A segmented temperature control type pharmaceutical intermediate crystallization kettle

CN224853829UActive Publication Date: 2026-10-16HUBEI ORGSYN CHEM CO LTD
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Patent Information

Application Number
CN202522029186.X
Authority / Receiving Office
CN · China
Patent Type
Utility models(China)
Current Assignee / Owner
Filing Date
2025-09-22
Publication Date
2026-10-16
Estimated Expiration
2035-09-22

AI Technical Summary

Technical Problem

[0003]目前,现有医药中间体结晶设备多为单段或简单分段式结构,存在以下突出问题:1.温度控制精度不足:传统设备多采用单一夹套或简单的双夹套设计,难以实现多阶段独立控温(如高温溶解、中温析晶、低温养晶的梯度温度需求),易因温度波动或局部温差过大导致晶体颗粒不均匀、杂质含量升高;2.物料混合效率低:搅拌装置多为单一类型叶片(如锚式或桨式),无法适配不同阶段物料粘度变化(如高温段高粘度、低温段易沉积),易造成局部浓度过高或过低,影响结晶均匀性;3.过程监控能力薄弱:缺乏对各段温度、压力的实时精准监测,难以及时调整工艺参数,导致结晶过程稳定性差,产品批次间一致性低;4.结构设计冗余:部分设备通过外部管道绕制实现分段控温,不仅占用空间大、能耗高,还存在冷热介质交叉污染风险

Benefits of technology

1、通过双层釜体组件形成上、中、下三个独立密闭循环腔(导热油/水冷/制冷剂循环腔),分别对应高温段、中温段、低温段的温度控制需求。各循环腔通过独立的循环介质入口与出口与外部系统连通,可精准调节各段温度,避免了传统设备因单段控温或冷热介质交叉导致的热量干扰,有效保障了结晶过程中温度梯度的稳定性,显著提升晶体纯度与晶型一致性;

✦ Generated by Eureka AI based on patent content.

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Abstract

The utility model discloses a segmented temperature control formula medical intermediate crystallization kettle, including double -deck kettle body subassembly, and the inner layer is divided into high, medium, low temperature section through annular partition, and the outer layer corresponds to form heat conduction oil / water cooling / refrigerant independent circulation cavity, and the configuration diversion body homogenization feed, three -section type stirring blade adaptation different section mixed demand, and temperature / pressure sensor real -time monitoring. Solve traditional equipment multistage temperature control inaccuracy, mix uneven, monitor the problem of deficiency, realize crystallization process temperature gradient accurate regulation and control, material high -efficient homogenization and process stability, improve medical intermediate crystallization quality and production efficiency.
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Description

Technical Field

[0001] This utility model relates to the field of pharmaceutical equipment technology, and in particular to a segmented temperature-controlled pharmaceutical intermediate crystallizing vessel. Background Technology

[0002] The crystallization process of pharmaceutical intermediates is a crucial step in drug synthesis, directly affecting the purity, crystal stability, and yield of the product. The crystallization process typically involves multiple stages, including dissolution, supersaturation precipitation, crystal growth, and crystal preservation. Each stage has significantly different requirements for temperature, mixing uniformity, and process stability. For example, the high-temperature stage requires rapid dissolution of the raw materials to promote complete reaction; the medium-temperature stage requires slow cooling to control the crystallization rate and prevent impurity encapsulation; and the low-temperature stage requires maintaining a stable supersaturation level to ensure sufficient crystal growth.

[0003] Currently, most existing pharmaceutical intermediate crystallization equipment has a single-stage or simple segmented structure, which has the following prominent problems: 1. Insufficient temperature control precision: Traditional equipment mostly adopts a single jacket or a simple double-jacket design, which makes it difficult to achieve independent temperature control in multiple stages (such as the gradient temperature requirements for high-temperature dissolution, medium-temperature crystallization, and low-temperature crystal growth). It is easy for temperature fluctuations or excessive local temperature differences to lead to uneven crystal particles and increased impurity content; 2. Low material mixing efficiency: The stirring device is mostly a single type of blade (such as anchor or paddle), which cannot adapt to the viscosity changes of materials in different stages (such as high viscosity in the high-temperature section and easy deposition in the low-temperature section). It is easy to cause local concentrations that are too high or too low, affecting the uniformity of crystallization; 3. Weak process monitoring capability: There is a lack of real-time and accurate monitoring of temperature and pressure in each stage, making it difficult to adjust process parameters in a timely manner, resulting in poor stability of the crystallization process and low consistency between product batches; 4. Redundant structural design: Some equipment achieves segmented temperature control through external pipe winding, which not only occupies a lot of space and consumes a lot of energy, but also poses a risk of cross-contamination between hot and cold media.

[0004] Therefore, there is an urgent need for a crystallization device that can achieve precise temperature control in multiple stages, improve mixing uniformity, and enhance process monitoring to meet the high requirements of pharmaceutical intermediate crystallization processes. Utility Model Content

[0005] The technical problem to be solved by this utility model is to overcome the defects of the prior art and provide a segmented temperature-controlled pharmaceutical intermediate crystallization vessel.

[0006] To solve the above-mentioned technical problems, this utility model provides the following technical solution: This utility model discloses a segmented temperature-controlled pharmaceutical intermediate crystallization vessel, comprising: a double-layer vessel assembly, vertically arranged, consisting of an inner reaction chamber and an outer insulation jacket, wherein the inner reaction chamber and the outer insulation jacket form independent and sealed circulation chambers from top to bottom; the inner reaction chamber is divided into a high-temperature section, a medium-temperature section, and a low-temperature section from top to bottom by at least two annular partitions, and each section is sealed and connected by the annular partitions; the inner layer of the high-temperature section is a high-temperature reaction chamber, and the outer layer is connected to the circulation chamber; a guide fluid is provided at the top of the high-temperature reaction chamber, and the top of the guide fluid is sealed to the main feed inlet. The system is interconnected; the inner layers of the medium-temperature section and the low-temperature section are respectively medium-temperature reaction chambers and low-temperature reaction chambers, and the outer layers are respectively connected to the corresponding circulation chambers; the bottom of the low-temperature section is provided with a discharge port, which is sealed and connected to the bottom of the low-temperature reaction chamber; the detection mechanism includes at least one temperature sensor and at least one pressure sensor, the temperature sensor being embedded in the inner wall of the high-temperature reaction chamber, the medium-temperature reaction chamber, and the low-temperature reaction chamber respectively; the pressure sensor is located on the inner side of the top of the outer layer of the high-temperature section; the stirring mechanism extends vertically through the top of the double-layer vessel assembly, is coaxially arranged with each reaction chamber, and is used to drive material mixing.

[0007] As a preferred embodiment of this utility model, the sealed circulation chamber between the outer insulation jacket and the inner reaction chamber is divided from top to bottom into: an upper heat-conducting oil circulation chamber, a middle water-cooling circulation chamber, and a lower refrigerant circulation chamber; wherein: the outer layer of the high-temperature section is connected to the heat-conducting oil circulation chamber; the outer layer of the medium-temperature section is connected to the water-cooling circulation chamber; and the outer layer of the low-temperature section is connected to the refrigerant circulation chamber; the top of the heat-conducting oil circulation chamber, the water-cooling circulation chamber, and the refrigerant circulation chamber are respectively provided with circulation medium inlets, and the bottom of each is respectively provided with circulation medium outlets, all of which are connected to the external circulation system of the double-layer reactor assembly; the circulation chambers are not interconnected.

[0008] As a preferred technical solution of this utility model, the guide fluid includes: an annular flow divider, the top of which is sealed and connected to the bottom of the main feed inlet; an inverted conical flow guide hood, the top of which is fixedly connected to the bottom of the annular flow divider; a porous sieve plate, which is inclinedly arranged below the inverted conical flow guide hood; and an umbrella-shaped flow divider plate, the top of which is fixedly connected to the bottom of the porous sieve plate, and the bottom of which is spaced apart from the inner wall of the bottom of the inner reaction chamber.

[0009] As a preferred embodiment of this utility model, the stirring mechanism includes: a three-section stirring shaft, consisting of a first shaft section, a second shaft section, and a third shaft section coaxially arranged from top to bottom; an explosion-proof drive motor, fixed to the top outer side of the high-temperature section, with its output shaft connected to the top of the three-section stirring shaft; anchor-type stirring blades, fixed to the outer periphery of the first shaft section and located inside the high-temperature reaction chamber; turbine stirring blades, fixed to the outer periphery of the second shaft section and located inside the medium-temperature reaction chamber; spiral stirring blades, fixed to the outer periphery of the third shaft section and located inside the low-temperature reaction chamber; and a mechanical seal assembly, disposed at the penetration point between the top of the double-layer vessel assembly and the three-section stirring shaft, to achieve dynamic sealing.

[0010] As a preferred embodiment of this utility model, the temperature sensor is a platinum resistance sensor, which is respectively disposed at 1 / 2 of the height of the inner wall of the high-temperature reaction chamber, the medium-temperature reaction chamber, and the low-temperature reaction chamber, with at least one sensor disposed in each reaction chamber; the pressure sensor is a diffused silicon pressure sensor, with its sensing end facing the interior of the high-temperature reaction chamber.

[0011] As a preferred technical solution of this utility model, the annular partition plate has a plurality of guide holes evenly distributed along the annular ring; the top of the double-layer vessel assembly is provided with a sealing top cover, the sealing top cover is detachably and sealingly connected to the top of the double-layer vessel assembly, and is also sealingly connected to the through part of the guide fluid; the main feed inlet and the drive end of the stirring mechanism are both provided through the sealing top cover.

[0012] Compared with the prior art, the beneficial effects of this utility model are as follows: 1. The double-layer reactor assembly forms three independent, sealed circulation chambers (heat transfer oil / water cooling / refrigerant circulation chambers) at the top, middle, and bottom, respectively, to meet the temperature control requirements of the high-temperature, medium-temperature, and low-temperature sections. Each circulation chamber is connected to the external system through independent circulation medium inlets and outlets, allowing for precise temperature adjustment of each section. This avoids heat interference caused by single-section temperature control or cross-contamination of hot and cold media in traditional equipment, effectively ensuring the stability of the temperature gradient during crystallization and significantly improving crystal purity and crystal form consistency. 2. Fluid Guide Design: Through the combination of annular flow divider, inverted conical flow guide hood, porous sieve plate and umbrella-shaped flow divider, the material in the main feed inlet is evenly dispersed into the high-temperature reaction chamber, avoiding localized excessive concentration or incomplete reaction caused by concentrated feed; Three-stage stirring blades: The high-temperature section uses anchor-type stirring blades to enhance radial mixing of high-viscosity materials, the medium-temperature section uses turbine stirring blades to promote crystal nucleus generation and dispersion through shearing action, and the low-temperature section uses spiral stirring blades to enhance axial flow to avoid material deposition, adapting to the characteristics of materials at different stages, greatly improving mixing uniformity and reducing the risk of impurity encapsulation; 3. In the testing mechanism, platinum resistance temperature sensors are embedded at half the height of the inner wall of each reaction chamber, enabling precise monitoring of the temperature in each section; diffused silicon pressure sensors are positioned facing the interior of the high-temperature reaction chamber to monitor the pressure in the high-temperature section in real time. Through the above monitoring data, the flow rate of the circulating medium or the stirring speed can be adjusted in a timely manner, achieving dynamic control of the crystallization process and significantly improving batch-to-batch consistency of the product. 4. The evenly distributed guide holes on the annular partition ensure independent temperature in each section while allowing material to be transferred between sections through natural flow, reducing external power consumption; the sealed top cover design of the double-layer vessel assembly, combined with the mechanical seal assembly, effectively prevents material leakage or intrusion of external impurities, meeting the stringent cleanliness requirements of pharmaceutical-grade production; the independent partitioning of the circulation chamber avoids cross-mixing of media at different temperatures, reducing system complexity and energy consumption, and improving equipment operational safety. Attached Figure Description

[0013] The accompanying drawings are provided to further illustrate the present invention and form part of the specification. They are used together with the embodiments of the present invention to explain the present invention, but do not constitute a limitation thereof. In the drawings: Figure 1 This is a schematic diagram of the overall structure of this utility model; Figure 2 This is the front view of this utility model; Figure 3 This is a cross-sectional structural schematic diagram of the present invention; Figure 4 This is a schematic diagram of the fluid guiding structure of this utility model; In the diagram: 1. High-temperature section; 2. Medium-temperature section; 3. Low-temperature section; 4. Stirring mechanism; 5. Detection mechanism; 6. Sealed top cover; 7. Main feed inlet; 8. Discharge outlet; 11. High-temperature reaction chamber; 12. Fluid guide; 21. Medium-temperature reaction chamber; 31. Low-temperature reaction chamber; 41. Three-section stirring shaft; 42. Explosion-proof drive motor; 43. Anchor-type stirring blades; 44. Turbine stirring blades; 45. Spiral stirring blades; 46. Mechanical seal assembly; 51. Temperature sensor; 52. Pressure sensor; 100. Double-layer vessel assembly; 101. Inner reaction chamber; 102. Outer insulation jacket; 103. Heat transfer oil circulation chamber; 104. Water-cooled circulation chamber; 105. Refrigerant circulation chamber; 121. Annular flow divider; 122. Inverted conical flow guide shroud; 123. Porous sieve plate; 124. Umbrella-shaped flow divider; 200. Annular partition; 201. Flow guide hole; 411. First shaft section; 412. Second shaft section; 413. Third shaft section. Detailed Implementation

[0014] The preferred embodiments of the present invention will be described below with reference to the accompanying drawings. It should be understood that the preferred embodiments described herein are for illustration and explanation only and are not intended to limit the present invention.

[0015] In the attached diagram, all identical reference numerals refer to the same components.

[0016] Example 1: Basic segmented temperature-controlled crystallizer (for general pharmaceutical intermediate crystallization scenarios) like Figure 1-4 As shown, this embodiment is a basic device applicable to the crystallization of most pharmaceutical intermediates, highlighting the basic connection relationships and functions of each core component.

[0017] Please see Figure 3 The double-layer reactor assembly 100 is integrally formed by welding an inner reaction chamber 101 and an outer insulation jacket 102. The inner reaction chamber 101 is a cylindrical shell, and the outer insulation jacket 102 is an annular sandwich structure. Between the two, three independent closed circulation chambers are formed from top to bottom: an upper heat transfer oil circulation chamber 103, a middle water-cooled circulation chamber 104, and a lower refrigerant circulation chamber 105. Each circulation chamber has a circulation medium inlet at the top, connecting to an external heat transfer oil pump, water pump, and refrigeration unit, and a circulation medium outlet at the bottom, returning to the external system. The circulation chambers are physically isolated by an extension structure of an annular partition 200, ensuring no cross-contamination of hot and cold media.

[0018] Annular baffle 200: A circular flat plate made of 304 stainless steel, with eight guide holes 201 (approximately 50mm in diameter) evenly distributed circumferentially. The distance between the center of the guide hole and the axis of the inner reaction chamber 101 is half the radius, ensuring that the temperature gradient remains undisturbed when the material flows naturally between sections. The upper end face of the annular baffle 200 is welded and sealed to the bottom surface of the high-temperature reaction chamber 11, the lower end face is welded and sealed to the top surface of the medium-temperature reaction chamber 21, and the lower end face of the bottommost annular baffle 200 is welded and sealed to the top surface of the low-temperature reaction chamber 31, achieving complete separation of the high, medium, and low-temperature sections.

[0019] Please see Figure 4The guide fluid 12 includes: an annular diverter 121, an inverted conical guide hood 122, a porous sieve plate 123, and an umbrella-shaped diverter 124; wherein the top of the umbrella-shaped diverter 124 is welded to the center of the lower end face of the porous sieve plate 123. The annular diverter 121 is a horizontal disc, with its upper end face sealed to the bottom of the main feed inlet 7 by a flange, and its lower end face welded to the large-diameter end of the inverted conical guide hood 122 (cone angle 60°); the porous sieve plate 123 is set at an inclination of 15° and is fixed to the small-diameter end of the inverted conical guide hood 122 by bolts, and its plate surface is uniformly opened with φ3mm sieve holes (opening rate 40%); the umbrella-shaped diverter 124 is an inverted hemispherical thin plate (thickness 5mm), with its top welded to the center of the lower end face of the porous sieve plate 123, and its bottom maintaining a 10mm gap with the bottom inner wall of the inner reaction chamber 101 to ensure that the material flows evenly into the high-temperature reaction chamber 11 along the umbrella-shaped surface after dispersion.

[0020] Please see Figure 3 The stirring mechanism 4 consists of a three-section stirring shaft 41, which, from top to bottom, comprises the first section 411 (80mm in diameter, 400mm in length), the second section 412 (70mm in diameter, 600mm in length), and the third section 413 (60mm in diameter, 800mm in length). The sections are connected by a keyway. An explosion-proof drive motor 42 is connected to the top of the three-section stirring shaft 41 via a coupling, and the motor housing is fixed to the sealed top cover 6 with bolts. Anchor-type stirring blades 43 (10mm thick, 20mm wide, 5mm gap from the inner wall of the inner reaction chamber 101) are bolted to the outer periphery of the first shaft section 411 (covering 2 / 3 of the high-temperature reaction chamber 11 in the height direction); turbine stirring blades 44 (150mm diameter, 6 blades, 45° angle between the blades and the horizontal plane) are fixed to the outer periphery of the second shaft section 412 (located in the upper middle part of the medium-temperature reaction chamber 21) with countersunk screws; spiral stirring blades 45 (200mm pitch, 30° spiral angle) are welded to the outer periphery of the third shaft section 413 (extending 200mm above the outlet 8 of the low-temperature reaction chamber 31). A mechanical seal assembly 46 (double-end mechanical seal, flushing fluid is deionized water) is located at the penetration point between the top of the double-layer vessel assembly 100 and the three-section stirring shaft 41. The outer sealing end face is welded to the sealing top cover 6, and the inner sealing end face is clearance-fitted with the three-section stirring shaft 41 (0.1mm gap).

[0021] Please see Figure 2The detection mechanism 5 consists of a temperature sensor 51, which is a platinum resistance thermometer (Pt100, accuracy ±0.1℃), embedded in the inner wall of the high-temperature reaction chamber 11, the medium-temperature reaction chamber 21, and the low-temperature reaction chamber 31 at half the height (600mm, 700mm, and 800mm from the bottom surface, respectively) via a threaded connection. The wire passes through the porous sieve plate 123 and is connected to the external temperature control system. The pressure sensor 52 is a diffused silicon pressure sensor, fixed to the inner side of the top of the outer layer of the high-temperature section 1 via a flange (50mm from the bottom surface of the sealed top cover 6). The sensing end faces the inside of the high-temperature reaction chamber 11 (20mm from the inner wall), and the signal line is connected to the external pressure monitoring system.

[0022] Sealing top cover 6: It is a hemispherical end cap welded from steel plate, which is detachably and sealed to the top of the double-layer vessel body assembly 100 by clamp (the sealing gasket is fluororubber). It has two through holes (80mm in diameter) for the main feed port 7 (DN80 sanitary clamp interface) and the output shaft of the explosion-proof drive motor 42 to pass through, respectively. The gap between the edge of the through hole and the passing part is filled with silicone rubber sealing ring.

[0023] Example 2: Crystallization kettle for high-viscosity materials (for intermediates with viscosity > 500 mPa·s) This embodiment optimizes the stirring mechanism 4 and the guide fluid 12 based on the basic model to meet the crystallization requirements of high-viscosity materials.

[0024] Improvement of the flow guide 12: The opening ratio of the porous sieve plate 123 is increased to 50% (the pore size is increased to φ5mm), and a flow guide strip is added to the upper end face of the umbrella-shaped flow divider plate 124 to enhance the initial dispersion of the material in the high-temperature reaction chamber 11 and avoid local overheating caused by gravity accumulation of high-viscosity materials.

[0025] Improvements to the stirring mechanism 4: The width of the anchor-type stirring blade 43 is increased to 30mm (the gap with the inner wall is adjusted to 8mm), and a spiral rib (5mm high, 150mm pitch) is added to the blade surface to enhance the axial circulation of high-viscosity materials; the turbine stirring blade 44 is replaced with a wide-blade turbine (8 blades, 30° angle between the blade and the horizontal plane) to increase the shear area and promote the uniform generation of crystal nuclei in high-viscosity materials; the pitch of the spiral stirring blade 45 is increased to 250mm (spiral angle 25°) to reduce rotational resistance and ensure the smooth discharge of high-viscosity materials in the low-temperature section 3.

[0026] Example 3: Explosion-proof reinforced crystallizer (for volatile and explosive intermediates) This embodiment focuses on enhancing sealing performance and explosion-proof design, and is suitable for crystallization processes of volatile intermediates such as nitration and chlorination.

[0027] Improvements to the double-layer reactor assembly 100: The weld connecting the outer insulation jacket 102 and the inner reaction chamber 101 is made by argon arc welding with penetration testing to ensure no leakage; rupture discs are added to the inlet and outlet of the circulating medium in each circulation chamber and are linked with the external safety valve to further enhance the explosion-proof capability.

[0028] Improvements to the top cover 6: Made of 316L stainless steel, it is connected to the top of the double-layer vessel assembly 100 by a quick-release clamp, and the sealing gasket is replaced with perfluoroether rubber; a double mechanical seal assembly 46 (with a double-end mechanical seal on the inner side and a labyrinth seal on the outer side) is added to the through part between the main feed port 7 and the stirring mechanism 4, and the gap is filled with high-temperature resistant grease.

[0029] Improvements to testing mechanism 5: Pressure sensor 52 is replaced with an explosion-proof diffused silicon pressure sensor and connected to an external safety barrier to prevent sparks from igniting volatile media; the wires of temperature sensor 51 are sheathed with polytetrafluoroethylene insulating tubing to prevent insulation aging at high temperatures.

[0030] The above embodiments, through adjustments to different structural configurations, cover common general scenarios, high-viscosity material scenarios, and explosion-proof enhanced scenarios in the crystallization process of pharmaceutical intermediates, verifying the applicability and reliability of this utility model under multi-dimensional requirements.

[0031] Finally, it should be noted that the above description is merely a preferred embodiment of this utility model and is not intended to limit the utility model. Although the utility model has been described in detail with reference to the foregoing embodiments, those skilled in the art can still modify the technical solutions described in the foregoing embodiments or make equivalent substitutions for some of the technical features. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of this utility model should be included within the protection scope of this utility model.

Claims

1. A segmented temperature-controlled pharmaceutical intermediate crystallization vessel, characterized in that, include: The double-layer reactor assembly (100) is vertically arranged and consists of an inner reaction chamber (101) and an outer insulation jacket (102). The inner reaction chamber (101) and the outer insulation jacket (102) form independent and sealed circulation chambers from top to bottom. The inner reaction chamber (101) is divided into a high-temperature section (1), a medium-temperature section (2), and a low-temperature section (3) from top to bottom by at least two annular partitions (200). Each section is sealed and connected by the annular partitions (200). The inner layer of the high-temperature section (1) is a high-temperature reaction chamber (11), and the outer layer is connected to the circulation chamber. A guide fluid (12) is provided at the top of the high-temperature reaction chamber (11), and the top of the guide fluid (12) is sealed and connected to the main feed inlet (7). The medium-temperature section (2) The inner layers of the low-temperature section (3) are respectively the medium-temperature reaction chamber (21) and the low-temperature reaction chamber (31), and the outer layers are respectively connected to the corresponding circulation chambers; the bottom of the low-temperature section (3) is provided with a discharge port (8), and the discharge port (8) is sealed and connected to the bottom of the low-temperature reaction chamber (31); the detection mechanism (5) includes at least one temperature sensor (51) and at least one pressure sensor (52), the temperature sensor (51) is embedded in the inner wall of the high-temperature reaction chamber (11), the medium-temperature reaction chamber (21) and the low-temperature reaction chamber (31); the pressure sensor (52) is set on the inner side of the top of the outer layer of the high-temperature section (1); the stirring mechanism (4) penetrates the top of the double-layer vessel assembly (100) in the vertical direction and is coaxially arranged with each section of the reaction chamber, and is used to drive the mixing of materials.

2. The segmented temperature-controlled pharmaceutical intermediate crystallizing vessel according to claim 1, characterized in that, The sealed circulation chamber between the outer insulation jacket (102) and the inner reaction chamber (101) is divided into the following sections from top to bottom: the upper heat transfer oil circulation chamber (103), the middle water cooling circulation chamber (104), and the lower refrigerant circulation chamber (105); wherein: the outer layer of the high temperature section (1) is connected to the heat transfer oil circulation chamber (103); the outer layer of the medium temperature section (2) is connected to the water cooling circulation chamber (104); the outer layer of the low temperature section (3) is connected to the refrigerant circulation chamber (105); the top of the heat transfer oil circulation chamber (103), the water cooling circulation chamber (104), and the refrigerant circulation chamber (105) are respectively provided with circulation medium inlets, and the bottom of the circulation medium outlets are respectively provided, all of which are connected to the external circulation system of the double-layer reactor assembly (100); the circulation chambers are not connected to each other.

3. The segmented temperature-controlled pharmaceutical intermediate crystallizing vessel according to claim 1, characterized in that, The guide fluid (12) includes: an annular flow divider (121), the top of which is sealed and connected to the bottom of the main feed inlet (7); an inverted conical flow guide hood (122), the top of which is fixedly connected to the bottom of the annular flow divider (121); a porous sieve plate (123), which is inclinedly arranged below the inverted conical flow guide hood (122); and an umbrella-shaped flow divider plate (124), the top of which is fixedly connected to the bottom of the porous sieve plate (123), and the bottom of which is spaced apart from the bottom inner wall of the inner reaction chamber (101).

4. The segmented temperature-controlled pharmaceutical intermediate crystallizing vessel according to claim 1, characterized in that, The stirring mechanism (4) includes: a three-section stirring shaft (41), which is composed of a first shaft section (411), a second shaft section (412), and a third shaft section (413) arranged coaxially from top to bottom; an explosion-proof drive motor (42), which is fixed on the outer side of the top of the high-temperature section (1), and the output shaft is connected to the top of the three-section stirring shaft (41); an anchor stirring blade (43), which is fixed on the outer periphery of the first shaft section (411) and located in the high-temperature reaction chamber (11); a turbine stirring blade (44), which is fixed on the outer periphery of the second shaft section (412) and located in the medium-temperature reaction chamber (21); a spiral stirring blade (45), which is fixed on the outer periphery of the third shaft section (413) and located in the low-temperature reaction chamber (31); and a mechanical seal assembly (46), which is set at the penetration part between the top of the double-layer vessel assembly (100) and the three-section stirring shaft (41) to achieve dynamic sealing.

5. A segmented temperature-controlled pharmaceutical intermediate crystallizing vessel according to claim 1, characterized in that, The temperature sensor (51) is a platinum resistance sensor, which is respectively set at 1 / 2 of the height of the inner wall of the high temperature reaction chamber (11), the medium temperature reaction chamber (21) and the low temperature reaction chamber (31), with at least one sensor in each reaction chamber; the pressure sensor (52) is a diffused silicon pressure sensor, with its sensing end facing the inside of the high temperature reaction chamber (11).

6. A segmented temperature-controlled pharmaceutical intermediate crystallizing vessel according to claim 1, characterized in that, The annular partition (200) has several flow guide holes (201) evenly distributed along the annular ring; the top of the double-layer vessel assembly (100) is provided with a sealing top cover (6), the sealing top cover (6) is detachably and sealed to the top of the double-layer vessel assembly (100), and is sealed to the through part of the flow guide (12); the main feed port (7) and the driving end of the stirring mechanism (4) are both set through the sealing top cover (6).