Efficient rectification water removal device

Abstract

The utility model provides a high-efficiency rectification dewatering device which is characterized in that a perhydroacenaphthene material is heated to a certain temperature through a tower kettle and an external circulation heating module, water vapor is condensed and flows back to a bubble cap distributor through a first condenser, water and perhydroacenaphthene are layered through the bubble cap distributor, water is produced from a side line at the lower layer of the bubble cap distributor, and the water is separated from the lower layer of the bubble cap distributor. According to the invention, the perhydroacenaphthene is introduced into the tower kettle, the perhydroacenaphthene at the upper layer is refluxed into the tower kettle for the next round of distillation reflux circulation until drying is completed, and a dried perhydroacenaphthene product is extracted through the second condenser, so that anhydrous magnesium sulfate is not needed for drying, additional material input is not needed, solid waste output is reduced, manual feeding and taking are not needed, and labor cost is reduced.

Description

Technical Field

[0001] This utility model relates to the field of distillation equipment, and in particular to a high-efficiency distillation dehydration device. Background Technology

[0002] Perhydroacenaphthene, also known as hydroacenaphthene, is an important chemical raw material used in the preparation of the pharmaceutical drug memantine hydrochloride, as well as in the production of flame retardants. Its molecular formula is C1. 12 H 20 It has a molecular weight of 164, a melting point of 36℃, a boiling point of 235℃, and a density (20℃, g / mL) of 0.927±0.002. It is soluble in dichloromethane.

[0003] Perhydroacenaphthene is a colorless, transparent, oily liquid. At room temperature, its solubility in water is low. In the preparation process of perhydroacenaphthene, water removal is a crucial step to ensure the smooth progress of the reaction and the purity of the product. The common method of water removal is to add anhydrous magnesium sulfate for drying. The strong hygroscopic properties of anhydrous magnesium sulfate effectively absorb moisture, forming hydrated magnesium sulfate, thereby reducing the water content in the perhydroacenaphthene and improving the purity and quality of the product. Afterwards, filtration and distillation are performed to finally obtain the pure product. The process is shown in the attached figure. Figure 1 As shown.

[0004] This dehydration method requires the use of magnesium sulfate for drying, which requires additional material input and will generate additional solid waste. On the other hand, during the drying and filtration process, manual operation is required to add solids and remove solids from the filter, which increases labor costs. Utility Model Content

[0005] Therefore, there is a need to provide a high-efficiency distillation dehydration device to solve this problem.

[0006] To achieve the above objectives, this utility model provides a high-efficiency distillation dehydration device, including a column reboiler. The column reboiler is provided with a first circulation port and a second circulation port, which are used to connect to an external circulation heating module to circulate and heat the acenaphthene material to a certain temperature. A distillation column is also provided at the top of the column reboiler, and a bubble cap distributor is installed at the top of the distillation column. The bottom side wall of the bubble cap distributor is provided with a water outlet. A first condenser is provided at the top of the bubble cap distributor and the two are connected. The top of the first condenser is provided with a first gas phase outlet, which is connected to a second gas phase inlet at the top of the second condenser through a gas pipe. The bottom of the second condenser is provided with a product outlet.

[0007] Furthermore, the external circulation heating module includes a circulation pipeline, a heater, and an external circulation pump. The two ends of the circulation pipeline are respectively connected to the first circulation port and the second circulation port, and the heater and the external circulation pump are connected in series along the path of the circulation pipeline.

[0008] Furthermore, the interior of the column reactor is provided with a column reactor distributor, which is located at the top of the column reactor.

[0009] Furthermore, it also includes a sampling port, which is located on the circulation pipeline and / or the discharge pipeline.

[0010] Furthermore, the interior of the distillation column is filled with packing material.

[0011] Furthermore, the packing material is a corrugated wire mesh packing material.

[0012] Furthermore, the length of the distillation column is 4m.

[0013] Furthermore, it also includes a control unit and a level gauge and a solenoid valve electrically connected thereto. The level gauge is located in the lower layer of the bubble distributor, and the solenoid valve is located at the outlet of the bubble distributor.

[0014] Unlike existing technologies, the above-mentioned technical solution heats the perhydroacenaphthene material to a certain temperature through a tower reboiler and an external circulation heating module. Water vapor is condensed and refluxed to a bubble cap distributor via a first condenser. The bubble cap distributor separates the water and perhydroacenaphthene into layers. Water is collected from the side stream of the lower layer of the bubble cap distributor, while the upper layer of perhydroacenaphthene is refluxed back into the tower reboiler for the next round of distillation and reflux circulation. This process continues until drying is complete. The dried perhydroacenaphthene product is then collected through a second condenser. This method eliminates the need for anhydrous magnesium sulfate for drying, requires no additional material input, reduces solid waste generation, and eliminates the need for manual feeding and unloading, thus lowering labor costs. Attached Figure Description

[0015] Figure 1 This is a schematic diagram of the structure of a high-efficiency distillation and dehydration device according to a specific embodiment;

[0016] Figure 2 A schematic diagram of a high-efficiency distillation dehydration device according to another specific embodiment;

[0017] Figure 3 A schematic diagram of a high-efficiency distillation dehydration device with a distillation column, as described in another specific embodiment;

[0018] Figure 4 A schematic diagram of a high-efficiency distillation dehydration device with a reboiler distributor, as described in another specific embodiment;

[0019] Figure 5 The diagram below shows a high-efficiency distillation and dehydration device with a level gauge and a solenoid valve, as described in another specific embodiment.

[0020] Explanation of reference numerals in the attached figures:

[0021] 10. Distillation column bottom; 101. Distillation column bottom distributor; 20. External circulation heating module; 201. Circulation pipeline; 202. Heater; 203. External circulation pump; 30. Bubble cap distributor; 40. First condenser; 50. Second condenser; 51. Discharge pipeline; 60. Distillation column; 70. Level gauge; 80. Solenoid valve. Detailed Implementation

[0022] To explain in detail the technical content, structural features, objectives, and effects of the technical solution, the following description is provided in conjunction with specific embodiments and accompanying drawings.

[0023] In this document, the term "embodiment" means that a specific feature, structure, or characteristic described in connection with an embodiment may be included in at least one embodiment of this application. The term "embodiment" appearing in various places throughout the specification does not necessarily refer to the same embodiment, nor does it specifically limit its independence or connection with other embodiments. In principle, in this application, as long as there are no technical contradictions or conflicts, the technical features mentioned in each embodiment can be combined in any way to form corresponding implementable technical solutions.

[0024] Unless otherwise defined, the technical terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application pertains; the use of related terms herein is merely for the purpose of describing particular embodiments and is not intended to limit this application.

[0025] In the description of this application, the term "and / or" is used to describe the logical relationship between objects, indicating that three relationships can exist. For example, A and / or B means: A exists, B exists, and A and B exist simultaneously. Additionally, the character " / " in this document generally indicates that the preceding and following objects have an "or" logical relationship.

[0026] In this application, terms such as “first” and “second” are used only to distinguish one entity or operation from another, and do not necessarily require or imply any actual quantity, hierarchy or order relationship between these entities or operations.

[0027] Unless otherwise specified, the use of terms such as “comprising,” “including,” “having,” or other similar expressions in this application is intended to cover non-exclusive inclusion, which does not exclude the presence of additional elements in a process, method, or product that includes the stated elements, such that a process, method, or product that includes a list of elements may include not only those defined elements but also other elements not expressly listed, or elements inherent to such a process, method, or product.

[0028] Similar to the understanding in the Examination Guidelines, in this application, expressions such as "greater than," "less than," and "exceeding" are understood to exclude the stated number; expressions such as "above," "below," and "within" are understood to include the stated number. Furthermore, in the description of the embodiments in this application, "multiple" means two or more (including two), and similar expressions related to "multiple" are also understood in this way, such as "multiple groups" and "multiple times," unless otherwise explicitly specified.

[0029] In the description of the embodiments of this application, the space-related expressions used, such as "center," "longitudinal," "lateral," "length," "width," "thickness," "upper," "lower," "front," "rear," "left," "right," "vertical," "horizontal," "vertical," "top," "bottom," "inner," "outer," "clockwise," "counterclockwise," "axial," "radial," and "circumferential," indicate the orientation or positional relationship based on the orientation or positional relationship shown in the specific embodiments or drawings. They are only for the purpose of describing the specific embodiments of this application or for the reader's understanding, and do not indicate or imply that the device or component referred to must have a specific position, a specific orientation, or be constructed or operated in a specific orientation. Therefore, they should not be construed as limitations on the embodiments of this application.

[0030] Unless otherwise expressly specified or limited, the terms "installation," "connection," "linking," "fixing," and "setting," as used in the description of the embodiments of this application, should be interpreted broadly. For example, "connection" can be a fixed connection, a detachable connection, or an integral setting; it can be a mechanical connection, an electrical connection, or a communication connection; it can be a direct connection or an indirect connection through an intermediate medium; it can be the internal connection of two components or the interaction between two components. For those skilled in the art to which this application pertains, the specific meaning of the above terms in the embodiments of this application can be understood according to the specific circumstances.

[0031] Please see Figures 1 to 5This embodiment provides a high-efficiency distillation and dehydration device, including a reboiler 10. The reboiler 10 is used to receive liquid descending from the device and, as a container, works with an external circulation heating module to heat the liquid to be distilled inside. The reboiler 10 can adopt a horizontal or leg-supported structure. The entire device is insulated, and the surface temperature of the insulation layer must not exceed 45°C. The heating module vaporizes the water inside and returns it to the column to maintain the distillation process. The reboiler 10 is located at the bottom of the overall device. The material of the reboiler 10 is usually stainless steel, such as SUS304 or SUS316L, which have good corrosion resistance and processing performance. The device head, cylinder, and insulation shell are also often made of 304 stainless steel. The insulation material may be high-temperature resistant polyurethane. The reboiler 10 is equipped with a first circulation port and a second circulation port, which are connected to the external circulation heating module 20 to circulate and heat the acenaphthene material to a certain temperature. Specifically, the heating module raises the internal temperature of the reboiler 10 to 150°C, achieving a vacuum state and a pressure of -0.1 MPa. A distillation column is also located at the top of the reboiler 10, with a bubble cap distributor installed at the top. It should be noted that the distillation column and the bottom of the bubble cap distributor 30 are in a sealed connection. Steam inside the reboiler 10 can rise through the distillation column to the interior of the bubble cap distributor 30. The steam contains water and organic acenaphthene. A water outlet is located on the bottom side wall of the bubble cap distributor 30, and a valve can be installed at the outlet. A pipeline connected to the valve leads the collected water to a collection tank for collection. A water pump can also be connected to the outlet to increase the water collection speed. A peristaltic pump can be used to easily control the pumping rate. The top of the blister distributor 30 is provided with a first condenser 40 and the two are connected. The top of the first condenser 40 is provided with a first gas phase outlet. The first gas phase outlet is connected to the second gas phase inlet at the top of the second condenser 50 through a gas pipe. The bottom of the second condenser 50 is provided with a product outlet.

[0032] The structures of the first condenser 40 and the second condenser 50 can both refer to the top condensers of existing distillation columns. The top condenser of a distillation column is a key piece of equipment in the distillation process, and its main structure is typically a shell-and-tube heat exchanger with corresponding tube bundles inside. In this type of condenser, the refrigerant enters the outer tube, while the vapor flows in the inner tube. When the refrigerant flows through the outer tube, it absorbs heat from the vapor inside the column, causing it to condense into a liquid, which then flows out through the condensate outlet at the bottom. The core function of the top condenser is to cool the vapor rising from the top of the column into a liquid; this process is called condensation. Effective condensation helps to recover high-purity light components and output these components as the top product. The vapor reaching the top of the column after multi-stage separation has a high content of light components. After entering the condenser, it is cooled to below saturation using a cooling medium (such as chilled water or refrigerant), thus converting the vapor into a liquid. Part of the condensed liquid is discharged from the system as distillate, and the other part is returned to the column as reflux, playing a role in reflux regulation of the separation process within the column. The function of the top condenser is to recover useful light components by condensing vapors, while maintaining heat and mass balance within the column, ensuring the continuity and efficiency of the distillation process.

[0033] This novel design comprehensively considers the solid-liquid state and physicochemical properties of the material for efficient dehydration of perhydroacenaphthene. Perhydroacenaphthene is a slightly water-soluble organic compound with a boiling point of 232℃, while water has a boiling point of 100℃. After entering the device, the perhydroacenaphthene material is heated to a certain temperature (150℃) by an external circulation heater 202 and subjected to total reflux under a certain vacuum degree (-0.1 MPa). Water vapor reaches the first condenser 40 and is condensed and refluxed. During the reflux process, water and a small amount of perhydroacenaphthene are... The bubble cap distributor 30 is used for stratification, with water in the lower layer and perhydroacenaphthene in the upper layer. Water containing a large amount of water and a small amount of perhydroacenaphthene is collected at the water inlet via a side-stream sampling method. Then, the perhydroacenaphthene in the upper layer of the bubble cap distributor 30 is refluxed back to the reboiler 10. This reflux process is repeated until the moisture content in the system falls below a certain level. At this point, the side-stream valve is closed, the first condenser 40 is shut off, and the perhydroacenaphthene is heated to its vapor temperature and condensed and collected through the second condenser 50 to obtain a dry perhydroacenaphthene product. The first condenser 40 and the second condenser 50 are located at the same height.

[0034] This novel method heats the acenaphthene material to a certain temperature using a reboiler 10 and an external circulation heating module. Water vapor is condensed and refluxed to a bubble distributor 30 via a first condenser 40. The bubble distributor 30 separates the water and acenaphthene into layers. Water is collected from the side stream of the lower layer of the bubble distributor 30, while the upper layer of acenaphthene is refluxed back into the reboiler 10 for the next round of distillation and reflux circulation. After drying is complete, the dried acenaphthene product is collected via a second condenser 50. This method eliminates the need for anhydrous magnesium sulfate for drying, requires no additional material input, reduces solid waste generation, and eliminates the need for manual feeding and retrieval, thus lowering labor costs.

[0035] Specifically, the external circulation heating module includes a circulation pipeline 201, a heater 202, and an external circulation pump 203. The two ends of the circulation pipeline 201 are connected to a first circulation port and a second circulation port, respectively. The heater 202 and the external circulation pump 203 are connected in series along the path of the circulation pipeline 201. The circulation pipeline 201 can be made of stainless steel, carbon steel, seamless steel pipe, or other materials. The heater 202 is used to heat the liquid in the circulation pipeline 201, causing it to partially vaporize. The generated vapor is returned to the device to maintain the distillation process. The heater 202 can be a commonly used device for heating organic materials in the prior art, which will not be elaborated here. The external circulation pump 203 is a centrifugal pump. Its working principle is to use the rotation of the impeller to generate centrifugal force, drawing the liquid into the pump body from the inlet, then accelerating the liquid and discharging it from the pump body, thus realizing the liquid transport. Centrifugal pumps are characterized by their simple structure, high efficiency, and stable flow rate. Axial flow pumps can also be used, which utilize the rotation of an impeller to push liquid axially, suitable for high-flow-rate and low-head liquid transportation. Mixed flow pumps, combining the characteristics of centrifugal and axial flow pumps, are suitable for medium-to-high-flow-rate and medium-head liquid transportation. Vortex pumps, using the power of a vortex to transfer liquid from one direction to another, are suitable for handling liquids containing gas or foam. Diaphragm pumps can also be used, and based on the power source of their actuators, they can be divided into three types: pneumatic, electric, and hydraulic. These include pneumatic diaphragm pumps powered by compressed air, electric diaphragm pumps powered by electricity, and electro-hydraulic diaphragm pumps powered by the pressure of the liquid medium (such as oil). The aforementioned types of external circulation pumps 203 can be selected and adjusted according to the actual production scale.

[0036] In some embodiments, a sampling port is also included, which is located on the circulation pipeline 201 and / or the discharge pipeline 51. Samples can be extracted through the sampling port on the circulation pipeline 201 for moisture content detection, facilitating monitoring of the material moisture content inside the device. Furthermore, materials can be promptly removed when a specified moisture content is reached, avoiding the consumption of additional energy and increased costs. Products can be extracted through the sampling port on the discharge pipeline 51 for testing to verify their moisture content and ensure product quality.

[0037] In some embodiments, a distillation distributor 101 is provided inside the distillation vessel 10, and the distributor 101 is located at the top of the distillation vessel 10. The structure of the distillation distributor 101 can be tubular, trough-type, disc-type, or a combination of these types. Its main function is to uniformly initially or redistribute the liquid at the top of the packing or at a certain height, thereby improving the effective surface for mass and heat transfer, improving interphase contact, and thus improving the efficiency of distillation. The working principle is as follows: using different flow driving forces and outflow methods, such as orifice flow and weir flow, the liquid is uniformly distributed onto the packing layer. For example, the tubular distillation distributor 101 uses several distribution branches installed on the main pipe, with spray holes at the bottom of each branch to ensure uniform liquid distribution. The disc-type distillation distributor 101 has liquid spray holes and a riser pipe on the base, separating the gas and liquid flow channels. The gas rises from the riser pipe, while the liquid maintains a certain level on the base and flows down from the spray holes. The column distributor 101 helps to achieve a more efficient separation and purification process.

[0038] In some embodiments, the distillation column 60 is internally packed with packing material. The packing material can be perforated corrugated packing, metal Intalox packing, metal saddle rings, or metal stepped rings, etc. Preferably, the packing material is a wire mesh packing. The length of the distillation column 60 is 4m. Wire mesh packing is a structured packing material, typically made of plastic or metal wire mesh, with a corrugated shape. This structure increases the specific surface area of ​​the packing, thus providing a larger gas-liquid contact area. Its main function is to promote sufficient contact and mass transfer between gas and liquid in the device, enabling rapid and efficient mass and heat transfer. Through its special structural design, wire mesh packing can form a phase interface with sufficient contact between the gas and liquid phases, allowing mass and heat exchange between the two phases on the packing surface. The composition of the two phases changes continuously along the height, enhancing the gas-liquid mass and heat transfer effect. The corrugated shape of the wire mesh packing helps the liquid form a thin film on the packing surface, increasing the gas-liquid contact time and improving mass transfer efficiency. It also reduces the resistance of gas passing through the packing layer, improving the throughput and efficiency of the distillation column.

[0039] In some embodiments, a control unit is also included, along with a level gauge 70 and a solenoid valve 80 electrically connected thereto. The level gauge 70 is located in the lower layer of the bubble distributor 30, and the solenoid valve 80 is located at the outlet of the bubble distributor 30. The control unit can be a PLC controller. The control unit receives electrical signals from the level gauge 70, and when the lower layer of the bubble distributor 30 reaches a specified level, the control unit controls the solenoid valve 80 to open, extracting the lower layer water. After extraction, the control unit closes the solenoid valve 80 to begin the next round of cyclic distillation. This reduces manual operation steps, improves efficiency, and lowers costs.

[0040] It should be noted that although the above embodiments have been described herein, this does not limit the scope of patent protection for this utility model. Therefore, any changes and modifications made to the embodiments described herein based on the innovative concept of this utility model, or equivalent structural or procedural transformations made using the content of this utility model's specification and drawings, directly or indirectly applying the above technical solutions to other related technical fields, are all included within the scope of protection of this utility model patent.

Claims

1. A high-efficiency distillation dehydration device, characterized in that: The system includes a reboiler, which has a first circulation port and a second circulation port. The first and second circulation ports are used to connect to an external circulation heating module to circulate and heat the acenaphthene material to a certain temperature. A distillation column is also provided at the top of the reboiler. A bubble cap distributor is installed at the top of the distillation column, and a water outlet is provided on the bottom side wall of the bubble cap distributor. A first condenser is provided at the top of the bubble cap distributor and the two are connected. The top of the first condenser has a first gas phase outlet, which is connected to the second gas phase inlet at the top of the second condenser through a gas pipe. The bottom of the second condenser has a product outlet.

2. The high-efficiency distillation dehydration device according to claim 1, characterized in that: The external circulation heating module includes a circulation pipeline, a heater, and an external circulation pump. The two ends of the circulation pipeline are connected to the first circulation port and the second circulation port, respectively. The heater and the external circulation pump are connected in series along the path of the circulation pipeline.

3. The high-efficiency distillation dehydration device according to claim 2, characterized in that: The tower retort is equipped with a tower retort distributor located at the top of the tower retort.

4. The high-efficiency distillation dehydration device according to claim 2, characterized in that: It also includes a sampling port, which is located on the circulation pipeline and / or the discharge pipeline.

5. The high-efficiency distillation dehydration device according to claim 4, characterized in that: The distillation column is filled with packing material.

6. The high-efficiency distillation dehydration device according to claim 5, characterized in that: The packing material is a corrugated wire mesh packing material.

7. The high-efficiency distillation dehydration device according to claim 6, characterized in that: The distillation column is 4m long.

8. The high-efficiency distillation dehydration device according to claim 1, characterized in that: It also includes a control unit and a level gauge and a solenoid valve electrically connected thereto. The level gauge is located in the lower layer of the bubble distributor, and the solenoid valve is located at the outlet of the bubble distributor.

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