Efficient oxytetracycline hydrochloride synthesis equipment and synthesis method thereof

Abstract

The invention belongs to the technical field of crystallization separation, and particularly relates to oxytetracycline hydrochloride high-efficiency synthesis equipment and a synthesis method thereof.The oxytetracycline hydrochloride high-efficiency synthesis equipment comprises a crystallization barrel used for containing a mixed solution and crystallizing through cooling; the cleaning ring is attached to the inner wall of the crystallization barrel and is driven by an air cylinder to ascend and descend so as to scrape crystals on the inner wall of the crystallization barrel out of the crystallization barrel; the collecting mechanism rotates around the crystallization barrel to receive the crystals brought out by the cleaning ring, the received crystals are flatly laid at a barrel opening of the crystallization barrel, the cleaning ring of the oxytetracycline hydrochloride efficient synthesis equipment scrapes oxytetracycline hydrochloride crystals on the inner wall of the crystallization barrel out of the crystallization barrel, and temperature conduction is prevented from being affected by the crystals; meanwhile, oxytetracycline hydrochloride crystals scraped out of the crystallization barrel are collected by a collecting mechanism and flatly laid at the barrel opening of the crystallization barrel, so that the mixed solution deposited at the bottom of the annular temporary storage tank enters the crystallization barrel again to be crystallized to form circulation.

Description

Technical Field

[0001] The present invention belongs to the technical field of crystallization separation, and specifically relates to crystallization from a solution, and in particular to a highly efficient synthesis device of oxytetracycline hydrochloride and a synthesis method thereof. Background Art

[0002] Oxytetracycline hydrochloride is a yellow crystalline powder, odorless, slightly bitter, slightly hygroscopic, easily soluble in water, slightly soluble in ethanol, and insoluble in chloroform or ether.

[0003] The preparation process of oxytetracycline hydrochloride includes: dissolving, filtering, crystallizing, drying and crushing. In the process of cooling crystallization, the mixed solution is easy to crystallize on the inner wall of the crystallization barrel, and the crystals have strong adhesion and are difficult to fall off automatically. At the same time, the crystals on the inner wall of the crystallization barrel will also affect temperature conduction and reduce crystallization efficiency.

[0004] Therefore, how to solve the problem that the crystals attached to the inner wall of the crystallization barrel reduce the crystallization efficiency during the preparation of oxytetracycline hydrochloride is a technical problem that technical personnel in this field urgently need to solve.

[0005] It should be noted that the above information disclosed in this background technology section is only used to understand the background technology of the present application concept, and therefore, the above description is not considered to constitute information of the prior art. Summary of the invention

[0006] The embodiments of the present disclosure at least provide a highly efficient synthesis device and method of oxytetracycline hydrochloride.

[0007] In the first aspect, the embodiments of the present disclosure provide an efficient synthesis device of oxytetracycline hydrochloride, which includes: a crystallization barrel, which is used to hold a mixed solution and crystallize by cooling; a cleaning ring, which is in contact with the inner wall of the crystallization barrel and is driven by a cylinder to achieve lifting and lowering so as to scrape the crystals on the inner wall of the crystallization barrel out of the crystallization barrel; and a collecting mechanism, which rotates around the crystallization barrel to receive the crystals brought out by the cleaning ring, and spreads the received crystals at the barrel mouth of the crystallization barrel.

[0008] In an optional embodiment, an annular temporary storage groove is provided at the barrel mouth of the crystallization barrel; the collecting mechanism rotates along the annular temporary storage groove to scrape the crystals on the cleaning ring onto the annular temporary storage groove and spread them flat.

[0009] In an optional embodiment, the collection mechanism includes: a scraper and a drive assembly; the bottom of the annular temporary storage groove is inclined; the upper surface of the cleaning ring is inclined, and its inclination slope is the same as the bottom of the annular temporary storage groove; the lower surface of the scraper is inclined, and its inclination slope is the same as the bottom of the annular temporary storage groove; wherein, when the cleaning ring extends out of the crystallization barrel, the drive assembly drives the scraper to rotate along the annular temporary storage groove to scrape the crystals on the cleaning ring to the annular temporary storage groove and spread them flat.

[0010] In an optional embodiment, one end of the scraper extends out of the annular temporary storage groove, and the scraper is inclined toward the rotation direction so as to scrape the crystals on the cleaning ring to the annular temporary storage groove.

[0011] In an optional embodiment, the driving assembly includes: an annular guide rail, a slip ring and a driver; the annular guide rail is arranged on the side wall of the crystallization barrel, the slip ring is arranged on the annular guide rail, and the scraper is arranged on the slip ring; the driver is engaged with the second gear on the side wall of the slip ring through the first gear to drive the slip ring to rotate, so that the scraper rotates along the annular temporary storage groove.

[0012] In an optional embodiment, a drain port connected to the crystallization barrel is provided at the bottom of the annular temporary storage tank; a filter membrane is provided in the drain port.

[0013] In an optional embodiment, the rising height of the cleaning ring increases gradually.

[0014] In the second aspect, the embodiment of the present disclosure provides a synthesis method using the high-efficiency oxytetracycline hydrochloride synthesis equipment as described above, which comprises the following steps: step S1, adding methanol, anhydrous calcium chloride, oxytetracycline powder and activated carbon into a container in sequence, and stirring the mixture; step S2, filtering the mixture to obtain a mixed solution; step S3, adding hydrogen chloride solution to the mixed solution in the crystallization barrel for cooling and crystallization; step S4, scraping the crystals on the inner wall of the crystallization barrel out of the crystallization barrel through a cleaning ring, and spreading the scraped crystals into an annular temporary storage tank at the barrel mouth through a collecting mechanism; step S5, crushing and packaging the crystals.

[0015] In an optional embodiment, the bottom of the annular temporary storage groove is inclined; the upper surface of the cleaning ring is inclined, and its inclination slope is the same as the bottom of the annular temporary storage groove; the lower surface of the scraper is inclined, and its inclination slope is the same as the bottom of the annular temporary storage groove.

[0016] In an optional embodiment, one end of the scraper extends out of the annular temporary storage groove, and the scraper is inclined toward the rotation direction.

[0017] The beneficial effect of the present invention is that the oxytetracycline hydrochloride efficient synthesis equipment and the synthesis method thereof scrape the oxytetracycline hydrochloride crystals on the inner wall of the crystallization barrel out of the crystallization barrel through a cleaning ring to prevent the crystallization from affecting the temperature conduction; at the same time, the oxytetracycline hydrochloride crystals scraped out of the crystallization barrel are collected by a collecting mechanism and spread flat at the barrel mouth of the crystallization barrel, so that the mixed solution deposited at the bottom of the annular temporary storage tank enters the crystallization barrel again for a crystallization formation cycle.

[0018] Other features and advantages of the present invention will be described in the following description, and partly become apparent from the description, or understood by practicing the present invention. The purpose and other advantages of the present invention are realized and obtained by the structures particularly pointed out in the description, claims and drawings.

[0019] In order to make the above-mentioned objects, features and advantages of the present invention more obvious and easy to understand, this article specifically cites preferred embodiments and provides detailed descriptions as follows in conjunction with the attached drawings. BRIEF DESCRIPTION OF THE DRAWINGS

[0020] In order to more clearly illustrate the specific implementation methods of the present invention or the technical solutions in the prior art, the drawings required for use in the specific implementation methods or the description of the prior art will be briefly introduced below. Obviously, the drawings described below are some implementation methods of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying creative work.

[0021] Figure 1 A schematic diagram of the structure of an efficient synthesis device of oxytetracycline hydrochloride provided in an embodiment of the present disclosure; Figure 2 A schematic diagram of the structure of a collection mechanism provided by an embodiment of the present disclosure; Figure 3 A schematic cross-sectional view of a collecting mechanism provided in an embodiment of the present disclosure; Figure 4 A schematic diagram of the structure of a cleaning ring lifting a scraper upward provided in an embodiment of the present disclosure.

[0022] In the figure: Crystallization barrel 1, annular temporary storage tank 11, and liquid discharge port 12; Stirring component 2; Cleaning ring 3; Collecting mechanism 4 , scraper 41 , driving assembly 42 , annular guide rail 421 , slip ring 422 , driver 423 , first gear 424 , second gear 425 , bracket 43 . DETAILED DESCRIPTION

[0023] In order to make the purpose, technical solution and advantages of the embodiments of the present invention clearer, the technical solution of the present invention will be clearly and completely described below in conjunction with the accompanying drawings. Obviously, the described embodiments are 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.

[0024] It should be noted that similar reference numerals and letters represent similar items in the following drawings, so once an item is defined in one drawing, it does not need to be further defined and explained in the subsequent drawings. In addition, in the drawings, the thickness of the components may be exaggerated or reduced in order to effectively describe the technical content.

[0025] Some embodiments of the present invention are described in detail below in conjunction with the accompanying drawings. In the absence of conflict, the following embodiments and features in the embodiments can be combined with each other.

[0026] like Figure 1 As shown, at least one embodiment provides a high-efficiency synthesis device of oxytetracycline hydrochloride, which includes: a crystallization barrel 1, which is used to hold a mixed solution and crystallize by cooling; a cleaning ring 3, which is in contact with the inner wall of the crystallization barrel 1 and is driven by a cylinder to achieve lifting and lowering so as to scrape the crystals on the inner wall of the crystallization barrel 1 out of the crystallization barrel 1; and a collecting mechanism 4, which rotates around the crystallization barrel 1 to receive the crystals brought out by the cleaning ring 3, and spreads the received crystals at the barrel mouth of the crystallization barrel 1.

[0027] Specifically, the cleaning ring 3 and the collecting mechanism 4 are controlled by the control module; the mixed solution in the crystallization barrel 1 is gradually crystallized by low temperature. When a certain amount of oxytetracycline hydrochloride crystals are formed on the inner wall of the crystallization barrel 1, the control module controls a lifting cylinder to drive the cleaning ring 3 to rise, thereby bringing the oxytetracycline hydrochloride crystals on the inner wall of the crystallization barrel 1 out of the crystallization barrel 1. Then the control module controls the collecting mechanism 4 to rotate, and the oxytetracycline hydrochloride crystals are scraped from the cleaning ring 3 to the barrel mouth of the crystallization barrel 1 through the rotation of the collecting mechanism 4, and the collected crystals are spread out.

[0028] In some embodiments, a stirring component 2 is provided in the crystallization barrel 1, and the stirring component 2 accelerates the crystallization of oxytetracycline hydrochloride by periodic stirring.

[0029] like Figure 2 As shown, in some embodiments, an annular temporary storage groove 11 is provided at the barrel mouth of the crystallization barrel 1; the collecting mechanism 4 rotates along the annular temporary storage groove 11 to scrape the crystals on the cleaning ring 3 onto the annular temporary storage groove 11 and spread them flat.

[0030] like Figure 3 As shown, in some embodiments, the collecting mechanism 4 includes: a scraper 41 and a driving assembly 42; the bottom of the annular temporary storage groove 11 is inclined; the upper surface of the cleaning ring 3 is inclined, and its inclination slope is the same as the bottom of the annular temporary storage groove 11; the lower surface of the scraper 41 is inclined, and its inclination slope is the same as the bottom of the annular temporary storage groove 11; wherein, when the cleaning ring 3 extends out of the crystallization barrel 1, the driving assembly 42 drives the scraper 41 to rotate along the annular temporary storage groove 11 to scrape the crystals on the cleaning ring 3 to the annular temporary storage groove 11 and spread them flat.

[0031] Specifically, the cleaning ring 3 stops when it rises to a point where its inclined surface is slightly higher than the bottom of the annular temporary storage tank 11, so that the scraper 41 can spread the received oxytetracycline hydrochloride crystals during rotation; wherein the scraper 41 is connected to the drive assembly 42 through the bracket 43, and the scraper 41 is inserted into the bracket 43, and a damping plate is provided between the two to increase the resistance, so that the scraper 41 will only rise after being subjected to force.

[0032] like Figure 4 As shown, in some embodiments, the rising height of the cleaning ring 3 increases gradually.

[0033] Specifically, the height to which the cleaning ring 3 rises each time after cleaning is a little higher than the previous time, in order to leave accumulation space for the annular temporary storage groove 11, that is, the cleaning ring 3 pushes the scraper 41 to overcome the resistance of the damping plate and rise.

[0034] In some embodiments, one end of the scraper 41 extends out of the annular temporary storage groove 11 , and the scraper 41 is inclined toward the rotation direction so as to scrape the crystals on the cleaning ring 3 to the annular temporary storage groove 11 .

[0035] Specifically, one end of the scraper 41 extends into the area of ​​the cleaning ring 3 , so as to facilitate scraping away the crystals on the cleaning ring 3 .

[0036] like Figure 2 As shown, in some embodiments, the driving assembly 42 includes: an annular guide rail 421, a slip ring 422 and a driver 423; the annular guide rail 421 is arranged on the side wall of the crystallization barrel 1, the slip ring 422 is arranged on the annular guide rail 421, and the scraper 41 is arranged on the slip ring 422; the driver 423 is engaged with the second gear 425 on the side wall of the slip ring 422 through the first gear 424 to drive the slip ring 422 to rotate, so that the scraper 41 rotates along the annular temporary storage groove 11.

[0037] Specifically, the driver 423 may be a servo motor, and a first gear 424 is disposed at a driving end of the servo motor. The first gear 424 meshes with a second gear 425 on a side wall of the slip ring 422 , thereby driving the slip ring 422 to rotate.

[0038] In some embodiments, a drain port 12 communicating with the crystallization barrel 1 is provided at the bottom of the annular temporary storage tank 11 ; a filter membrane is provided in the drain port 12 .

[0039] Specifically, the oxytetracycline hydrochloride crystals accumulated on the annular temporary storage tank 11 will carry the mixed solution, and the mixed solution will gradually accumulate to the bottom of the annular temporary storage tank 11, and then be discharged from the drain port 12 at the bottom of the annular temporary storage tank 11 and enter the crystallization barrel 1 again.

[0040] At least one embodiment also provides a method for synthesizing an efficient oxytetracycline hydrochloride synthesis device, which comprises the following steps: step S1, adding methanol, anhydrous calcium chloride, oxytetracycline powder and activated carbon into a container in sequence, and stirring the mixture; step S2, filtering the mixture to obtain a mixed solution; step S3, adding hydrogen chloride solution to the mixed solution in the crystallization barrel for cooling and crystallization; step S4, scraping the crystals on the inner wall of the crystallization barrel out of the crystallization barrel through a cleaning ring, and spreading the scraped crystals into an annular temporary storage tank at the barrel mouth through a collecting mechanism; step S5, crushing and packaging the crystals.

[0041] In some embodiments, the bottom of the annular temporary storage groove 11 is inclined; the upper surface of the cleaning ring 3 is inclined, and its inclination slope is the same as the bottom of the annular temporary storage groove 11; the lower surface of the scraper 41 is inclined, and its inclination slope is the same as the bottom of the annular temporary storage groove 11.

[0042] In some embodiments, one end of the scraper 41 extends out of the annular temporary storage groove 11, and the scraper 41 is tilted toward the rotation direction.

[0043] In summary, the oxytetracycline hydrochloride efficient synthesis equipment and synthesis method thereof scrape the oxytetracycline hydrochloride crystals on the inner wall of the crystallization barrel 1 out of the crystallization barrel 1 through the cleaning ring 3 to prevent the crystallization from affecting the temperature conduction; at the same time, the oxytetracycline hydrochloride crystals scraped out of the crystallization barrel 1 are collected by the collecting mechanism 4 and spread flat at the barrel mouth of the crystallization barrel 1, so that the mixed solution deposited at the bottom of the annular temporary storage tank 11 enters the crystallization barrel 1 again for crystallization formation cycle.

[0044] Herein, when it is mentioned that a first component is located on a second component, this may mean that the first component may be directly formed on the second component, or a third component may be interposed between the first component and the second component.

[0045] In this article, when an element or layer is referred to as being "located on," "engaged to," "connected to," "attached to," or "coupled to" another element or layer, it may be directly located on, engaged, connected, attached to, or coupled to another element or layer, or there may be intermediate elements or layers. In contrast, when an element is referred to as being "directly on," "directly engaged to," "directly connected to," "directly attached to," or "directly coupled to" another element or layer, there may be no intermediate elements or layers. Other words used to describe the relationship between elements should be interpreted in a similar manner (e.g., "between" versus "directly between," "adjacent" versus "directly adjacent," etc.). As used herein, the term "and / or" includes any and all combinations of one or more of the associated listed items.

[0046] Herein, example embodiments of the present disclosure will be described in more detail with reference to the accompanying drawings. As used herein, expressions such as "at least one of..." modify the entire list of elements when following a list of elements, rather than modifying individual elements in the list. For example, the expression "at least one of a, b, and c" should be understood to include only a, only b, only c, both a and b, both a and c, both b and c, or all of a, b, and c.

[0047] The terms used herein are only used to describe specific exemplary configurations and are not intended to be limited. As used herein, the singular articles "one", "an" and "the" may also be intended to include plural forms, unless it is clearly indicated above that this is not the case. The terms "comprise", "include" and "have" are inclusive, and therefore specify the presence of features, steps, operations, elements and / or components, but do not exclude the presence or addition of one or more other features, steps, operations, elements, components and / or combinations thereof. The method steps, processes and operations described herein should not be interpreted as necessarily requiring them to be performed in the specific order discussed or shown, unless specifically identified as an execution order. Additional or alternative steps may be adopted.

[0048] As used herein, the phrases "in one embodiment," "according to one embodiment," "in some embodiments," and the like generally refer to the fact that the particular feature, structure, or characteristic following the phrase may be included in at least one embodiment of the present disclosure. Therefore, a particular feature, structure, or characteristic may be included in more than one embodiment of the present disclosure, so that these phrases do not necessarily refer to the same embodiment. As used herein, the terms "example," "exemplary," and the like are used to "serve as an example, instance, or illustration." Any implementation, aspect, or design described herein as "example" or "exemplary" is not necessarily to be construed as preferred or superior to other implementations, aspects, or designs. On the contrary, the use of the terms "example," "exemplary," and the like is intended to present concepts in a concrete manner.

[0049] In the description of the embodiments of the present invention, unless otherwise clearly specified and limited, the terms "installed", "connected", and "connected" 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 or an electrical connection; it can be a direct connection or an indirect connection through an intermediate medium, or it can be the internal communication of two components. For ordinary technicians in this field, the specific meanings of the above terms in the present invention can be understood according to specific circumstances.

[0050] In the description of the present invention, it should be noted that the orientation or positional relationship indicated by the terms "center", "upper", "lower", "left", "right", "vertical", "horizontal", "inside", "outside", etc. is based on the orientation or positional relationship shown in the drawings, which is only for the convenience of describing the present invention and simplifying the description, rather than indicating or implying that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and therefore cannot be understood as a limitation of the present invention. In addition, terms such as "first", "second" and other numerical terms do not imply an order or sequence when used in this document unless explicitly indicated above. Therefore, without departing from the teachings of the example embodiments, the first element, component, region, layer or section discussed above may be referred to as a second element, component, region, layer or section.

[0051] Spatially relative terms, such as "inside", "outside", "below", "below", "down", "above", "on", etc., may be used herein to facilitate description of the relationship of one element or feature to another element or feature as illustrated in the figure. In addition to the orientation depicted in the figure, spatially relative terms may be intended to cover different orientations of the device in use or operation. For example, if the device in the figure is turned over, the elements described as "below" or "below" other elements or features will be oriented to be "above" other elements or features. Therefore, the example term "below" can cover the orientation above and below. The device can be oriented in other ways (rotated 90 degrees or in other orientations), and the spatially relative descriptors used herein are interpreted accordingly.

[0052] In the above discussion, unless otherwise stated, the terms "about," "approximately," "substantially," etc., when used to describe a numerical value, mean a variation of + / - 10% of the value.

[0053] Based on the above ideal embodiments of the present invention, the relevant staff can make various changes and modifications without departing from the technical concept of the present invention through the above description. The technical scope of the present invention is not limited to the contents of the specification, and its technical scope must be determined according to the scope of the claims.

Claims

1. An efficient synthesis device for oxytetracycline hydrochloride, characterized in that: include: A crystallization barrel (1) is used to hold the mixed solution and crystallize it by cooling; A cleaning ring (3) is fitted with the inner wall of the crystallization barrel (1) and is driven by a cylinder to move up and down so as to scrape the crystals on the inner wall of the crystallization barrel (1) out of the crystallization barrel (1); and The collecting mechanism (4) rotates around the crystallization barrel (1) to receive the crystals brought out by the cleaning ring (3), and spreads the received crystals flat at the barrel mouth of the crystallization barrel (1).

2. The high-efficiency oxytetracycline hydrochloride synthesis equipment according to claim 1, characterized in that: An annular temporary storage groove (11) is provided at the barrel opening of the crystallization barrel (1); The collecting mechanism (4) rotates along the annular temporary storage groove (11) to scrape the crystals on the cleaning ring (3) onto the annular temporary storage groove (11) and spread them flat.

3. The high-efficiency synthesis equipment of oxytetracycline hydrochloride according to claim 2, characterized in that: The collecting mechanism (4) comprises: a scraper (41) and a driving assembly (42); The bottom of the annular temporary storage groove (11) is arranged to be inclined; The upper surface of the cleaning ring (3) is arranged to be inclined, and its inclination slope is the same as the bottom of the annular temporary storage groove (11); The lower surface of the scraper (41) is arranged to be inclined, and its inclination slope is the same as the bottom of the annular temporary storage groove (11); When the cleaning ring (3) extends out of the crystallization barrel (1), the drive assembly (42) drives the scraper (41) to rotate along the annular temporary storage groove (11) to scrape the crystals on the cleaning ring (3) to the annular temporary storage groove (11) and spread them flat.

4. The high-efficiency synthesis equipment of oxytetracycline hydrochloride according to claim 3, characterized in that: One end of the scraper (41) extends out of the annular temporary storage groove (11), and the scraper (41) is inclined in the direction of rotation so as to facilitate scraping the crystals on the cleaning ring (3) to the annular temporary storage groove (11).

5. The high-efficiency synthesis equipment of oxytetracycline hydrochloride according to claim 4, characterized in that: The driving assembly (42) comprises: an annular guide rail (421), a slip ring (422) and a driver (423); The annular guide rail (421) is arranged on the side wall of the crystallization barrel (1), the slip ring (422) is arranged on the annular guide rail (421), and the scraper (41) is arranged on the slip ring (422); The driver (423) meshes with a second gear (425) on the side wall of the slip ring (422) via a first gear (424) to drive the slip ring (422) to rotate, thereby causing the scraper (41) to rotate along the annular temporary storage groove (11).

6. The high-efficiency synthesis equipment of oxytetracycline hydrochloride according to claim 5, characterized in that: The bottom of the annular temporary storage tank (11) is provided with a liquid discharge port (12) which is connected to the crystallization barrel (1); A filter membrane is arranged in the liquid discharge port (12).

7. The high-efficiency synthesis equipment of oxytetracycline hydrochloride according to claim 6, characterized in that: The rising height of the cleaning ring (3) increases gradually.

8. A synthesis method using the oxytetracycline hydrochloride high-efficiency synthesis equipment according to claim 1, characterized in that: The steps include: Step S1, adding methanol, anhydrous calcium chloride, oxytetracycline powder and activated carbon into a container in sequence, and stirring the mixture; Step S2, filtering the mixture to obtain a mixed solution; Step S3, adding hydrogen chloride solution to the mixed solution in the crystallization barrel for cooling and crystallization; Step S4, scraping the crystals on the inner wall of the crystallization barrel out of the crystallization barrel by a cleaning ring, and spreading the scraped crystals into an annular temporary storage tank at the barrel mouth by a collecting mechanism; Step S5, crushing and packaging the crystals.

9. The synthesis method of the oxytetracycline hydrochloride efficient synthesis equipment according to claim 8, characterized in that: The bottom of the annular temporary storage groove (11) is arranged to be inclined; The upper surface of the cleaning ring (3) is arranged to be inclined, and its inclination slope is the same as the bottom of the annular temporary storage groove (11); The lower surface of the scraper (41) is arranged to be inclined, and its inclination slope is the same as the bottom of the annular temporary storage groove (11).

10. The synthesis method of the oxytetracycline hydrochloride efficient synthesis equipment according to claim 9, characterized in that: One end of the scraper (41) extends out of the annular temporary storage groove (11), and the scraper (41) is arranged to be inclined toward the rotation direction.

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