Device for removing moisture in organic solvent
By designing the feed at the top of the distillation column and implementing continuous oil-water phase separation, the problem of removing water from organic solvents has been solved, enabling efficient and safe continuous production and meeting the demand for high-purity organic solvents.
Patent Information
- Application Number
- CN202520073090.0
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Filing Date
- 2025-01-13
- Publication Date
- 2026-01-06
- Estimated Expiration
- 2035-01-13
AI Technical Summary
Existing technologies struggle to efficiently remove moisture from organic solvents, especially when ethanol and water form an azeotrope. Conventional distillation methods often fail to achieve a water content below 0.5%, and batch azeotropic distillation suffers from low yield and high energy consumption, making it unsuitable for large-scale production.
The distillation column adopts a top-feed design, combined with a settling tank, an inverted U-shaped bend, and a pressure balance pipe, to introduce continuous oil-water phase separation, preventing gas-liquid entrainment and flooding. Through the combined linkage of oil-water phase separators A and B, rapid separation and continuous production are achieved.
It achieves a high-capacity, low-energy-consumption continuous dehydration process, with a product moisture content of ≤0.5%, meeting the requirement of organic solvent purity of over 99.5%, avoiding material loss and safety risks, and improving production efficiency and process safety.
Smart Images
Figure CN223760437U_ABST
Abstract
Description
Technical Field
[0001] This utility model relates to the field of pharmaceutical and chemical production equipment and distillation purification and dehydration technology, and in particular to a device for removing moisture from organic solvents. Background Technology
[0002] In the production processes of pharmaceutical intermediates and fine chemicals, organic solvents that can form azeotropes with water, such as ethanol, are frequently encountered. In production applications, the purity requirement for anhydrous ethanol is 99.5% or higher, with particularly stringent requirements for controlling water content. Even small or trace amounts of water can directly affect the normal use of organic solvents and the yield and quality of related products. Taking ethanol as an example, under normal pressure, ethanol forms an azeotrope with water, consisting of 95.0% ethanol and 5.0% water, with an azeotropic point of 78.1°C. This azeotrope is difficult to separate from water. Therefore, conventional distillation conditions rarely yield ethanol with a water content below 0.5%. Using conventional distillation methods to evaporate ethanol will maintain its water content at around 5.0%.
[0003] Batch azeotropic distillation is a commonly used method for removing water from organic solvents for purification; simply put, it involves distilling batches of solvent one pot at a time. Its significant drawbacks are low yield, low efficiency, and relatively high energy consumption. It is only suitable for small enterprises, laboratories, or pilot plants for dehydration and purification of organic solvents. Therefore, designing a continuous dehydration method that is suitable for more manufacturers and features a simple, efficient, and stable process is of great value. Summary of the Invention
[0004] To address the shortcomings of existing intermittent distillation dehydration devices, this invention discloses a device for removing moisture from organic solvents. It incorporates a design that feeds from the top of the distillation column and collects the product from the column. A settling device is installed between the bottom of the distillation column and the distillation vessel. Continuous oil-water phase separation is implemented, along with a reverse U-shaped bend and a pressure balancing pipe. Compared to intermittent azeotropic distillation dehydration, this device effectively prevents gas-liquid entrainment and flooding, rapidly removes moisture from organic solvents, has high capacity, low energy consumption, and can continuously feed and collect qualified products with a moisture content below 0.5%.
[0005] This utility model discloses a device for removing moisture from organic solvents, comprising: a distillation kettle, a distillation column, a reboiler, a settling tank, a fluid distributor, a crude product condenser, a pre-mixed phase inlet, an oil-water phase separator A, an oil-water phase separator B, a pre-oil phase outlet, a post-mixed phase inlet, a post-oil phase outlet, a water-carrying agent transfer tank, a water-carrying agent metering tank, a circulating pump, a flow meter, a diversion trough, a qualified product condenser, an online detection sampling point, a non-qualified product control valve, a qualified product control valve, a qualified product receiving tank, a crude product storage tank, a crude product feeding pump, a crude product spray head, a reverse U-shaped bend, a pressure balance pipe, and a wastewater outlet. The device is characterized in that a reboiler is installed inside the distillation kettle, the distillation column is located directly above the distillation kettle, a settling tank is installed between the bottom of the distillation column and the distillation kettle, and the top of the distillation column is connected to the crude product via a pipe. The product condenser is connected to oil-water phase separator A. The upstream oil phase outlet of oil-water phase separator A is connected to the downstream mixed phase inlet of oil-water phase separator B. The downstream oil phase outlet of oil-water phase separator B is connected to a water-carrying agent transfer tank. The water-carrying agent transfer tank is connected to a water-carrying agent metering tank via a pipeline. The bottom of the water-carrying agent transfer tank is connected to the top of the distillation column via a circulating pump. A fluid distributor is installed at the top of the distillation column. The bottoms of oil-water phase separator A and oil-water phase separator B are connected together and connected to a wastewater outlet via a pipeline and a reverse U-bend. The diversion channel is located in the middle of the distillation column and is connected to the qualified product condenser via a pipeline. An online detection sampling point, a non-conforming product control valve, and a qualified product control valve are installed at the front end of the material outlet of the qualified product condenser. The qualified product control valve is connected forward to the qualified product receiving tank. The above-mentioned components are organically combined to achieve the function of effectively removing water from the organic solvent that azeotropically reacts with water.
[0006] Preferably, the device for removing moisture from organic solvents according to the present invention is characterized in that the settler, located between the bottom of the distillation column and the distillation kettle, is spherical, ellipsoidal, or cylindrical in shape, and its diameter is 1.5-2.5 times the diameter of the distillation column. This design aims to prevent gas-liquid entrainment or flooding caused by overheating during distillation, ensuring product purity and process safety.
[0007] Preferably, the device for removing moisture from organic solvents according to the present invention is characterized in that the crude product condenser consists of 2-4 units with a heat exchange area of 100m². 2 The spiral plate condensers are combined in parallel, or 2-4 shell-and-tube condensers are combined in parallel, with a heat exchange area of 200-400 m2. The purpose of this design is to ensure that the mixed gas exiting the distillation column is rapidly condensed, avoiding the backward movement of organic solvent gas, which could lead to material waste and safety risks.
[0008] Preferably, the device for removing water from organic solvents according to the present invention is characterized in that the oil-water phase separator A and the oil-water phase separator B are connected in parallel in series via pipelines, and their internal structures are identical, with corresponding components having the same height. The purpose of this design is to allow the mixed phase to undergo rapid two-stage separation, avoiding or minimizing the return of the aqueous phase to the distillation column.
[0009] Preferably, the device for removing water from organic solvents according to the present invention is characterized in that the middle position of the oil-water phase separator A and the middle position of the oil-water phase separator B are provided with the same fluid disperser, a wave-damping plate is provided in the upper middle part, and a settling plate is provided in the lower middle part. The purpose of this design is also to prevent fluctuations during the oil-water separation process, promote the rising of the oil phase and the sinking of the water phase, and achieve rapid separation of the oil and water phases.
[0010] Preferably, the device for removing water from organic solvents according to the present invention is characterized in that the top height of the inverted U-shaped bend is the same as the height of the oil phase outlet at the top of oil-water separator A and the oil phase outlet at the top of oil-water separator B. This design aims to prevent the oil phase level from falling below the oil phase outlet height, thereby improving separation efficiency.
[0011] Preferably, the device for removing moisture from organic solvents according to the present invention is characterized in that a pressure balance pipe is connected to the top of the inverted U-shaped bend, and the pressure balance pipe is connected to the atmosphere. This design aims to prevent the inverted U-shaped bend from acting as a siphon, thus avoiding the complete discharge of the liquid from the oil-water separator due to siphon action.
[0012] The device for removing water from organic solvents described in this utility model has four significant beneficial effects: (1) The design of the settling device can effectively avoid gas-liquid entrainment or flooding during the distillation process, which is very beneficial to product purity and process safety; (2) The use of a crude product condenser with a large heat exchange area can quickly condense the mixed gas, thereby effectively avoiding material loss and safety risks; (3) The combination of oil-water phase separator A and oil-water phase separator B can promote the rapid and thorough separation of the oil phase and the water phase; (4) The combination of the reverse U-shaped bend and the pressure balance pipe can effectively prevent material loss, thereby achieving safe production process and orderly and controllable production process. Attached Figure Description
[0013] To more clearly illustrate the technical solutions in the embodiments of this utility model or the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are only some embodiments of this utility model. For those skilled in the art, other drawings can be obtained based on these drawings.
[0014] Figure 1 In the middle section: Distillation kettle 01, Distillation column 02, Reboiler 03, Settling tank 04, Crude product condenser 05, Forward mixed phase inlet 06, Oil-water phase separator A 07, Oil-water phase separator B 08, Forward oil phase outlet 09, After-mixed phase inlet 10, After-oil phase outlet 11, Water-containing agent transfer tank 12, Water-containing agent metering tank 13, Circulating pump 14, Flow meter 15, Drainage tank 16, Qualified product condenser 17, Online detection sampling point 18. Non-conforming product control valve 191, conforming product control valve 192, conforming product receiving tank 19, crude product storage tank 20, crude product feeding pump 21, crude product spray head 22, steam inlet 23, steam trap 24, reverse U-bend 25, pressure balancing pipe 26, wastewater outlet 27, fluid distributor 28, material inlets 51 and 171, material outlets 52 and 172, cooling water inlets 53 and 173, cooling water outlets 54 and 174. Detailed Implementation
[0015] To make the objectives, technical solutions, and advantages of this utility model clearer, the following description is provided in conjunction with... Figure 1 The specific embodiments of this implementation will be further described.
[0016] This specific embodiment describes an apparatus for removing moisture from organic solvents, comprising: a distillation kettle 01, a distillation column 02, a reboiler 03, a settling tank 04, a crude product condenser 05, a pre-mixed phase inlet 06, an oil-water phase separator A 07, an oil-water phase separator B 08, a pre-oil phase outlet 09, a post-mixed phase inlet 10, a post-oil phase outlet 11, a water-carrying agent transfer tank 12, a water-carrying agent metering tank 13, a circulating pump 14, a flow meter 15, a diversion trough 16, and a qualified product cooler. The components include: condenser 17, online sampling point 18, non-conforming product control valve 191, conforming product control valve 192, conforming product receiving tank 19, crude product storage tank 20, crude product feeding pump 21, crude product spray head 22, steam inlet 23, steam trap 24, reverse U-bend 25, pressure balance pipe 26, wastewater outlet 27, fluid distributor 28, material inlets 51 and 171, material outlets 52 and 172, cooling water inlets 53 and 173, and cooling water outlets 54 and 174. The organic combination of these components effectively removes some of the moisture from the organic solvent that azeotropically reacts with water.
[0017] Furthermore, the apparatus for removing water from organic solvents described in this specific embodiment is characterized in that a reboiler 03 is provided inside the distillation kettle 01, the distillation column 02 is located directly above the distillation kettle 01, a settling device 04 is provided between the bottom of the distillation column 02 and the distillation kettle 01, the top of the distillation column 02 is connected to an oil-water phase separator A07 via a pipe and a crude product condenser 05, the front oil phase outlet 09 at the top of the oil-water phase separator A07 is connected to the rear mixed phase inlet 10 in the middle of the oil-water phase separator B08, the rear oil phase outlet 11 at the top of the oil-water phase separator B08 is connected to a water-carrying agent transfer tank 12, and the water-carrying agent transfer tank 12 is connected to a water-carrying agent transfer tank 12 via a pipe. A water-based metering tank 13 is connected to the distillation column 02 via a circulating pump 14 at its bottom. A fluid distributor 28 is installed at the top of the distillation column 02. The oil-water separators A07 and B08 are connected at their bottoms and connected to the wastewater outlet 27 via pipes and a reverse U-bend 25. A diversion channel 16 is located in the middle of the distillation column 02 and is connected to the qualified product condenser 17 via pipes. An online sampling point 18, a non-conforming product control valve 191, and a qualified product control valve 192 are installed at the front end of the material outlet 172 of the qualified product condenser 17. The qualified product control valve 192 is connected forward to the qualified product receiving tank 19. The above-mentioned components are organically combined to effectively remove water from the organic solvent that azeotropically reacts with water.
[0018] Furthermore, the device for removing moisture from organic solvents described in this specific embodiment is characterized in that the settler, disposed between the bottom of the distillation column and the distillation kettle, is spherical, ellipsoidal, or cylindrical in shape, and its diameter is 1.5-2.5 times the diameter of the distillation column. This design aims to prevent gas-liquid entrainment or flooding caused by overheating during distillation, ensuring product purity and process safety.
[0019] Furthermore, the device for removing moisture from organic solvents described in this specific embodiment is characterized in that the crude product condenser is composed of 2-4 spiral plate condensers with a heat exchange area of 100 m² connected in parallel, or 2-4 shell-and-tube condensers connected in parallel, with a heat exchange area of 200-400 m². The purpose of this design is to ensure rapid condensation of the mixed gas exiting the distillation column, preventing the organic solvent gas from shifting downstream, thus avoiding material waste and safety risks.
[0020] Furthermore, in this specific embodiment of the apparatus for removing water from organic solvents, the oil-water phase separator A and the oil-water phase separator B are connected in parallel in series via pipelines. Both have identical internal structures and the same height for each component. This design aims to allow the mixed phase to undergo rapid two-stage separation, avoiding or minimizing the return of the aqueous phase to the distillation column.
[0021] Furthermore, in the specific embodiment of this device for removing water from organic solvents, the fluid disperser is identical to that in the middle of the oil-water phase separator A and the middle of the oil-water phase separator B, with a wave-damping plate in the upper middle and a settling plate in the lower middle. This design aims to prevent fluctuations during oil-water separation, promote the rising of the oil phase and the settling of the water phase, and achieve rapid separation of the oil and water phases.
[0022] Furthermore, in this specific embodiment of the apparatus for removing water from organic solvents, the top height of the inverted U-shaped bend is the same as the height of the oil phase outlet at the top of oil-water separator A and the oil phase outlet at the top of oil-water separator B. This design aims to prevent the oil phase level from falling below the oil phase outlet height, thereby improving separation efficiency.
[0023] Furthermore, in this specific embodiment of the apparatus for removing moisture from organic solvents, the top of the inverted U-shaped bend is connected to a pressure balance pipe, which is connected to the atmosphere. This design aims to prevent the inverted U-shaped bend from acting as a siphon, thus avoiding the complete discharge of the liquid from the oil-water separator due to siphoning.
[0024] Furthermore, the device for removing water from organic solvents described in this specific embodiment has the following simple operating procedure: First, check the closed status of the corresponding pipes and valves in the distillation system, inject the organic solvent-water mixture into the distillation kettle 01, start the reboiler 03, and when the temperature at the top of the column rises to the azeotropic point, start the circulation pump 14 according to the process specifications, so that the water-carrying agent is transported from the water-carrying agent transfer tank 12 to the top of the column through the flow meter 15, and then evenly sprayed from top to bottom through the fluid distributor 28 at the top of the column. A certain flow rate of water-carrying agent enters the distillation column 02, forming a "organic solvent-water-water-carrying agent" mixed phase. This three-phase mixture passes through the crude product condenser 05 at the top of the column and then sequentially enters the oil-water phase separators A07 and B08 for orderly oil-water phase separation. The oil phase, composed of "water-carrying agent + organic solvent," enters the water-carrying agent transfer tank 12, and is then transferred by the circulating pump 14 to the fluid distributor 28 at the top of the column, flowing downwards in a continuous cycle. The wastewater separated from oil-water phase separators A and B... Under the combined action of the reverse U-shaped bend 25 and the pressure balance pipe 26, the mixture is discharged in an orderly manner, maintaining a balance between the inflow of the mixed phase and the outflow of the oil and water phases throughout the entire oil-water phase separation process. When the online detection port 18 displays a message indicating that the moisture content is ≤0.5% and the content of the organic solvent to be purified is ≥99.5%, the qualified product receiving control valve 192 is opened and the unqualified product control valve 191 is closed. This allows the nearly anhydrous organic solvent to be condensed and cooled by the qualified product condenser 17 before being collected. The product is received in tank 19; during the operation process, the replenishment rate of the pure product containing water is controlled to maintain the balance between the loss and replenishment; the separated wastewater is discharged through the lower part of oil-water separator A and oil-water phase separator B via reverse U-shaped bend 25; in this way, crude organic solvent is continuously fed, qualified organic solvent is continuously extracted, and wastewater flows out at a constant rate, thus forming a continuous azeotropic distillation dehydration mode, which can continuously obtain high-quality organic solvent with a moisture content ≤0.5% and a main content ≥99.5%.
[0025] The device described in this utility model for removing water from organic solvents has four significant beneficial effects: (1) The design of the settling device can effectively avoid gas-liquid entrainment or flooding during the distillation process, which is very beneficial to product purity and process safety; (2) The use of a crude product condenser with a large heat exchange area can quickly condense the mixed gas, thereby effectively avoiding material loss and safety risks; (3) The combination of oil-water phase separator A and oil-water phase separator B can promote the rapid and thorough separation of the oil phase and the water phase; (4) The combination of the reverse U-shaped bend and the pressure balance pipe can effectively prevent material loss, thereby achieving safe production process and orderly and controllable process.
[0026] This device, as described in the present invention, is a device for removing moisture from organic solvents. It also has the advantages of reasonable layout, convenient operation, high production efficiency, stable production process, and safe and reliable operation.
[0027] Any modifications, equivalent substitutions, or improvements made within the spirit and principles of this utility model shall be included within the protection scope of this utility model. The protection scope of this utility model shall conform to the widest range consistent with the principles and novel features described herein.
Claims
1. An apparatus for removing moisture from an organic solvent comprising: The rectification kettle, rectification tower, reboiler, settler, fluid distributor, crude product condenser, front mixed phase inlet, oil-water separator A, oil-water separator B, front oil phase outlet, rear mixed phase inlet, rear oil phase outlet, water carrying agent transfer tank, water carrying agent metering tank, circulating pump, flow meter, drainage groove, qualified product condenser, online detection sampling point, unqualified product control valve, qualified product control valve, qualified product receiving tank, crude product storage tank, crude product feeding pump, crude product spray head, reverse U-shaped bend, pressure balance pipe, wastewater outlet, characterized in that the reboiler is arranged in the rectification kettle, the rectification tower is arranged directly above the rectification kettle, the settler is arranged between the bottom of the rectification tower and the rectification kettle, the top of the rectification tower is connected with the oil-water separator A through a pipe and a crude product condenser, the front oil phase outlet at the upper part of the oil-water separator A is connected with the rear mixed phase inlet at the middle part of the oil-water separator B, the rear oil phase outlet at the upper part of the oil-water separator B is connected with the water carrying agent transfer tank, the water carrying agent transfer tank is connected with the water carrying agent metering tank through a pipe, the bottom of the water carrying agent transfer tank is connected with the top of the rectification tower through a circulating pump, the fluid distributor is arranged at the top of the rectification tower, the oil-water separator A and the oil-water separator B are connected together at the bottom and connected with the wastewater outlet through a pipe and a reverse U-shaped bend, the drainage groove is arranged in the middle part of the rectification tower and connected with the qualified product condenser through a pipe, the online detection sampling point, the unqualified product control valve and the qualified product control valve are arranged at the front end of the material outlet of the qualified product condenser, and the qualified product control valve is connected with the qualified product receiving tank.
2. The apparatus for removing moisture from an organic solvent according to claim 1, wherein The settler arranged between the bottom of the rectification tower and the rectification kettle is in the shape of a sphere, an ellipsoid or a cylinder, and the diameter of the settler is 1.5-2.5 times the diameter of the rectification tower.
3. The apparatus for removing moisture from an organic solvent according to claim 1, wherein The rough product condenser is composed of 2-4 spiral plate condensers with heat exchange area of 100m 2 2, or 2-4 columnar condensers with heat exchange area of 200-400m2.
4. The apparatus for removing moisture from an organic solvent of claim 1, wherein, The oil-water separator A and the oil-water separator B are connected together in parallel in a pipe series mode, and the internal structures of the two are the same, and the heights of the corresponding components are the same.
5. The apparatus for removing moisture from an organic solvent of claim 1, wherein The middle parts of the oil-water separator A and the oil-water separator B are provided with the same fluid distributor, the middle upper parts are provided with wave blocking plates, and the middle lower parts are provided with settling plates.
6. The apparatus for removing moisture from an organic solvent of claim 1, wherein, The top of the reverse U-shaped bend is at the same height as the front oil phase outlet at the upper part of the oil-water separator A and the rear oil phase outlet at the upper part of the oil-water separator B.
7. The apparatus for removing moisture from an organic solvent of claim 1, wherein, The top of the reverse U-shaped bend is connected with the pressure balance pipe, and the pressure balance pipe is connected with the atmosphere.