Concentrated solution freezing crystallizer for salifying preparation of erythromycin oxime

Abstract

The invention discloses a concentrated solution freezing crystallization machine for salifying preparation of erythromycin oxime, and relates to the technical field of salifying preparation of erythromycin oxime, the concentrated solution freezing crystallization machine comprises a rack, a supporting plate is fixedly connected to the position, close to the edge, of the bottom of the rack, and a guide sliding groove is formed in the lower position of the surface of the supporting plate; and the top of the rack is fixedly connected with a hoist. According to the concentrated solution freezing crystallizer for salifying preparation of erythromycin oxime, a cavity is formed in the position between the temperature adjusting assembly and the temperature slowing assembly, heating water is introduced into the cavity, erythromycin oxime salt is evaporated and concentrated through water bath heating, then hot water is discharged to enable the temperature of a concentrated solution to reach a metastable area, and the interior of the temperature slowing assembly is slowly cooled; the erythromycin oxime crystals are separated out, the electric rotary table drives the magnetic sliding block to rotate, the temperature slowing assembly scrapes off the adhered crystals, and the problems that the heat transfer performance is deteriorated and the yield of the erythromycin oxime is low due to the fact that crystal scales are very easy to crystallize between a cooled solution and a heat transfer surface are solved.

Description

Technical Field

[0001] The invention relates to the technical field of erythromycin oxime salt preparation, in particular to a concentrated liquid freezing crystallizer for erythromycin oxime salt preparation. Background Art

[0002] Erythromycin oxime is a white crystalline powder, which is easily soluble in organic solvents such as methanol and dichloromethane. In order to overcome the disadvantage of erythromycin being unstable under acidic conditions, a second-generation novel erythromycin derivative has been developed. In the current synthesis process, erythromycin oxime salt is generally synthesized first, filtered and then neutralized with alkali to obtain erythromycin oxime. When filtering erythromycin oxime salt, part of erythromycin oxime salt remains in the mother liquor, resulting in a low overall yield of erythromycin oxime. On the other hand, when synthesizing erythromycin oxime, organic bases such as triethylamine and pyridine are used. Triethylamine and the reaction solvent methanol are azeotropic and difficult to recover. Alternatively, inorganic bases such as sodium hydroxide are used to neutralize with hydroxylamine hydrochloride to generate water, which affects the reaction and results in poor product quality. Recrystallization is required to meet the requirements of the next step of production. The Chinese patent announcement number is: CN103537115A discloses "A crystallization cooler and method for extending the operating cycle of an external circulation crystallizer". In this patent, heat exchange is carried out through vaporization and condensation of the working fluid. The working temperature of the working fluid can be controlled to reduce the temperature difference between the inside and outside of the crystallization cooler, eliminate scaling, and extend the operating cycle of the crystallizer. Since the working fluid transfers heat through vaporization and condensation, the heat transfer coefficient is large and the heat exchange area can be reduced.

[0003] The existing concentrated liquid freezing crystallizer for preparing erythromycin oxime salt has structural design defects. When erythromycin oxime is prepared into salt, the particle size of the product crystals is too fine, resulting in poor solid-liquid separation effect of the crystallization liquid, and scale is very easy to form between the cooled solution and the heat transfer surface, which not only deteriorates the heat transfer performance but also leads to a low yield of erythromycin oxime. Summary of the invention

[0004] The invention provides a concentrated liquid freezing crystallizer for preparing erythromycin oxime salt, which solves the problems mentioned in the above background technology.

[0005] To achieve the above objectives, the present invention is implemented by the following technical solutions: a concentrated liquid freezing crystallizer prepared by erythromycin oxime salt formation, comprising a frame, a support plate is fixedly connected to the bottom of the frame near the edge, a guide slide is provided below the surface of the support plate, a hoist is fixedly connected to the top of the frame, a screw is connected to the inner side of the hoist through a thread, and further comprising:

[0006] A concentrating mechanism, which is fixedly mounted above the surface of the support plate and is used for heating and concentrating the erythromycin oxime salt solution and scraping the erythromycin oxime crystals adhered to the inner wall;

[0007] A cooling mechanism, wherein the cooling mechanism is fixedly mounted at the bottom end of the screw, the inner side of the cooling mechanism is slidably connected to the surface of the frame, and the cooling mechanism is used for cooling and crystallizing erythromycin oxime;

[0008] The concentrating mechanism comprises a motor, the output end of the motor is fixedly connected to a temperature control component, an electric turntable is fixedly connected to the upper position of the surface of the temperature control component, the output end of the electric turntable is fixedly connected to a connector, a magnetic slider is fixedly connected to the surface of the connector, and a temperature relief component is fixedly connected to the inner side of the temperature control component.

[0009] Preferably, the motor is fixedly mounted above the surface of the support plate, and the concentrating mechanism further comprises a feed pipe, which is fixedly mounted in the middle of the surface of the temperature regulating component.

[0010] Preferably, the temperature regulating component comprises a shell, the shell is fixedly mounted on the output end of the motor, a connecting rod is fixedly connected to the upper position of the inner side of the shell, the oximation of erythromycin A is completely carried out at a certain temperature for a certain period of time, then the temperature is lowered to room temperature and water is added to fully precipitate the oxime salt and dissolve the inorganic salt, etc., the oxime salt is filtered to obtain the oxime salt, and then a polar solvent such as methanol and ethanol is added, and liquid alkali is added to dissolve the oxime salt, water is added dropwise to cool and crystallize the erythromycin oxime, and the erythromycin oxime is dried after centrifugal filtration to obtain erythromycin oxime. In the process of preparing the erythromycin oxime salt, the erythromycin oxime salt is transported to the interior of the temperature regulating component by a feed pipe.

[0011] Preferably, the temperature control component also includes a discharge shell, which is fixedly installed at an upper position of the outer surface of the outer shell, the inner side surface of the outer shell is fixedly connected to a first spiral tube, the bottom end of the first spiral tube is fixedly connected to a first U-shaped tube, the magnetic slider and the slide cylinder are both magnetic and attract each other, the slide cylinder is driven by the magnetic force to slide inside the circular guide rail, the interior of the embedded wall is transported with erythromycin oxime salt solution, the pipe fitting for transporting heated liquid is fixedly installed at the bottom of the outer shell, the rotating axis of the pipe fitting coincides with the axis of the motor, the guide groove is used to guide the rotation of the pipe fitting, and during concentration, the pipe fitting passes heated water into the interior of the cavity, and the water bath heating method allows the liquid to be quickly concentrated.

[0012] Preferably, the temperature-reducing component comprises an embedded wall, the upper position of the outer surface of the embedded wall is fixedly mounted on the end surface of the connecting rod, and the upper position of the inner side surface of the embedded wall is fixedly connected with a circular guide rail.

[0013] Preferably, the temperature-reducing component also includes a sliding cylinder, which is slidably mounted on the inner side of the circular guide rail, and the bottom of the sliding cylinder is fixedly connected to a U-shaped frame bar, and the inner side of the U-shaped frame bar is fixedly connected to a perforated plate. The connection of the connector converts the rotation of the electric turntable into a circular rotation of the magnetic slider, and a cavity is provided between the temperature regulating component and the temperature-reducing component, and a cavity is also provided inside the speed increasing component. After the erythromycin oxime salt solution is concentrated on the inner side of the temperature-reducing component, the erythromycin oxime salt solution is rapidly cooled to a metastable zone. During the process, the temperature-reducing component stirs the erythromycin oxime salt solution. When the solution reaches the metastable zone, the opening and closing machine drives the screw to move downward, and the lifting platform is driven to move up and down by the fixed cylinder.

[0014] Preferably, the cooling mechanism comprises a fixed cylinder, the top of which is fixedly mounted on the bottom end of the screw rod, the outer surface of which is rotatably connected to a lifting platform, and the lifting platform is slidably mounted on the outer surface of the frame.

[0015] Preferably, the cooling mechanism further comprises an extension wall, the top end of the extension wall is fixedly mounted on the lower surface of the lifting platform, the bottom end of the extension wall is fixedly connected with a speed increasing component, and the top of the speed increasing component is fixedly connected with a connecting component.

[0016] Preferably, the speed increasing component comprises a fixed wall, the outer surface of which is fixedly connected to a second spiral tube, the bottom end of which is fixedly connected to a second U-shaped tube, the downward movement of the fixed wall causes the liquid level of the erythromycin oxime salt solution to be raised upward, at which time the erythromycin oxime salt solution is in a metastable zone, a liquid at a relatively low temperature is introduced into the interior of the second spiral tube, and the temperature difference between the solution and the cooling gas can be adjusted by adjusting the temperature of the liquid, thereby avoiding the problem of finer crystal particles caused by a large temperature difference, the second spiral tube is not in direct contact with the fixed wall, and therefore, the gas between the fixed wall and the outer embedded wall is indirectly cooled.

[0017] Preferably, the speed increasing assembly further comprises an opening ring, a surface of which is provided with a plurality of through holes, a bottom of which is fixedly mounted on the top of the fixed wall, and a bottom of which is fixedly connected to an outer embedded wall.

[0018] Preferably, the connecting component includes a connecting shell, the bottom of which is fixedly mounted on the top of the perforated ring, and the top of the connecting shell is fixedly connected with a T-section ring. There are two half shells. During installation, the T-section ring is embedded into the inner side of the connecting shell. Subsequently, the two half shells are welded together. When the fixed wall is driven to move downward, the rubber ring is in close contact with the top of the embedded wall, so that a cavity is formed between the outer shell, the embedded wall, the fixed wall and the outer embedded wall, and the fan drives the gas to circulate inside the cavity.

[0019] Preferably, the connecting component also includes a fan, which is fixedly mounted on the surface of the T-section ring. There are multiple fans, a half shell is fixedly connected to the upper position of the T-section ring surface, and a rubber ring is fixedly connected to the bottom of the half shell.

[0020] The present invention provides a concentrated liquid freezing crystallizer for preparing erythromycin oxime salt. It has the following beneficial effects:

[0021] 1. The concentrated liquid freezing crystallizer prepared by erythromycin oxime salt formation has a cavity formed between the temperature regulating component and the slow-temperature component, and heated water is introduced into the cavity. The erythromycin oxime salt is evaporated and concentrated by water bath heating, and then the hot water is discharged to make the temperature of the concentrated liquid reach the metastable zone. The temperature inside the slow-temperature component is slowly cooled, and erythromycin oxime crystals are precipitated. The electric turntable drives the magnetic slider to rotate, and the slow-temperature component scrapes off the adhered crystals, thereby solving the problem that the cooled solution and the heat transfer surface are very easy to crystallize and scale, which not only leads to the deterioration of the heat transfer performance but also leads to a low yield of erythromycin oxime.

[0022] 2. In the concentrated liquid freezing crystallizer prepared by erythromycin oxime salt formation, the sliding cylinder rotates under the attraction of magnetism, and the perforated plate stirs the erythromycin oxime salt solution, so that the erythromycin oxime salt solution is quickly concentrated, and the heated water is quickly discharged. When the solution is quickly cooled to a temperature close to the metastable zone, the cooling water is transported to the cavity, so that the erythromycin oxime salt solution can quickly reach the metastable zone, and the unsaturation of the solution is increased. In this process, the rotating perforated plate improves the efficiency of concentration and cooling, and avoids premature crystallization due to local low temperature.

[0023] 3. The concentrated liquid freezing crystallizer for preparing erythromycin oxime salt has an extended wall to firmly support the speed-increasing component, and the speed-increasing component is driven down to fit closely with the inner side of the slow-temperature component. At this time, the speed-increasing component, the temperature-adjusting component and the interior of the slow-temperature component are connected, and the introduction of cooling water causes the gas in the connected space to be cooled down. The solution is cooled and crystallized in a slow-temperature manner, which solves the problem of poor solid-liquid separation effect of the crystallization liquid due to the fine particle size of the product crystals when preparing erythromycin oxime salt.

[0024] 4. In the freeze crystallizer for concentrated solution prepared by erythromycin oxime salt formation, the temperature of the outer embedded wall is slowly and evenly lowered to the crystallization temperature. During the process, the erythromycin oxime salt solution is in a static state, and the distance between the solution and the outer embedded wall is uniform. The local supersaturation of the solution is stable and uniform when crystallizing. The temperature-reducing component is in a static state or a slowly rotating state, so that the temperature drops slowly when the erythromycin oxime crystals are precipitated. However, due to the large contact area of ​​the erythromycin oxime solution for cooling, the efficiency of the erythromycin oxime crystallization is rapidly increased, and at the same time, the precipitated crystal particles are not too small to be difficult to separate.

[0025] 5. In the concentrated liquid freezing crystallizer for preparing erythromycin oxime salt, the position between the outer embedded wall and the inner embedded wall forms a solution cooling crystallization zone, the solution in this zone is slowly cooled down, and due to the temperature difference, the solution preferentially adheres to the surface of the outer embedded wall and the inner embedded wall for crystallization, and the solution crystal particles are relatively large in the undisturbed and crystallized state. After the crystallization is completed, the U-shaped frame bar is driven to rotate, and the U-shaped frame bar is tightly fitted with the surface of the outer embedded wall and the inner embedded wall, thereby scraping off the large crystal particles attached to the outer embedded wall and the inner embedded wall, and the solution and the particles are discharged along the discharge shell, so that the product rate of erythromycin oxime salt preparation is higher. BRIEF DESCRIPTION OF THE DRAWINGS

[0026] Figure 1 A first overall stereogram of a concentrated liquid freezing crystallizer for preparing erythromycin oxime salt of the present invention;

[0027] Figure 2 A second overall stereogram of the concentrated liquid freezing crystallizer for preparing the erythromycin oxime salt of the present invention;

[0028] Figure 3 It is a schematic diagram of the overall structure of the concentration mechanism of the present invention;

[0029] Figure 4 It is a schematic diagram of the structure of a part of the concentration mechanism of the present invention;

[0030] Figure 5 It is a structural schematic diagram of the temperature control component of the present invention;

[0031] Figure 6 It is a structural schematic diagram of the temperature-reducing component of the present invention;

[0032] Figure 7 It is a structural schematic diagram of the cooling mechanism of the present invention;

[0033] Figure 8 It is a structural schematic diagram of the speed increasing assembly of the present invention;

[0034] Fig. 9 It is a schematic diagram of the structure of the connection component of the present invention.

[0035] In the figure: 1, frame; 2, support plate; 3, guide slide; 4, hoist; 5, screw; 6, concentration mechanism; 61, motor; 62, temperature adjustment component; 621, shell; 622, connecting rod; 623, discharge shell; 624, first spiral tube; 625, first U-shaped tube; 63, feed tube; 64, electric turntable; 65, connector; 66, magnetic slider; 67, temperature slowing component: 671, embedded wall; 672, circular guide rail; 67 3. Sliding cylinder; 674. U-shaped frame strip; 675. Perforated plate; 7. Cooling mechanism; 71. Fixed cylinder; 72. Lifting platform; 73. Extension wall; 74. Speed ​​increasing assembly; 741. Fixed wall; 742. Second spiral tube; 743. Second U-shaped tube; 744. Perforated ring; 745. External embedded wall; 75. Connecting assembly; 751. Connecting shell; 752. T-section ring; 753. Fan; 754. Half shell; 755. Rubber ring. DETAILED DESCRIPTION

[0036] 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.

[0037] First embodiment: Figure 1-Figure 4 As shown, the present invention provides a technical solution: a concentrated liquid freezing crystallizer prepared by erythromycin oxime salt formation, comprising a frame 1, a support plate 2 is fixedly connected to the bottom of the frame 1 near the edge, a guide slide 3 is provided below the surface of the support plate 2, a hoist 4 is fixedly connected to the top of the frame 1, and a screw 5 is threadedly connected to the inner side of the hoist 4, and further comprising:

[0038] A concentrating mechanism 6, which is fixedly mounted above the surface of the support plate 2, and is used for heating and concentrating the erythromycin oxime salt solution and scraping the erythromycin oxime crystals adhered to the inner wall;

[0039] A cooling mechanism 7, which is fixedly mounted at the bottom end of the screw 5, and whose inner side surface is slidably connected to the surface of the frame 1, and is used for cooling and crystallizing erythromycin oxime;

[0040] The concentrating mechanism 6 includes a motor 61, the output end of the motor 61 is fixedly connected to a temperature regulating component 62, the upper position of the surface of the temperature regulating component 62 is fixedly connected to an electric turntable 64, the output end of the electric turntable 64 is fixedly connected to a connector 65, the surface of the connector 65 is fixedly connected to a magnetic slider 66, and the inner side of the temperature regulating component 62 is fixedly connected to a temperature slowing component 67;

[0041] The motor 61 is fixedly mounted on the upper portion of the surface of the support plate 2 . The concentrating mechanism 6 further comprises a feed pipe 63 . The feed pipe 63 is fixedly mounted on the middle portion of the surface of the temperature regulating component 62 .

[0042] When in use, the oximation of erythromycin A is completed at a certain temperature for a certain period of time, then the temperature is lowered to room temperature, water is added to fully precipitate the oxime salt and dissolve the inorganic salt, etc., the oxime salt is filtered, and then a polar solvent such as methanol or ethanol is added, and liquid alkali is added to dissolve the oxime salt, and water is added dropwise to cool and crystallize the erythromycin oxime, and the erythromycin oxime is dried after centrifugal filtration. In the process of preparing the erythromycin oxime salt, the erythromycin oxime salt is transported to the interior of the temperature regulating component 62 by the feed pipe 63, and the temperature regulating component 62 and the slow temperature component 6 A cavity is formed between 7, and heated water is introduced into the cavity. The erythromycin oxime salt is evaporated and concentrated by water bath heating, and then the hot water is discharged to make the temperature of the concentrated solution reach the metastable zone. The interior of the slow-temperature component 67 is slowly cooled down, and erythromycin oxime crystals are precipitated. The electric turntable 64 drives the magnetic slider 66 to rotate, and the slow-temperature component 67 scrapes off the adhered crystals, thereby solving the problem that scale is very easy to crystallize between the cooled solution and the heat transfer surface, which not only leads to deterioration of the heat transfer performance but also leads to a low yield of erythromycin oxime.

[0043] Second embodiment: Figure 3-Figure 6 As shown, the temperature control component 62 includes a shell 621, which is fixedly mounted on the output end of the motor 61, and a connecting rod 622 is fixedly connected to the upper position of the inner side of the shell 621. The temperature control component 62 also includes a discharge shell 623, which is fixedly mounted on the upper position of the outer surface of the shell 621, and a first spiral tube 624 is fixedly connected to the inner side of the shell 621, and a first U-shaped tube 625 is fixedly connected to the bottom end of the first spiral tube 624;

[0044] The temperature-reducing component 67 includes an embedded wall 671, the upper position of the outer surface of the embedded wall 671 is fixedly installed on the end face of the connecting rod 622, and the upper position of the inner side surface of the embedded wall 671 is fixedly connected to a circular guide rail 672. The temperature-reducing component 67 also includes a sliding cylinder 673, which is slidably installed on the inner side surface of the circular guide rail 672, and the bottom of the sliding cylinder 673 is fixedly connected to a U-shaped frame bar 674, and the inner side surface of the U-shaped frame bar 674 is fixedly connected to a perforated plate 675.

[0045] When in use, the magnetic slider 66 and the slide cylinder 673 are both magnetic and attract each other. The slide cylinder 673 is driven by the magnetic force to slide inside the circular guide rail 672, and the erythromycin oxime salt solution is transported inside the embedded wall 671. The pipe for transporting the heated liquid is fixedly installed at the bottom of the shell 621. The rotating axis of the pipe coincides with the axis of the motor 61. The guide groove 3 is used to guide the rotation of the pipe. During concentration, the pipe introduces heated water into the cavity, and the liquid is quickly concentrated by water bath heating. The slide cylinder 673 rotates under the attraction of magnetism, and the perforated plate 675 stirs the erythromycin oxime salt solution, so that the erythromycin oxime salt solution is quickly concentrated. The heated water is quickly discharged. When the solution is quickly cooled to near the metastable zone, cooling water is transported to the cavity, so that the erythromycin oxime salt solution can quickly reach the metastable zone, and the unsaturation of the solution increases. In this process, the rotating perforated plate 675 improves the efficiency of concentration and cooling, and avoids local low temperature and premature crystallization.

[0046] The third embodiment: Figure 3 , Figure 7 As shown, the output end of the motor 61 is fixedly connected to a temperature adjustment component 62, the upper position of the surface of the temperature adjustment component 62 is fixedly connected to an electric turntable 64, the output end of the electric turntable 64 is fixedly connected to a connector 65, the surface of the connector 65 is fixedly connected to a magnetic slider 66, and the inner side of the temperature adjustment component 62 is fixedly connected to a temperature-slowing component 67;

[0047] The motor 61 is fixedly mounted on the upper surface of the support plate 2. The concentrating mechanism 6 further comprises a feed pipe 63, which is fixedly mounted on the middle portion of the surface of the temperature regulating component 62.

[0048] The cooling mechanism 7 includes a fixed cylinder 71, the top of which is fixedly mounted on the bottom end of the screw 5, the outer surface of the fixed cylinder 71 is rotatably connected to a lifting platform 72, the lifting platform 72 is slidably mounted on the outer surface of the frame 1, the cooling mechanism 7 also includes an extension wall 73, the top of the extension wall 73 is fixedly mounted on the lower surface of the lifting platform 72, the bottom end of the extension wall 73 is fixedly connected to a speed increasing component 74, and the top of the speed increasing component 74 is fixedly connected to a connecting component 75.

[0049] When in use, the connection of the connector 65 converts the rotation of the electric turntable 64 into the circular rotation of the magnetic slider 66. A cavity is provided between the temperature regulating component 62 and the slow-temperature component 67, and a cavity is also provided inside the speed increasing component 74. After the erythromycin oxime salt solution is concentrated on the inner side of the slow-temperature component 67, the erythromycin oxime salt solution is rapidly cooled to the metastable zone. During this process, the slow-temperature component 67 stirs the erythromycin oxime salt solution. When the solution reaches the metastable zone, the hoist 4 drives the screw 5 to move downward in a spiral, and the lifting platform 72 is driven by the fixed cylinder 71 to move up and down, and the extended wall 73 firmly supports the speed increasing component 74. The speed increasing component 74 is driven to descend and fits tightly with the inner side of the temperature reducing component 67. At this time, the interiors of the speed increasing component 74, the temperature regulating component 62 and the temperature reducing component 67 are connected. The introduction of cooling water causes the gas in the connected space to be cooled down, and the solution is cooled and crystallized in a slow temperature manner, which solves the problem of poor solid-liquid separation effect of the crystallization liquid due to the fine particle size of the product crystals during the salt preparation of erythromycin oxime.

[0050] Fourth embodiment: Figure 7-Figure 9 As shown, the speed increasing assembly 74 includes a fixed wall 741, the outer surface of the fixed wall 741 is fixedly connected to a second spiral tube 742, the bottom end of the second spiral tube 742 is fixedly connected to a second U-shaped tube 743, and the speed increasing assembly 74 also includes an opening ring 744, the surface of the opening ring 744 is provided with a plurality of through holes, the bottom of the opening ring 744 is fixedly mounted on the top of the fixed wall 741, and the bottom of the opening ring 744 is fixedly connected to an outer embedded wall 745;

[0051] The connecting component 75 includes a connecting shell 751, the bottom of which is fixedly mounted on the top of the opening ring 744, and the top of the connecting shell 751 is fixedly connected to a T-shaped cross-section ring 752. The connecting component 75 also includes a fan 753, which is fixedly mounted on the surface of the T-shaped cross-section ring 752. There are multiple fans 753, and a half shell 754 is fixedly connected to the upper position of the surface of the T-shaped cross-section ring 752, and a rubber ring 755 is fixedly connected to the bottom of the half shell 754.

[0052] When in use, the downward movement of the fixed wall 741 causes the liquid level of the erythromycin oxime salt solution to be raised upward. At this time, the erythromycin oxime salt solution is in a metastable zone. A liquid at a relatively low temperature is introduced into the interior of the second spiral tube 742. The temperature of the liquid can be adjusted to adjust the temperature difference between the solution and the cooling gas, thereby avoiding the problem of finer crystal particles caused by a large temperature difference. The second spiral tube 742 is not in direct contact with the fixed wall 741, so the gas between the fixed wall 741 and the outer embedded wall 745 is indirectly cooled, and the temperature of the outer embedded wall 745 is slowly and evenly reduced to the crystallization temperature. During this process, the erythromycin oxime salt solution is in a static state, and the distance between the solution and the outer embedded wall 745 is uniform. The local supersaturation of the solution is stable and uniform when crystallizing. The temperature-reducing component 67 is in a static state or a slowly rotating state, so that the temperature is slowly reduced when the erythromycin oxime crystals are precipitated. However, due to the large cooling contact area of ​​the erythromycin oxime solution, the efficiency of the erythromycin oxime crystallization is rapidly increased, and at the same time, the precipitated crystal particles are not too small to be difficult to separate.

[0053] Fifth embodiment: Figure 6 , Figure 8 As shown, the upper position of the outer surface of the embedded wall 671 is fixedly installed on the end surface of the connecting rod 622, and the upper position of the inner side surface of the embedded wall 671 is fixedly connected with a circular guide rail 672. The temperature-slowing component 67 also includes a sliding cylinder 673, which is slidably installed on the inner side surface of the circular guide rail 672. The bottom of the sliding cylinder 673 is fixedly connected with a U-shaped frame bar 674, and the inner side surface of the U-shaped frame bar 674 is fixedly connected with a perforated plate 675.

[0054] The outer surface of the fixed wall 741 is fixedly connected to a second spiral tube 742, and the bottom end of the second spiral tube 742 is fixedly connected to a second U-shaped tube 743. The speed increasing assembly 74 also includes an open hole ring 744, and a plurality of through holes are opened on the surface of the open hole ring 744. The bottom of the open hole ring 744 is fixedly installed on the top of the fixed wall 741, and the bottom of the open hole ring 744 is fixedly connected to an outer embedded wall 745.

[0055] When in use, there are two half shells 754. When installed, the T-section ring 752 is embedded into the inner side of the connecting shell 751. Then, the two half shells 754 are welded together. When the fixed wall 741 is driven to move downward, the rubber ring 755 is in close contact with the top of the embedded wall 671, so that a cavity is formed between the outer shell 621, the embedded wall 671, the fixed wall 741 and the outer embedded wall 745. The fan 753 drives the gas to circulate inside the cavity, and the position between the outer wall 745 and the inner wall 671 forms a solution cooling crystal. Zone, the solution in this zone is slowly cooled down, due to the temperature difference, the solution preferentially adheres to the surface of the outer embedded wall 745 and the inner embedded wall 671 for crystallization, and in the undisturbed and crystallized state, the solution crystal particles are relatively large, after the crystallization is completed, the U-shaped frame bar 674 is driven to rotate, at this time the U-shaped frame bar 674 is tightly fitted with the surface of the outer embedded wall 745 and the inner embedded wall 671, thereby scraping off the large crystal particles attached to the outer embedded wall 745 and the inner embedded wall 671, and the solution and particles are discharged along the discharge shell 623, so that the erythromycin oxime salt preparation product rate is higher.

[0056] It should be noted that, in this article, relational terms such as first and second, etc. are only used to distinguish one entity or operation from another entity or operation, and do not necessarily require or imply any such actual relationship or order between these entities or operations. Moreover, the terms "include", "comprise" or any other variants thereof are intended to cover non-exclusive inclusion, so that a process, method, article or device including a series of elements includes not only those elements, but also other elements not explicitly listed, or also includes elements inherent to such process, method, article or device. In the absence of further restrictions. The sentence "includes an element defined by... does not exclude the existence of other identical elements in the process, method, article or device including the element".

Claims

1. A concentrated liquid freeze crystallizer for preparing erythromycin oxime salt, comprising a frame (1), characterized in that: A support plate (2) is fixedly connected to the bottom of the frame (1) near the edge, a guide groove (3) is provided below the surface of the support plate (2), a gate hoist (4) is fixedly connected to the top of the frame (1), a screw rod (5) is connected to the inner side of the gate hoist (4) via a thread, and further comprises: A concentrating mechanism (6), the concentrating mechanism (6) is fixedly mounted above the surface of the support plate (2), and the concentrating mechanism (6) is used for heating and concentrating the erythromycin oxime salt solution and scraping the erythromycin oxime crystals adhered to the inner wall; A cooling mechanism (7), wherein the cooling mechanism (7) is fixedly mounted on the bottom end of the screw (5), the inner side surface of the cooling mechanism (7) is slidably connected to the surface of the frame (1), and the cooling mechanism (7) is used for cooling and crystallizing erythromycin oxime; The concentrating mechanism (6) comprises a motor (61), the output end of the motor (61) is fixedly connected to a temperature regulating component (62), an electric turntable (64) is fixedly connected above the surface of the temperature regulating component (62), the output end of the electric turntable (64) is fixedly connected to a connector (65), a magnetic slider (66) is fixedly connected to the surface of the connector (65), and a temperature-reducing component (67) is fixedly connected to the inner side surface of the temperature regulating component (62).

2. The concentrated liquid freezing crystallizer prepared by erythromycin oxime salt formation according to claim 1, characterized in that: The motor (61) is fixedly mounted above the surface of the support plate (2). The concentration mechanism (6) further comprises a feed pipe (63). The feed pipe (63) is fixedly mounted in the middle of the surface of the temperature regulating component (62).

3. A concentrated liquid freezing crystallizer for preparing erythromycin oxime salt according to claim 2, characterized in that: The temperature adjustment component (62) comprises a shell (621), the shell (621) is fixedly mounted on the output end of the motor (61), and a connecting rod (622) is fixedly connected to the upper position of the inner side surface of the shell (621).

4. The concentrated liquid freezing crystallizer prepared by erythromycin oxime salt formation according to claim 3, characterized in that: The temperature control component (62) further comprises a discharge shell (623), wherein the discharge shell (623) is fixedly mounted above the outer surface of the outer shell (621), the inner side surface of the outer shell (621) is fixedly connected to a first spiral tube (624), and the bottom end of the first spiral tube (624) is fixedly connected to a first U-shaped tube (625).

5. The concentrated liquid freezing crystallizer prepared by erythromycin oxime salt formation according to claim 4, characterized in that: The temperature-reducing component (67) comprises an embedded wall (671), the upper position of the outer surface of the embedded wall (671) is fixedly mounted on the end surface of the connecting rod (622), and the upper position of the inner side surface of the embedded wall (671) is fixedly connected to a circular guide rail (672).

6. The concentrated liquid freeze crystallizer prepared by erythromycin oxime salt formation according to claim 5, characterized in that: The temperature-reducing component (67) further comprises a sliding cylinder (673), wherein the sliding cylinder (673) is slidably mounted on the inner side of the circular guide rail (672), the bottom of the sliding cylinder (673) is fixedly connected to a U-shaped frame bar (674), and the inner side of the U-shaped frame bar (674) is fixedly connected to a perforated plate (675).

7. The concentrated liquid freeze crystallizer prepared by erythromycin oxime salt formation according to claim 1, characterized in that: The cooling mechanism (7) comprises a fixed cylinder (71), the top of which is fixedly mounted on the bottom end of the screw rod (5), the outer surface of which is rotatably connected to a lifting platform (72), and the lifting platform (72) is slidably mounted on the outer surface of the frame (1).

8. The concentrated liquid freezing crystallizer prepared by erythromycin oxime salt formation according to claim 7, characterized in that: The cooling mechanism (7) further comprises an extension wall (73), the top end of the extension wall (73) being fixedly mounted on the lower surface of the lifting platform (72), the bottom end of the extension wall (73) being fixedly connected to a speed increasing component (74), and the top of the speed increasing component (74) being fixedly connected to a connecting component (75).

9. The concentrated liquid freezing crystallizer prepared by erythromycin oxime salt formation according to claim 8, characterized in that: The speed increasing component (74) comprises a fixed wall (741), the outer surface of the fixed wall (741) is fixedly connected to a second spiral tube (742), and the bottom end of the second spiral tube (742) is fixedly connected to a second U-shaped tube (743).

10. The concentrated liquid freeze crystallizer for preparing erythromycin oxime salt according to claim 9, characterized in that: The speed increasing assembly (74) further comprises an open hole ring (744), a surface of which is provided with a plurality of through holes, the bottom of the open hole ring (744) being fixedly mounted on the top of the fixed wall (741), and the bottom of the open hole ring (744) being fixedly connected to an outer embedded wall (745).

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