Y type DTB crystallization kettle
By designing a Y-type DTB crystallizer, the integrated equipment solves the problems of lengthy traditional crystallization processes and dispersed equipment, achieving efficient solid-liquid separation and crystal protection, thereby improving crystallization efficiency and product quality.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- KELI SITUO (CHANGZHI) TECHNOLOGY CO LTD
- Filing Date
- 2025-08-28
- Publication Date
- 2026-07-24
AI Technical Summary
Traditional crystallization processes involve dispersed equipment, resulting in lengthy processes, large equipment footprints, low efficiency, and easily damaged crystals, which affects product quality.
The Y-type DTB crystallizer is adopted, which combines the integrated design of the crystallizer body and the clear liquid body. Solid-liquid separation is achieved through gravity settling and overflow. It integrates chemical reaction, crystallization and preliminary separation processes, and uses a propeller-type agitator and a guide tube to optimize fluid circulation.
It significantly shortens the process flow, improves production efficiency, reduces equipment investment and energy consumption, enhances crystal quality and separation effect, reduces crystal breakage, and optimizes crystal morphology and particle size distribution.
Smart Images
Figure CN224541018U_ABST
Abstract
Description
Technical Field
[0001] This utility model belongs to the field of chemical equipment technology, specifically relating to a Y-type DTB crystallization kettle. Background Technology
[0002] In the field of chemical equipment technology, especially for the production of high-value-added crystals in industries such as pharmaceuticals (e.g., API crystallization), fine chemicals, food, and electronic materials, the efficiency and stability of crystallization processes are crucial. Reaction crystallization or anti-solvent crystallization processes are widely used in these industries, but traditional crystallization processes have many problems that urgently need to be solved. In traditional crystallization processes, the three key steps—reaction, crystallization, and solid-liquid separation—are typically performed separately in multiple independent devices. This decentralized operation mode results in a lengthy process flow, large equipment footprint, and significant capital investment for equipment purchases and site rentals. Furthermore, the collaborative operation of multiple devices leads to low overall efficiency and extended production cycles. Even more disadvantageous is that in the mechanical separation step, the slurry has a low solids content and large crystal particle spacing. Due to the interaction between the crystals and the separation equipment components, the fragile crystal structure is easily damaged, thus affecting the quality and performance of the crystal product. Utility Model Content
[0003] To overcome the shortcomings of existing technologies, this utility model provides a Y-type DTB crystallization vessel, which can shorten the process flow, optimize the crystallization process, achieve precise separation and collection of clear liquid, and further improve production efficiency.
[0004] This utility model is achieved through the following technical solution.
[0005] This utility model provides a Y-type DTB crystallization vessel, including a crystallization vessel body and a clear liquid vessel body. The clear liquid vessel body is connected to the side of the crystallization vessel body. A flow port is provided on the lower part of the side wall of the crystallization vessel body. The crystallization vessel body is connected to the lower end of the clear liquid vessel body through the flow port. A feed port is provided on the lid of the crystallization vessel body. A discharge port is provided at the bottom of the crystallization vessel body. A first overflow port is provided on the upper part of the side wall of the crystallization vessel body. At least two second overflow ports at different horizontal heights are provided on the side wall of the clear liquid vessel body. A jacket is provided outside the side wall of the crystallization vessel body. A circulating medium inlet is provided on the upper part of the jacket and a circulating medium outlet is provided on the lower part of the jacket. A guide cylinder is fixedly installed inside the crystallization vessel body. A stirring shaft is installed inside the crystallization vessel body. A stirring motor for driving the stirring shaft to rotate is installed on the lid of the crystallization vessel body. At least one set of propeller-type stirrers is installed on the stirring shaft.
[0006] As a further improvement to the above solution, the guide tube is coaxially arranged with the stirring shaft, and the propulsion stirrer is located inside the guide tube.
[0007] As a further improvement to the above solution, support lugs are provided on the outer wall of the jacket and the outer wall of the clear liquid vessel.
[0008] As a further improvement to the above solution, the guide tube is connected to the inner wall of the crystallization vessel through a support plate.
[0009] As a further improvement to the above scheme, at least two sets of propeller-type agitators are installed on the stirring shaft, and at least one set of propeller-type agitators is located below the flow port.
[0010] As a further improvement to the above scheme, the second overflow port is provided with 2 to 6 outlets.
[0011] As a further improvement to the above solution, a ventilation duct is provided on the lid of the clear liquid vessel.
[0012] As a further improvement to the above solution, an arc-shaped protrusion is provided at the bottom of the crystallization vessel.
[0013] As a further improvement to the above solution, a thermometer mounting port and a level gauge mounting port are provided on the side wall of the crystallization vessel.
[0014] As a further improvement to the above solution, the crystallization vessel and the clear liquid vessel are integrally configured to form a Y-shaped vessel.
[0015] The beneficial effects of this utility model are: Compared with the traditional approach of using multiple independent devices such as reaction vessels, crystallization vessels, and separation equipment, the Y-type vessel of this invention significantly reduces the equipment footprint through the integrated design of the crystallization vessel body and the clear liquid vessel body; it also reduces related supporting facilities (such as pumps, valves, and pipelines), effectively lowering initial investment and operating costs.
[0016] In this invention, the Y-shaped vessel composed of the crystallization vessel and the clear liquid vessel can complete three core processes: chemical reaction, crystallization process and preliminary solid-liquid separation (clear liquid removal), eliminating the material transfer steps between equipment, significantly shortening the process flow and improving the overall operating efficiency.
[0017] In this invention, the clear liquid vessel body, combined with the second overflow port, can quickly and efficiently separate crystal particles from the reaction liquid / mother liquor, significantly improving the crystallizer's processing capacity per unit time.
[0018] In this invention, preliminary separation is achieved by relying on gravity settling and overflow, which greatly reduces the material handling volume of subsequent separation equipment such as centrifuges and filters, and reduces energy consumption.
[0019] In this invention, the design of second overflow ports at different heights provides flexibility for the operation of the clear liquid vessel. Operators can judge the concentration of crystal particles in the clear liquid based on real-time monitoring (such as turbidity, particle counter) or process experience, and adjust the thickness of the clear liquid layer and the discharge position according to the crystal sedimentation characteristics and clarification requirements. Attached Figure Description
[0020] Figure 1 This is a schematic diagram of the structure of this utility model; Figure 2 This is a schematic diagram of the support plate in this utility model; Figure 3 This utility model contains a schematic diagram of the propulsion mixer.
[0021] In the diagram: 1. Crystallization vessel; 101. Flow port; 102. Feed inlet; 103. Discharge outlet; 104. First overflow port; 105. Thermometer mounting port; 106. Level gauge mounting port; 2. Clear liquid vessel; 201. Second overflow port; 3. Jacket; 301. Circulating medium inlet; 302. Circulating medium outlet; 4. Guide tube; 5. Stirring shaft; 6. Stirring motor; 7. Propeller stirrer; 8. Support lug; 9. Support plate; 10. Ventilation duct; 11. Arc-shaped protrusion. Detailed Implementation
[0022] To further illustrate the technical solution of this utility model, the following description is provided in conjunction with the accompanying drawings and embodiments.
[0023] like Figures 1 to 3 As shown, this utility model provides a Y-type DTB crystallizer, which includes a crystallizer body 1 and a clear liquid vessel body 2. A flow port 101 is provided on the lower part of the side wall of the crystallizer body 1, and the crystallizer body 1 is connected to the lower end of the clear liquid vessel body 2 through the flow port 101. The clear liquid vessel body 2 can directly remove a large amount of mother liquor, reducing the load on subsequent solid-liquid separation equipment. A feed inlet 102 is provided on the lid of the crystallizer body 1, a discharge port 103 is provided at the bottom of the crystallizer body 1, and a first overflow port 104 is provided on the upper part of the side wall of the crystallizer body 1. At least two second overflow ports 201 at different horizontal heights are provided on the side wall of the crystallizing vessel 1. A jacket 3 is provided on the outside of the side wall of the crystallizing vessel 1. A circulating medium inlet 301 is provided on the upper part of the jacket 3 and a circulating medium outlet 302 is provided on the lower part of the jacket 3. A guide cylinder 4 is fixedly provided inside the crystallizing vessel 1. A stirring shaft 5 is provided inside the crystallizing vessel 1. The guide cylinder 4 is coaxially arranged with the guide cylinder 5. A stirring motor 6 for driving the stirring shaft 5 to rotate is installed on the lid of the crystallizing vessel 1. At least one set of propeller-type stirrers 7 are installed on the stirring shaft 5.
[0024] Furthermore, the crystallization vessel 1 and the clear liquid vessel 2 are integrated into one unit to form a Y-shaped vessel.
[0025] Furthermore, the lower part of the clear liquid vessel 2 is inclined and connected to the flow port 101 to prevent crystals from depositing at the bottom of the clear liquid vessel 2.
[0026] Furthermore, the propulsion agitator 7 is located inside the guide tube 4.
[0027] Furthermore, three sets of propeller-type agitators 7 are provided, all of which are located inside the guide tube 4. The propeller-type agitators 7 are three-blade propeller agitators, such as the TXL three-blade propeller agitator.
[0028] Furthermore, the outer wall of the jacket 3 and the outer wall of the clear liquid vessel 2 are provided with support lugs 8, and the number of support lugs 8 can be set according to requirements.
[0029] Furthermore, the guide tube 4 is connected to the inner wall of the crystallization vessel 1 through the support plate 9, and the guide tube 4 can be welded to the crystallization vessel 1 through the support plate 9.
[0030] Furthermore, the support plate 10 includes an upper support plate, a middle support plate, and a lower support plate, wherein the upper support plate is located above the flow port 101 and the lower support plate is located below the flow port 101.
[0031] Furthermore, at least one set of propeller mixers 7 is located below the flow port 101.
[0032] Furthermore, the height and number of the second overflow port 201 can be selected according to process requirements, and a regulating valve can be installed at the second overflow port 201.
[0033] Preferably, the second overflow port 201 is provided with 2 to 6 outlets.
[0034] In this invention, by setting a second overflow port 201, gravity overflow is used to replace mechanical separation, thus completely preserving the morphology of needle-shaped crystals, and providing a process basis for continuous production by continuously removing the clear liquid.
[0035] During reaction crystallization or antisolvent crystallization, the crystallization rate of the product often changes dynamically due to factors such as reaction progress, feeding rate, concentration, and temperature. This directly leads to fluctuations in the concentration of fine crystals entrained in the supernatant. By adjusting the second overflow port 201 at different heights, the fluctuations in crystal concentration at different stages can be effectively addressed.
[0036] When the crystallization rate is fast and the concentration of entrained crystals in the clear liquid is high (there are many fine crystals or incompletely settled crystals), a higher position of the second overflow port 201 is selected. This indirectly increases the sedimentation path length and residence time of the clear liquid in the separation zone, allowing more fine crystals to settle back to the main body 1 area of the crystallizer, thereby effectively reducing the amount of crystals entrained in the overflow liquid and ensuring the separation effect. When the crystallization rate is slow and the concentration of entrained crystals in the clear liquid is low (close to clarification), a lower position of the second overflow port 201 can be selected. This can remove the clear liquid more quickly, improve the mother liquor treatment efficiency, maintain the optimized solid-liquid ratio and supersaturation in the crystallizer, and is beneficial to the control of the crystallization process.
[0037] Furthermore, a ventilation duct 10 is provided on the lid of the clear liquid vessel 2.
[0038] Furthermore, an arc-shaped protrusion 11 is provided at the bottom of the crystallization vessel 1. When the propeller-type agitator is working, it can push the liquid downwards. After the liquid is accelerated and regulated by the guide tube, it impacts the bottom of the crystallization vessel. The arc-shaped protrusion 11 can change the direction of fluid flow, causing the fluid to split and turn, prompting the fluid to flow from the bottom to the side wall and top of the crystallization vessel 1, forming a more complex and efficient circulating flow field. At the same time, it can also eliminate potential dead zones at the bottom of the vessel, ensuring that the material in all parts of the vessel can continuously participate in the crystallization process. This circulation is conducive to fully mixing the material in all parts of the vessel, making the solute and solvent contact more uniformly. For reaction crystallization or anti-solvent crystallization processes, it can promote the more orderly arrangement of solute molecules to form crystals, improve the uniformity and quality of crystallization, and enhance the overall crystallization efficiency.
[0039] The arc-shaped protrusion 11 allows the crystal to slide down the arc surface to the discharge position, reducing the accumulation of crystals in other parts of the bottom of the vessel.
[0040] The arc-shaped protrusion 11 can prevent blockage of the discharge port and avoid crystal accumulation and blockage near the discharge port. The arc-shaped protrusion 11 provides a certain buffering and guiding effect when the crystal is close to the discharge port 103, so that the crystal can flow out of the crystallization vessel 1 more smoothly and ensure the continuity of the crystallization operation. Furthermore, a thermometer mounting port 105 and a level gauge mounting port 106 are provided on the side wall of the crystallization vessel 1. The thermometer mounting port 105 is connected to a thermometer via a flange, and the level gauge mounting port 106 is connected to a level gauge via a flange. The level gauge can be a single-flange differential pressure level gauge.
[0041] Furthermore, the upper part of the crystallization vessel 1 is provided with a first overflow port 104, and the upper part of the clear liquid vessel 2 is provided with a second overflow port 201. The height of the first overflow port 104 is higher than that of the second overflow port 201. When the feed exceeds the liquid holding volume, it can overflow through the first overflow port 104 to prevent the material from being overfilled.
[0042] Working principle: In this invention, the reaction and crystallization process is mainly carried out in the crystallization vessel 1. After crystallization is completed (or during the process), a slurry containing crystal particles is formed in the vessel. Under the action of the propeller-type agitator 7 and fluid dynamics, the heavier crystal particles are mainly enriched and retained in the bottom area of the crystallization vessel 1 and discharged from the outlet 103.
[0043] The supernatant containing very few or tiny particles (with the goal of clarification) enters the connected clear liquid vessel 2 under the action of gravity or pressure difference.
[0044] The liquid entering the clear liquid vessel 2 has an extremely low particle content, achieving preliminary clarification.
[0045] The initially clarified liquid flows out through the second overflow port 201 at different heights on the clear liquid vessel body 2. Example
[0046] In this embodiment, the Y-type DTB crystallization vessel is used for the production of antisolvent crystallization of a certain pharmaceutical intermediate. The target product is a pharmaceutical intermediate with strict requirements on crystal morphology and particle size. The effective volume of the crystallization vessel 1 is 1000 L, and the effective volume of the clear liquid vessel 2 is 200 L. There are four second overflow ports 201 (with heights of 30 cm, 45 cm, 60 cm, and 75 cm from the top surface of the crystallization vessel, respectively).
[0047] Operating procedures: Reaction / crystallization stage: Add intermediate acetone solution (600 L) to crystallization vessel 1, control the temperature at 25℃, add antisolvent pure water (200 L / h) at a constant flow rate, and stir at 100 rpm. Crystals nucleate and grow, forming a suspension slurry.
[0048] Dynamic overflow control: 30 minutes before feeding (peak period for fine crystals): Online monitoring shows a sudden increase in the concentration of clear liquid particles (>50,000 particles / mL). Switch to the highest second overflow port (30 cm position) to increase the settling height and intercept fine crystals. Feed for 30-90 minutes (stable growth period): When the particle concentration drops to 5000-10000 particles / mL, switch to the second overflow port in the middle position (45 cm position) to balance the separation efficiency and processing speed; End of feeding stage (clarification period): When the particle concentration is stable at <1000 particles / mL, switch to the lowest second overflow port (75cm position) to quickly remove the mother liquor and maintain crystallization kinetics.
[0049] Product output: The clear liquid continuously overflows to the solvent recovery unit, and the bottom valve of crystallization vessel 1 discharges high solid content crystal slurry (solid content ≥30%).
[0050] Comparative Example 1 The above-mentioned drug intermediates are produced using a traditional process with independent reaction vessels, crystallization vessels, and centrifuges: antisolvent crystallization. After separation using a centrifuge, the crystal breakage rate is as high as 18%; the product entrainment loss in the mother liquor is about 6%; the target particle size D90 compliance rate is 85%; the single batch production cycle is as long as 20 hours (including transfer, filtration, and drying); the mother liquor entrainment loss is 6%; and the particle concentration fluctuation range of the overflow liquid throughout the process is >±50%.
[0051] Compared with Comparative Example 1, the crystal quality produced by the Y-type DTB crystallizer in Example 1 was significantly improved. After separation by centrifuge, the crystal breakage rate was reduced to 0.8% (compared to 18% in the centrifugation process); the target particle size D90 compliance rate was 100% (compared to only 85% in the traditional process); the single batch cycle was shortened by 40% (from 20 hours to 12 hours); the mother liquor entrainment loss was controlled within 0.4% (compared to 6% in the original process); a single device completed the reaction, crystallization, and primary separation, reducing the need for three intermediate storage tanks and saving on equipment purchase and maintenance costs; the overflow mother liquor was directly reused, reducing solvent distillation energy consumption by 35%; and the overall overflow liquid particle concentration fluctuation range was <±15% (compared to >±50% in traditional batch separation).
[0052] The foregoing has shown and described the basic principles, main features, and advantages of this utility model. It will be apparent to those skilled in the art that this utility model is not limited to the details of the exemplary embodiments described above, and that it can be implemented in other specific forms without departing from the spirit or basic characteristics of this utility model. Therefore, the embodiments should be considered exemplary and non-limiting in all respects. The scope of this utility model is defined by the appended claims rather than the foregoing description, and thus all variations falling within the meaning and scope of equivalents of the claims are intended to be included within this utility model.
[0053] Furthermore, it should be understood that although this specification describes embodiments, not every embodiment contains only one independent technical solution. This narrative style is merely for clarity. Those skilled in the art should consider the specification as a whole, and the technical solutions in each embodiment can also be appropriately combined to form other embodiments that can be understood by those skilled in the art.
Claims
1. A Y-type DTB crystallization vessel, characterized in that: The system includes a crystallization vessel (1) and a clear liquid vessel (2). The lower part of the side wall of the crystallization vessel (1) is provided with a flow port (101). The crystallization vessel (1) is connected to the lower end of the clear liquid vessel (2) through the flow port (101). The lid of the crystallization vessel (1) is provided with a feed port (102). The bottom of the crystallization vessel (1) is provided with a discharge port (103). The upper part of the side wall of the crystallization vessel (1) is provided with a first overflow port (104). The side wall of the clear liquid vessel (2) is provided with at least two second overflow ports at different horizontal heights. Outlet (201), a jacket (3) is provided on the outside of the side wall of the crystallization vessel (1), a circulating medium inlet (301) is provided on the upper part of the jacket (3), a circulating medium outlet (302) is provided on the lower part of the jacket (3), a guide tube (4) is fixedly provided inside the crystallization vessel (1), a stirring shaft (5) is provided inside the crystallization vessel (1), a stirring motor (6) for driving the stirring shaft (5) to rotate is installed on the lid of the crystallization vessel (1), and at least one set of propeller-type stirrers (7) are installed on the stirring shaft (5).
2. The Y-type DTB crystallization vessel according to claim 1, characterized in that: The guide tube (4) is coaxially arranged with the stirring shaft (5), and the propulsion stirrer (7) is located inside the guide tube (4).
3. The Y-type DTB crystallization reactor according to claim 1, characterized in that: Supporting lugs (8) are provided on the outer wall of the jacket (3) and the outer wall of the clear liquid vessel (2).
4. The Y-type DTB crystallization reactor according to claim 3, characterized in that: The guide tube (4) is connected to the inner wall of the crystallization vessel (1) through the support plate (9).
5. A Y-type DTB crystallization reactor according to claim 1, characterized in that: At least two sets of propeller-type agitators (7) are installed on the stirring shaft (5), and at least one set of propeller-type agitators (7) is located below the flow port (101).
6. The Y-type DTB crystallization reactor according to claim 1, characterized in that: The second overflow port (201) has 2 to 6 outlets.
7. A Y-type DTB crystallization reactor according to claim 1, characterized in that: The lid of the clear liquid vessel (2) is equipped with a ventilation tube (10).
8. A Y-type DTB crystallization reactor according to claim 1, characterized in that: The bottom of the crystallization vessel (1) is provided with an arc-shaped protrusion (11).
9. A Y-type DTB crystallization reactor according to claim 1, characterized in that: The side wall of the crystallization vessel (1) is provided with a thermometer mounting port (105) and a level gauge mounting port (106).
10. A Y-type DTB crystallization vessel according to claim 1, characterized in that: The crystallization vessel (1) and the clear liquid vessel (2) are integrally configured to form a Y-shaped vessel.