Reduced pressure distillation collecting device

Abstract

The utility model relates to a reduced pressure distillation collecting device, belongs to the technical field of reduced pressure distillation, and solves the problems that the existing reduced pressure distillation collecting device is low in cooling efficiency, low in energy utilization rate, insufficient in operation automation degree, poor in condenser stability and to-be-improved in system safety. According to the device, on the basis of traditional water bath cooling, a cooling device and a cooling liquid circulating system are additionally arranged, an electronic thermometer and automatic control are combined, and a vacuum buffer tank fixed by a fixed stand column and protected by an intelligent switch is adopted, so that the cooling efficiency and the energy use are optimized. Through the improvements, the stability of the condenser is enhanced, the operation automation is realized, the system safety is improved, meanwhile, the product yield is remarkably improved by reducing fraction volatilization and guaranteeing the sample purity, and the wide application potential is shown.

Description

Technical Field

[0001] This utility model relates to the field of vacuum distillation technology, and in particular to a vacuum distillation collection device. Background Technology

[0002] With the continuous development of the chemical industry and the increasing advancement of laboratory technology, vacuum distillation, as a highly efficient separation technique, has been widely used in fields such as chemical synthesis, drug extraction, and essential oil separation. It achieves the separation and purification of heat-sensitive or low-boiling-point compounds by reducing the pressure within the system, causing the liquid to boil at a temperature below its normal boiling point.

[0003] However, existing vacuum distillation collection devices present some challenges when processing low-boiling fractions. Under prolonged vacuum conditions, low-boiling fractions may volatilize due to overheating, reducing product yield. Existing devices typically do not adequately consider the cooling of the fraction receiving flask, which may heat up during distillation, exacerbating fraction volatilization.

[0004] To address this issue, some laboratories and industrial production processes have employed methods such as water baths or ice-water baths to lower the temperature of the distillation receiving flasks. However, these methods fail to provide uniform cooling and are limited by the water temperature or the melting point of ice, resulting in insufficient cooling, especially during prolonged distillation processes, where rapid cooling is difficult and increases the risk of overheating and volatilization of the distillate. Utility Model Content

[0005] Based on the above analysis, the present invention aims to provide a vacuum distillation collection device to solve the problem that existing vacuum distillation collection devices may cause product volatilization and low product yield due to insufficient cooling effect when collecting low-boiling-point fractions.

[0006] The objective of this utility model is mainly achieved through the following technical solutions:

[0007] The present invention provides a vacuum distillation collection device, including a vacuum distillation apparatus, a low-temperature circulation apparatus and a vacuum pump. The vacuum distillation apparatus includes a distillation flask, a straight condenser connected to the mouth of the distillation flask, a fraction receiving flask connected to the outlet of the straight condenser, and a cooling device disposed below the fraction receiving flask.

[0008] The low-temperature circulation equipment includes a low-temperature circulation equipment inlet and a low-temperature circulation equipment outlet; the low-temperature circulation equipment draws coolant from the low-temperature circulation equipment outlet through pipelines, passing it successively through a straight condenser tube and a cooling device, and finally returning it to the low-temperature circulation equipment inlet;

[0009] The cooling device is placed in a water basin and achieves cooling through a water bath.

[0010] Furthermore, the cooling device comprises one or more cooling elements, including but not limited to cooling coils or cooling plates, all equipped with internal flow channel designs; the cooling coils are spiral coils or serpentine coils; the cooling plates are disc-shaped plates, which may be disc-shaped plates without through holes or with through holes.

[0011] Furthermore, an electronic thermometer is installed inside the water basin, and the electronic thermometer is connected to the temperature controller of the low-temperature circulation equipment.

[0012] Furthermore, the cooling device includes at least one fixed column and a fixed block. The side of the fixed column is fixedly connected to the side of the cooling device, the bottom of the fixed column is fixedly connected to the upper surface of the fixed block, and the lower surface of the fixed block is fixedly connected to the bottom of the water basin.

[0013] Furthermore, the fraction receiving flask is connected to a horn tube and a straight condenser tube; the horn tube is equipped with a horn tube vacuum interface.

[0014] Furthermore, the vacuum pump is connected to the horn-shaped vacuum interface via a pipeline for vacuuming and pressure reduction.

[0015] Furthermore, the vacuum pump includes a vacuum buffer tank, the top of which is provided with a vacuum buffer tank outlet, and the vacuum buffer tank outlet is connected to the horn tube vacuum interface through a pipeline; the vacuum buffer tank outlet is equipped with a vacuum buffer tank smart switch, which automatically shuts off when the vacuum pump is damaged or the power is cut off.

[0016] Furthermore, the straight condenser tube has a straight condenser tube inlet and a straight condenser tube outlet. Coolant flows in from the straight condenser tube inlet, passes through the inside of the condenser tube, and flows out from the straight condenser tube outlet.

[0017] Furthermore, the cooling device has a cooling device inlet and a cooling device outlet. Coolant flows in from the cooling device inlet, passes through the interior of the cooling device, and flows out from the cooling device outlet.

[0018] Furthermore, the liquid outlet of the low-temperature circulation equipment is connected to the liquid inlet of the straight condenser tube by a pipeline, the liquid outlet of the straight condenser tube is connected to the liquid inlet of the cooling device by a pipeline, and the liquid outlet of the cooling device is connected to the liquid inlet of the low-temperature circulation equipment by a pipeline.

[0019] Compared with the prior art, the present invention can achieve at least one of the following beneficial effects:

[0020] 1. The vacuum distillation collecting device of this utility model adds a cooling device to the traditional water bath. On the basis of water bath cooling, the cooling liquid in the cooling device can further cool the distillate. The contact between the cooling liquid and the distillate receiving bottle is more uniform, which improves the cooling efficiency, reduces the volatilization of the distillate, and increases the product yield.

[0021] 2. The vacuum distillation collection device of this utility model takes into account the recycling of coolant. The coolant is first cooled by a straight condenser tube, and then further cooled by a cooling device. This cooling method of multiple uses not only improves cooling efficiency, but also improves energy utilization by recycling coolant.

[0022] 3. This utility model's vacuum distillation collection device, through the combination of an electronic thermometer and an automatic temperature control system, achieves precise control of the coolant temperature, effectively preventing distillate evaporation. This design significantly improves the automation level of operation and process safety, while reducing the need for manual monitoring.

[0023] 4. The cooling device of this utility model forms a stable structure by setting fixed columns in four directions and connecting them with fixed blocks and water basins. This fixed structure enhances the stability and durability of the condenser, thereby improving the overall performance of the vacuum distillation collection device.

[0024] 5. The vacuum distillation collection device of this utility model is equipped with a vacuum buffer tank, and its top outlet is equipped with an intelligent switch that can automatically shut off when the vacuum pump fails, so as to maintain the system pressure balance, effectively prevent liquid backflow, ensure that the sample is not contaminated, and significantly improve the safety and reliability of the system.

[0025] In this invention, the above-described technical solutions can be combined with each other to achieve more preferred combinations. Other features and advantages of this invention will be set forth in the following description, and some advantages will become apparent from the description or be learned by practicing this invention. The objectives and other advantages of this invention can be realized and obtained from the details specifically pointed out in the text and accompanying drawings. Attached Figure Description

[0026] The accompanying drawings are for illustrative purposes only and are not intended to limit the scope of the invention. Throughout the drawings, the same reference numerals denote the same parts.

[0027] Figure 1 This is a schematic diagram of the vacuum distillation equipment in the device of this utility model;

[0028] Figure 2 This is a schematic diagram of the low-temperature circulation equipment in the device of this utility model;

[0029] Figure 3 This is a schematic diagram of the vacuum pump in the device of this utility model;

[0030] Figure 4a This is a front view of the fixed structure of the cooling device;

[0031] Figure 4b This is a top view of the fixed structure of the cooling device;

[0032] Figure 5 This is a schematic diagram of the vacuum buffer tank in the device of this utility model;

[0033] Figure 6 This is a schematic diagram of the pipeline connection of the novel device in this experiment.

[0034] Figure 7 This is a top view of the cooling plate of the device of this utility model; where (a) and (b) are two layouts of the internal flow channels.

[0035] Figure label:

[0036] 1-Low-temperature circulation equipment; 2-Low-temperature circulation equipment outlet; 3-Low-temperature circulation equipment inlet; 4-Constant-temperature heating magnetic stirrer; 5-Distillation flask; 6-Straight condenser tube outlet; 7-Straight condenser tube; 8-Straight condenser tube inlet; 9-Cooling device outlet; 10-Cooling device inlet; 11-Cooling device; 12-Friction receiving flask; 13-Bullhorn tube vacuum interface; 14-Vacuum pump; 15-Vacuum pump interface; 16-Water basin; 17-Distillation head; 18-Distillation head inlet; 19-Distillation head outlet; 20-Vacuum buffer tank outlet; 21-Vacuum buffer tank intelligent switch; 22-Vacuum buffer tank; 23-First fixed column; 24-Second fixed column; 25-Third fixed column; 26-Fourth fixed column; 27-Fixing block; 28-Internal flow channel. Detailed Implementation

[0037] The preferred embodiments of the present invention will now be described in detail with reference to the accompanying drawings, which constitute a part of this application and are used together with the embodiments of the present invention to illustrate the principles of the present invention, but are not intended to limit the scope of the present invention.

[0038] A specific embodiment of this utility model discloses a vacuum distillation collection device, including a vacuum distillation apparatus, a low-temperature circulation apparatus 1, and a vacuum pump 14.

[0039] Vacuum distillation equipment such as Figure 1As shown, it includes a distillation flask 5, a straight condenser 7 connected to the mouth of the distillation flask 5, a fraction receiving flask 12 connected to the outlet of the straight condenser 7, and a cooling device 11 disposed below the fraction receiving flask 12; the cooling device 11 is disposed in a water basin 16, which can be made of stainless steel or other suitable materials, and is used to achieve cooling by water bath.

[0040] Furthermore, to optimize cooling performance, the cooling device 11 consists of one or more cooling elements, which can be in the form of cooling coils or cooling plates, and are all equipped with internal flow channels 28 for more efficient heat exchange. The cooling coils are spiral coils or serpentine coils; the cooling plates are disc-shaped plates, which may or may not have through holes. Figure 7 The middle section shows two layout options for the internal flow channels 28 of the cooling plate.

[0041] Preferably, the cooling coil adopts a finned design. This finned structure increases the heat dissipation area and significantly improves heat transfer efficiency. Therefore, while achieving the same cooling effect, the finned tube occupies less space, saving space while ensuring cooling efficiency.

[0042] In one embodiment, the cooling plate is disposed parallel to the bottom of the water basin 16, and its periphery is parallel to the inner wall of the water basin 16.

[0043] Specifically, the distillation flask 5 is used to hold the sample to be distilled. The straight condenser 7 is used to guide the vapor from the distillation flask 5. The fraction receiving flask 12 is used to receive the condensed fraction. The cooling device 11 is used to cool the fraction receiving flask 12.

[0044] Compared with traditional water bath cooling technology, the present invention adds a cooling device 11 to the water bath cooling technology. The cooling liquid in the cooling device 11 further cools the distillate, and the contact between the cooling liquid and the distillate receiving bottle 12 is more uniform, which improves the cooling efficiency, reduces the volatilization of the distillate, and improves the product yield.

[0045] The cryogenic circulation device 1 is as follows Figure 2 As shown, it includes a cryogenic circulation equipment inlet 3 and a cryogenic circulation equipment outlet 2; the cryogenic circulation equipment 1 draws coolant from the cryogenic circulation equipment outlet 2 through pipelines, passing through a straight condenser 7 and a cooling device 11, and finally returns to the cryogenic circulation equipment inlet 3, thus completing the purpose of cooling circulation.

[0046] Compared to the single-stage cooling method commonly used in traditional technologies, the low-temperature circulating equipment of the present invention performs two-stage cooling by having the coolant flow sequentially through the straight condenser 7 and the cooling device 11. This not only enhances the cooling effect but also significantly improves energy efficiency and operational economy by recycling the coolant.

[0047] Furthermore, an electronic thermometer is installed in the water basin 16. The electronic thermometer is connected to the temperature controller of the low-temperature circulation device 1. When the temperature of the coolant in the water basin 16 exceeds the set value, the low-temperature circulation device 1 is triggered to increase the cooling efficiency, so as to maintain the stable temperature of the coolant and prevent the distillate in the distillate receiving bottle 12 from evaporating.

[0048] Furthermore, the fixing structure of the cooling device 11 is as follows: Figure 4a , 4b As shown, it includes at least one fixed column and a fixing block 27. The side of the fixed column is fixedly connected to the side of the cooling device 11, the bottom end of the fixed column is fixedly connected to the upper surface of the fixing block 27, and the lower surface of the fixing block 27 is fixedly connected to the bottom of the water basin 16 to form a stable support structure. The fixing connection methods include, but are not limited to, welding, gluing, and mechanical fastening.

[0049] Preferably, there are four fixed columns: a first fixed column 23, a second fixed column 24, a third fixed column 25, and a fourth fixed column 26. The first fixed column 23, the second fixed column 24, the third fixed column 25, and the fourth fixed column 26 are arranged in a four-sided symmetrical manner around the cooling device 11, meaning that the four fixed columns are located at the four corners of a rectangle, square, or rhombus, respectively. This layout can provide stable support and ensure the balanced distribution of the weight of the cooling device 11.

[0050] Furthermore, the vacuum distillation apparatus also includes a constant-temperature heating magnetic stirrer 4, positioned below the distillation flask 5, for heating the distillation flask 5 to cause the sample in the distillation flask 5 to evaporate due to heat. The distillation flask 5 is equipped with a distillation head 17, which has a distillation head inlet 18 and a distillation head outlet 19. The distillation head inlet 18 is inserted into the mouth of the distillation flask 5, and the distillation head outlet 19 is connected to the inlet of the straight condenser tube 7.

[0051] Furthermore, the fraction receiving bottle 12 is connected to the straight condenser tube 7 via a horn tube; the horn tube is provided with a horn tube vacuum interface 13.

[0052] Furthermore, the vacuum pump 14 as... Figure 3 As shown, the vacuum pump interface 15 is connected to the horn-shaped tube vacuum interface 13 via a pipeline for vacuuming and depressurization. By maintaining a low-pressure environment, the sample evaporates at a lower temperature, avoiding thermal decomposition or degradation that may occur at high temperatures.

[0053] Furthermore, the vacuum pump 14 includes a vacuum buffer tank 22, such as Figure 5As shown. The top of the vacuum buffer tank 22 is provided with a vacuum buffer tank outlet 20, and the outlet is connected to the horn tube vacuum interface 13 through a pipeline; the vacuum buffer tank outlet 20 is equipped with a vacuum buffer tank smart switch 21, which automatically closes when the vacuum pump 14 is damaged or the power is cut off.

[0054] This design ensures pressure balance within the system in the event of sudden failure or power loss of the vacuum pump 14. It effectively prevents backflow of liquid within the vacuum pump 14, thus protecting the samples in the system from contamination.

[0055] Furthermore, the straight condenser 7 includes an inner steam tube and an outer coolant tube sleeved outside the inner steam tube. The inner steam tube is used to guide steam from the distillation flask 5, and the outer coolant tube is used to flow coolant.

[0056] Furthermore, the straight condenser tube 7 has a straight condenser tube inlet 8 and a straight condenser tube outlet 6. Coolant flows in from the straight condenser tube inlet 8, passes through the inside of the condenser tube, and flows out from the straight condenser tube outlet 6.

[0057] The inlet of the straight condenser tube 7 is designed to be at a lower position, while the outlet is at a higher position. This design helps to form a stable counter-current heat exchange, allowing the coolant in the condenser tube to come into more full contact with the steam and improve condensation efficiency.

[0058] Furthermore, the cooling device 11 has a cooling device inlet 10 and a cooling device outlet 9. Coolant flows in from the cooling device inlet 10, passes through the interior of the cooling device 11 to cool the condenser, and flows out from the cooling device outlet (9) to re-enter the low-temperature circulation equipment 1.

[0059] Specifically, the coolant enters from the bottom of the cooling device 11 and flows upwards, forming a counter-current heat exchange. This flow pattern enhances the contact between the coolant and the inner wall of the condenser, improving heat exchange efficiency. Through this mechanism, the temperature of the cooling device 11 decreases, thereby cooling the water in the water basin 16. Ultimately, the temperature of the fraction receiving flask 12 is reduced, decreasing fraction evaporation and improving collection efficiency and product yield.

[0060] Furthermore, such as Figure 6 As shown, the liquid outlet 2 of the low-temperature circulation equipment is connected to the liquid inlet 8 of the straight condenser tube by a pipeline, the liquid outlet 6 of the straight condenser tube is connected to the liquid inlet 10 of the cooling device by a pipeline, and the liquid outlet 9 of the cooling device is connected to the liquid inlet 3 of the low-temperature circulation equipment by a pipeline.

[0061] During vacuum distillation, the sample is placed in distillation flask 5 and heated simultaneously by a thermostatically heated magnetic stirrer 4, evaporating the sample into a gas. The gas condenses into a liquid in a straight condenser 7 and flows into a fraction receiving flask 12. The fraction receiving flask 12 is cooled by a cooling device 11. During this process, a vacuum pump 14 continuously evacuates the system to reduce pressure, and a cryogenic circulation device 1 is continuously turned on to circulate and cool the coolant.

[0062] Compared with existing technologies, the vacuum distillation collection device provided in this embodiment achieves a more efficient cooling effect by integrating a cooling device 11 into the fraction receiving flask 12, based on the traditional water bath. The cooling device 11 ensures more uniform contact between the coolant and the fraction receiving flask 12, significantly improving cooling efficiency. The multiple cooling processes of the straight condenser 7 and the cooling device 11, as well as the recycling of the coolant, further improve energy efficiency. This design is particularly suitable for vacuum distillation of low-boiling-point samples, effectively preventing fraction evaporation caused by prolonged vacuum, ensuring experimental yield, and improving product quality and output.

[0063] The above description is only a preferred embodiment of the present utility model, but the protection scope of the present utility model is not limited thereto. Any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope disclosed in the present utility model should be included within the protection scope of the present utility model.

Claims

1. A reduced pressure distillation collection apparatus, characterized by, The device comprises a reduced pressure distillation device, a low-temperature circulation device (1) and a vacuum pump (14), The reduced pressure distillation device comprises a distillation flask (5), a straight condenser tube (7) connected with the mouth of the distillation flask (5), a fraction receiving flask (12) connected with the outlet of the straight condenser tube (7), and a cooling device (11) arranged below the fraction receiving flask (12). The low-temperature circulation device (1) comprises a low-temperature circulation device liquid inlet (3) and a low-temperature circulation device liquid outlet (2); the low-temperature circulation device (1) returns the cooling liquid from the low-temperature circulation device liquid outlet (2) to the low-temperature circulation device liquid inlet (3) through the straight condenser tube (7) and the cooling device (11) in sequence. The cooling device (11) is arranged in a water basin (16) and cooled by water bath.

2. The reduced pressure distillation collection apparatus according to claim 1, wherein, The cooling device (11) is composed of one or more cooling elements, which include but are not limited to cooling coil or cooling disc, and are all equipped with internal flow channel (28) design; the cooling coil is spiral coil or serpentine coil; the cooling disc is disc-shaped plate, which is disc-shaped plate without or with through hole.

3. The reduced pressure distillation collection apparatus according to claim 1, wherein, An electronic thermometer is arranged in the water basin (16) and connected with the temperature controller of the low-temperature circulation device (1).

4. The reduced pressure distillation collection apparatus according to claim 2, wherein, The cooling device (11) comprises at least one fixed column and fixed block (27), the side surface of the fixed column is fixedly connected with the side surface of the cooling device (11), the bottom end of the fixed column is fixedly connected with the upper surface of the fixed block (27), and the lower surface of the fixed block (27) is fixedly connected with the bottom of the water basin (16).

5. The reduced pressure distillation collection apparatus according to claim 1, wherein, The fraction receiving flask (12) is connected with the straight condenser tube (7) through a horn tube, and the horn tube is provided with a horn tube vacuum interface (13).

6. The reduced pressure distillation collection apparatus according to claim 5, wherein, The vacuum pump (14) is connected with the horn tube vacuum interface (13) through a pipeline for vacuum pumping.

7. The reduced pressure distillation collection apparatus according to claim 6, wherein, The vacuum pump (14) comprises a vacuum buffer tank (22), the top of the vacuum buffer tank (22) is provided with a vacuum buffer tank gas outlet (20), the vacuum buffer tank gas outlet (20) is connected with the horn tube vacuum interface (13) through a pipeline, and the vacuum buffer tank gas outlet (20) is provided with a vacuum buffer tank intelligent switch (21) which is automatically closed when the vacuum pump (14) is damaged or powered off.

8. The reduced pressure distillation collection apparatus according to claim 1, wherein, The straight condenser tube (7) has a straight condenser tube liquid inlet (8) and a straight condenser tube liquid outlet (6), the cooling liquid flows into the straight condenser tube liquid inlet (8), passes through the inside of the condenser tube, and flows out of the straight condenser tube liquid outlet (6).

9. The reduced pressure distillation collection apparatus according to claim 8, wherein, The cooling device (11) has a cooling device liquid inlet (10) and a cooling device liquid outlet (9), the cooling liquid flows into the cooling device liquid inlet (10), passes through the inside of the cooling device (11), and flows out of the cooling device liquid outlet (9).

10. A reduced pressure distillation collection apparatus according to claim 9, wherein, The low-temperature circulation device liquid outlet (2) is connected with the straight condenser tube liquid inlet (8) through a pipeline, the straight condenser tube liquid outlet (6) is connected with the cooling device liquid inlet (10) through a pipeline, and the cooling device liquid outlet (9) is connected with the low-temperature circulation device liquid inlet (3) through a pipeline.

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