogenic concentrator according to claim 3, characterized in that: A maintenance passage is provided on the side wall of the lower cylinder.

6. The cryogenic concentrator according to claim 1, characterized in that: The heating unit is a heating jacket; the heating jacket is arranged on the side wall near the bottom end of the middle cylinder.

7. The cryogenic concentrator according to claim 1, characterized in that: The liquid pipeline includes a horizontal pipe and a vertical pipe; The transverse pipe penetrates the side wall of the middle cylinder from outside to inside and extends to the top of the turntable; the transverse pipe is threadedly connected to the side wall of the middle cylinder, and a regulating valve is provided at one end of the transverse pipe exposed from the middle cylinder; One end of the vertical tube is connected to one end of the horizontal tube arranged in the middle cylinder body, and the other end is arranged toward the direction close to the containing groove and has the liquid injection head movably installed thereon; the total length of the vertical tube and the liquid injection head is arranged to match the inner space of the middle cylinder body.

8. The cryogenic concentrator according to claim 7, characterized in that: A replacement channel is arranged on the side wall of the upper cylinder; the replacement channel is sealed or opened by a flange.

9. The cryogenic concentrator according to claim 1, characterized in that: The containing groove is a cylindrical structure.

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