A distillation apparatus for difluoroethyl acetate

Abstract

The utility model discloses a kind of difluoroacetate rectifying devices including distillation tank, condensing tower and circulating pump group;The inside of the distillation tank is fixedly installed with web baffle, and its surface is evenly distributed with several heating components, and heating component includes resistance heating rod and the heat conduction sheet distributed on the surface of resistance heating rod;Safety valve and pressure gauge are provided at the top of distillation tank, for controlling the stable pressure in tank;The liquid inlet end of the circulating pump group is communicated with the inner cavity of the bottom of distillation tank, and the liquid outlet end is connected with spray pipe, and several atomizing nozzles are evenly installed on the surface of spray pipe, for realizing the redistribution and gas-liquid mass transfer enhancement of liquid.The device is through the synergic structure of "circulating spray+spiral heat conduction+high-efficiency condensation", realizes the rapid evaporation, sufficient mass transfer and stable condensation reflux of difluoroacetate, significantly improves rectification efficiency and product purity, with the advantages of low energy consumption, high thermal stability and safe and reliable operation.

Description

Technical Field

[0001] This utility model relates to the field of purification technology for fluorine-containing organic compounds, specifically a difluoroethyl acetate distillation apparatus. Background Technology

[0002] Difluoroethyl acetate is an important fluorinated organic compound widely used in pharmaceuticals, pesticides, and high-performance solvents. Due to its high volatility and certain thermal instability, distillation is typically employed during production to purify it, removing unreacted raw materials, low-boiling byproducts, and high-boiling impurities. However, traditional difluoroethyl acetate distillation units suffer from several shortcomings in structural design and thermal management, hindering further improvements in separation efficiency and product purity.

[0003] Currently, commonly used distillation equipment mainly includes basic units such as vertical distillation columns, reboiler, condensers, and external circulation pipelines. Traditional equipment typically uses bottom electric heating or external jacket heating to achieve material evaporation, with the condenser at the top of the column handling gas-liquid separation and reflux control. For example, some conventional equipment uses heating rods to directly heat the liquid, but the heating surface is limited, resulting in uneven heat conduction; other equipment uses hot oil circulation or electric heating mantles, which can improve temperature control accuracy, but in fluorine-containing organic systems, problems such as localized overheating and solution decomposition are prone to occur. In addition, conventional distillation columns mostly adopt a single upward airflow structure, with limited gas-liquid contact area, making it difficult to achieve sufficient mass transfer.

[0004] In the condensation and reflux stages, traditional condensers are often located outside the top of the column, resulting in slow gas condensation and uneven distribution of reflux liquid, leading to poor stability of the distillation process. At the same time, reflux regulation relies on manual operation, making it difficult to achieve automatic balance, resulting in high energy consumption and complex operation.

[0005] In view of this, this paper studies and improves the existing problems, and provides a difluoroethyl acetate distillation device to solve the current problems. The aim is to solve the problems and improve the practical value through this technology. Utility Model Content

[0006] This utility model aims to solve one of the technical problems existing in the prior art or related technologies.

[0007] Therefore, the technical solution adopted by this utility model is as follows: a distillation apparatus for difluoroethyl acetate, comprising a distillation tank, a condenser, and a circulating pump group. A mesh partition is installed inside the distillation tank, and several heating elements are evenly arranged on its surface; the heating elements consist of resistance heating rods and heat-conducting plates distributed on their surfaces.

[0008] After the liquid at the bottom of the distillation tank is drawn by the circulating pump group, it is redistributed through the spray pipe and several atomizing nozzles, so that the liquid is sprayed in the form of mist onto the heating zone, where it comes into full contact with the rising steam to form an enhanced mass transfer process.

[0009] Specifically, the design uses a "bottom circulation + upper atomization" method to ensure uniform heating of the liquid in the evaporation zone, significantly improving heat transfer efficiency and gas-liquid contact area, thereby achieving efficient distillation separation of difluoroethyl acetate under stable temperature control conditions.

[0010] In a preferred embodiment, the distillation vessel is further configured as follows: the distillation vessel is a vertical, sealed structure, and a safety valve and pressure gauge are installed on the top of the vessel to control the pressure inside the vessel and prevent overpressure caused by the high volatility of difluoroethyl acetate.

[0011] Specifically, through the linkage control of the safety valve and the pressure gauge, real-time pressure monitoring and automatic release can be achieved during operation to prevent solvent spraying or tank deformation, thereby improving the safety of system operation.

[0012] In a preferred embodiment, the mesh partition is further configured such that it is made of corrosion-resistant stainless steel wire mesh or Teflon-coated structure, and is used to support the heating assembly and separate the distillation zone from the liquid reflux zone.

[0013] Specifically, the structure has excellent resistance to acids, alkalis and fluorinated solvents, ensuring structural stability even under high temperature and highly polar environments, thereby extending the service life of the equipment and preventing contamination by impurities.

[0014] In a preferred embodiment, the resistance heating rod and the heat-conducting sheet are further configured as an integrated structure, with the heat-conducting sheet spirally distributed along the resistance heating rod, so that the atomized liquid forms a liquid film on the surface, promoting evaporation.

[0015] Specifically, a three-dimensional uniform heat distribution is achieved through a spiral heat-conducting structure, which avoids the decomposition of difluoroethyl acetate due to local high temperatures, while increasing the liquid's heat-receiving area and improving thermal energy utilization and evaporation rate.

[0016] In a preferred embodiment, the condensation tower is further configured as follows: the condensation tower is a vertical cylindrical structure with a condensation coil inside, and the outer wall of the coil has a cooling medium inlet and outlet.

[0017] Specifically, the condenser can achieve efficient condensation and reflux through a circulating cooling medium, which allows the vapor to be rapidly liquefied and redistributed to the distillation tank, thereby maintaining the gas-liquid balance of the system and improving the purity of the distillation.

[0018] In a preferred embodiment, the spray pipe may be a planar spiral structure or a ring structure, with a plurality of atomizing nozzles evenly distributed circumferentially on its surface to form a uniform droplet distribution.

[0019] Specifically, this atomization distribution structure can form a stable mist field in the distillation zone, promote the uniform mixing of reflux liquid and rising vapor, improve the mass transfer coefficient, and enhance the reaction stability and energy efficiency of the evaporation layer.

[0020] In a preferred embodiment, the circulating pump assembly is further configured such that it employs a corrosion-resistant magnetic pump structure, and the pump body material is a polytetrafluoroethylene liner or 316L stainless steel.

[0021] Specifically, the pump set features strong sealing, high corrosion resistance, and no mechanical leakage, which can effectively prevent fluorinated organic matter from corroding the pump body and ensure the stability and tightness of continuous system operation.

[0022] In a preferred embodiment, the distillation vessel is further configured such that an insulation layer is provided on the outside of the distillation vessel, and the insulation layer adopts a composite aluminum silicate fiber or vacuum insulation material structure.

[0023] Specifically, the insulation layer can effectively reduce heat loss, maintain a constant internal temperature in the distillation tank, further reduce energy consumption, and improve the thermal stability of difluoroethyl acetate.

[0024] The beneficial effects achieved by this utility model are as follows: 1. In this invention, a heating assembly consisting of a resistance heating rod and a spiral heat-conducting plate is installed inside the distillation tank. Combined with an atomizing spray system formed by a circulating pump and spray pipes, uniform heating of difluoroethyl acetate liquid and enhanced gas-liquid mass transfer are achieved. This structure can form a stable thin liquid film and micro-atomized droplets during evaporation, significantly improving the evaporation rate and separation efficiency, avoiding material decomposition caused by localized overheating, thereby achieving a distillation process with high energy utilization and efficient mass transfer.

[0025] 2. In this invention, a closed-loop system consisting of a condenser tower and a distillation tank, along with the coordinated control of a safety valve and pressure gauge at the top, achieves simultaneous regulation of gas-liquid circulation, condensation reflux, and system safety during the distillation process. This structure not only improves the purification accuracy and separation stability of difluoroethyl acetate but also effectively prevents solvent evaporation, energy loss, and overpressure risks, possessing comprehensive technical advantages of high efficiency, safety, energy saving, and strong applicability. Attached Figure Description

[0026] Figure 1 This is a schematic diagram of the overall structure of one embodiment of the present utility model; Figure 2 This is a schematic diagram of the cross-sectional structure of a distillation tank according to an embodiment of the present invention; Figure 3 This is a schematic diagram of the heating component structure according to an embodiment of the present invention; Figure 4 This is a schematic diagram of the structure of a spray pipe and its surface atomizing nozzle according to an embodiment of the present invention.

[0027] Figure label: 100. Distillation tank; 110. Mesh partition; 120. Heating assembly; 121. Resistance heating rod; 122. Heat-conducting plate; 200. Condensation tower; 300. Circulating pump set; 310. Spray pipe; 320. Atomizing nozzle. Detailed Implementation

[0028] To make the objectives, technical solutions, and advantages of this utility model clearer, the present utility model will be further described in detail below with reference to specific embodiments and accompanying drawings. It should be noted that, unless otherwise specified, the embodiments and features of the present utility model can be combined with each other.

[0029] It should be understood that these descriptions are merely exemplary and not intended to limit the scope of this invention.

[0030] The following describes, with reference to the accompanying drawings, some embodiments of the present invention, a difluoroethyl acetate distillation apparatus.

[0031] Combination Figures 1-4 As shown, the present invention provides a difluoroethyl acetate distillation apparatus, including a distillation tank 100, a condenser tower 200, and a circulating pump group 300.

[0032] Distillation tank 100 is used for heating, evaporating, and separating difluoroethyl acetate from impurities; condenser tower 200 is used for condensing and refluxing the vapor to achieve component separation and product purification; circulating pump set 300 is used for continuous liquid circulation and spray distribution within the device. This structure realizes automatic closed-loop operation of evaporation, atomization, condensation, and reflux.

[0033] like Figure 2 As shown, the distillation tank 100 is a vertical, closed structure. A safety valve and a pressure gauge are installed on the top of the tank to control the operating pressure inside the tank and prevent the risk of overpressure caused by the rapid evaporation of difluoroethyl acetate vapor, thereby ensuring the safety and stability of the equipment operation.

[0034] A mesh partition 110 is fixedly installed on the inner side of the distillation tank 100. The mesh partition 110 forms a gas-liquid partition structure to support the heating component 120 and enable sufficient mass transfer and heat exchange between the rising vapor and the reflux liquid in this area. The tank body is covered with an insulation layer to reduce heat loss, maintain a constant temperature environment inside the tank, and ensure the thermal stability of the distillation process.

[0035] like Figure 3As shown, the mesh partition 110 is made of corrosion-resistant stainless steel wire mesh or Teflon coating, and several heating components 120 are uniformly installed on its surface. The mesh partition 110 is used to support and fix the heating components 120, while allowing gas and liquid to pass freely to form a stable gas-liquid exchange surface.

[0036] The heating assembly 120 includes a resistance heating rod 121 and a heat-conducting plate 122 disposed on the outer surface of the resistance heating rod 121. The resistance heating rod 121 is the main heating element, and the heat-conducting plate 122 is spirally distributed along the heating rod to form a continuous heat-conducting channel.

[0037] During heating operation, a thin liquid film forms at the contact surface between the heat-conducting plate 122 and the atomized liquid, enabling the liquid to heat up rapidly and produce uniform micro-atomized evaporation, significantly improving the evaporation rate of difluoroethyl acetate. This structure achieves efficient energy utilization and avoids material decomposition caused by localized high temperatures.

[0038] like Figure 4 As shown, the circulating pump unit 300 is located at the bottom of the distillation tank 100, with its inlet end connected to the inner cavity of the distillation tank 100, and is used to draw liquid from the bottom of the tank. The circulating pump unit 300 adopts a corrosion-resistant magnetic pump structure, and the pump body material is polytetrafluoroethylene lining or 316L stainless steel to meet the chemical stability requirements of the difluoroethyl acetate system and prevent acidic impurities from causing equipment corrosion.

[0039] The outlet end of the circulating pump unit 300 is connected to a spray pipe 310. The spray pipe 310 can be a planar spiral structure or a circular structure, and its surface is uniformly arranged with several atomizing nozzles 320 along the circumference. When the circulating pump unit 300 is working, the liquid at the bottom of the tank is pressurized and sprayed out through the spray pipe 310, and then formed into fine droplets by the atomizing nozzles 320 and uniformly sprayed above the heating component 120.

[0040] This process enables the redistribution of liquid in the heating zone and enhances gas-liquid mass transfer, allowing steam and liquid to mix thoroughly and significantly improving evaporation uniformity and distillation efficiency.

[0041] like Figure 1 As shown, the condenser 200 is connected to the top of the distillation tank 100 and has a vertical cylindrical structure. The inside of the tower is equipped with a condenser coil. The outer wall of the condenser coil is provided with a cooling medium inlet and outlet. The cooling medium, such as circulating cooling water or ethanol refrigerant, flows in it to absorb the heat of the steam, causing the rising difluoroethyl acetate vapor to condense rapidly into liquid.

[0042] The condensed liquid flows back along the column wall to the interior of the distillation tank 100, where it forms a gas-liquid cycle with the atomized liquid at the bottom, thus achieving closed-loop reflux of the distillation system and product purification.

[0043] The outer surface of the distillation tank 100 is covered with an insulation layer. The insulation layer is made of composite aluminum silicate fiber or vacuum insulation material, which can effectively isolate external heat exchange, reduce energy loss, and maintain a stable internal temperature.

[0044] Meanwhile, the safety valve and pressure gauge at the top of the distillation tank 100 constitute a safety monitoring system. The safety valve can automatically release pressure when the pressure inside the tank exceeds the set value to prevent system overpressure; the pressure gauge displays the gas pressure status inside the tank in real time, making it convenient for operators to monitor the system operation.

[0045] Work process: During operation, crude difluoroethyl acetate solution is injected into distillation tank 100, and heating component 120 is started. The liquid gradually evaporates into gas under the combined action of resistance heating rod 121 and heat-conducting plate 122.

[0046] After the circulating pump group 300 is started, a portion of the liquid is drawn from the bottom of the tank and sent to the spray pipe 310. The liquid is atomized and sprayed out through the atomizing nozzle 320, forming a uniform droplet mist layer inside the tank. In the high-temperature environment inside the distillation tank 100, the evaporation efficiency is improved, and the gas-liquid contact in the evaporation zone is sufficient. The large droplets that condense fall onto the surface of the resistance heating rod 121 and the heat-conducting plate 122 to form a thin film, which fully exchanges heat with the resistance heating rod 121 and the heat-conducting plate 122, and quickly vaporizes and rises.

[0047] Gas-phase difluoroethyl acetate vapor rises and enters the condenser tower 200, where it is condensed into liquid and refluxed under the cooling effect of the condenser coil, achieving recycling and purification. High-boiling-point impurities remain at the bottom of the tank and gradually accumulate, thus completing the component separation.

[0048] In the description of this specification, the terms "one embodiment," "some embodiments," "specific embodiment," etc., refer to a specific feature, structure, material, or characteristic described in connection with that embodiment or example, which is included in at least one embodiment or example of the present invention. In this specification, the illustrative expressions of the above terms do not necessarily refer to the same embodiment or example. Furthermore, the specific features, structures, materials, or characteristics described may be combined in any suitable manner in one or more embodiments or examples.

[0049] Although embodiments of the present invention have been shown and described, those skilled in the art will understand that various changes, modifications, substitutions and alterations can be made to these embodiments without departing from the principles and spirit of the present invention, the scope of which is defined by the claims and their equivalents.

Claims

1. A difluoroethyl acetate distillation apparatus, characterized in that, The system includes a distillation tank (100), a condenser (200), and a circulating pump group (300). A mesh partition (110) is fixedly installed on the inner side of the distillation tank (100), and a number of heating components (120) are evenly distributed on the surface of the mesh partition (110). The heating components (120) include a resistance heating rod (121) and a number of heat-conducting plates (122) distributed on the surface of the resistance heating rod (121). The liquid inlet of the circulating pump group (300) is connected to the inner cavity at the bottom of the distillation tank (100), and the liquid outlet of the circulating pump group (300) is connected to a spray pipe (310). A number of atomizing nozzles (320) are evenly installed on the surface of the spray pipe (310) for realizing liquid redistribution and enhanced gas-liquid mass transfer during the distillation process.

2. The difluoroethyl acetate distillation apparatus according to claim 1, characterized in that, The distillation tank (100) is a vertical, sealed structure. A safety valve and a pressure gauge are installed on the top of the tank to control the pressure inside the tank and prevent overpressure caused by the rapid evaporation of difluoroethyl acetate vapor.

3. The difluoroethyl acetate distillation apparatus according to claim 1, characterized in that, The mesh partition (110) is made of corrosion-resistant stainless steel wire mesh or Teflon coating structure, used to support the heating assembly (120) and separate the distillation zone from the liquid reflux zone.

4. The difluoroethyl acetate distillation apparatus according to claim 1, characterized in that, The resistance heating rod (121) and the heat-conducting plate (122) are an integrated structure, and the heat-conducting plate (122) is spirally distributed along the resistance heating rod (121).

5. The difluoroethyl acetate distillation apparatus according to claim 1, characterized in that, The condensing tower (200) is a vertical cylindrical structure with a condensing coil inside the tower body. The outer wall of the condensing coil has a cooling medium inlet and outlet.

6. The difluoroethyl acetate distillation apparatus according to claim 1, characterized in that, The spray pipe (310) has a planar spiral structure or a circular structure, and a number of atomizing nozzles (320) are evenly arranged along the surface direction. Each atomizing nozzle (320) is connected to the inside of the spray pipe (310).

7. The difluoroethyl acetate distillation apparatus according to claim 1, characterized in that, The circulating pump set (300) adopts a corrosion-resistant magnetic pump structure, and its pump body material is polytetrafluoroethylene lining or 316L stainless steel.

8. The difluoroethyl acetate distillation apparatus according to claim 1, characterized in that, The distillation vessel (100) is provided with an external heat insulation layer, which is made of composite aluminum silicate fiber or vacuum insulation material.

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