Device for dehydrating and recovering excessive alcohol in esterification reaction

Abstract

The utility model relates to an esterification reaction excess alcohol dehydration recovery device which comprises a deacidification tower and a dehydration assembly, a feed port of the deacidification tower is communicated with a raw material pipe, the dehydration assembly is divided into an evaporator and a membrane filter, an input end of the evaporator is communicated with a discharge pipe of the deacidification tower, and an output pipe of the evaporator is communicated with the inside of the membrane filter. A drainage pipe is arranged on one side of the membrane filter; a heat compensation assembly is also arranged in the deacidification tower and is communicated with the interior of the evaporator through a pipeline; according to the application, the deacidified material is firstly heated by the evaporator to be in a gaseous state, then the deacidified material is pressurized by the heat pump and conveyed into the membrane filter, and water in the steam-state material is separated by the pervaporation membrane, so that the anhydrous alcohol product is obtained, the anhydrous alcohol steam can be effectively utilized for the second time, and the energy consumption is reduced. Therefore, only the heat pump needs to be powered, and in the process, the whole equipment can be maintained without shutdown, so that the recovery efficiency is greatly improved.

Description

Technical Field

[0001] This utility model relates to the field of pharmaceutical and chemical technology, specifically to a device for dehydrating and recovering excess alcohol from esterification reactions. Background Technology

[0002] In esterification reactions, excess alcohol is added to ensure complete reaction. After the product is extracted, this excess alcohol needs to be recycled. This alcohol contains water produced in the esterification reaction and a small amount of unreacted or hydrolyzed organic acids. During the recycling process, it is necessary to dehydrate and remove the organic acids.

[0003] Traditional treatment methods involve dehydration and acid removal using distillation columns, which consumes a large amount of steam and results in high recovery costs. In particular, methods that use alkali to neutralize acidity require not only filtering the solid precipitate in the recovery solution but also separating water and anhydrous alcohol. After prolonged operation, the equipment must be shut down periodically for cleaning or maintenance to prevent clogging caused by precipitation from acid-base neutralization, which would prevent the equipment from operating continuously and thus affect the overall recovery efficiency of the production equipment. Utility Model Content

[0004] Based on the above description, this utility model provides a device for dehydrating and recovering excess alcohol in esterification reaction, which solves the shortcomings of existing excess alcohol dehydration and recovery equipment that requires a large amount of steam, increases recovery costs, and cannot operate continuously, resulting in low recovery efficiency.

[0005] This utility model is achieved through the following technical solution:

[0006] An esterification reaction excess alcohol dehydration and recovery device includes a deacidification tower and a dehydration component. The feed inlet of the deacidification tower is connected to a raw material pipe. The interior of the dehydration component is divided into upper and lower layers by a partition, and an evaporator and a membrane filter are installed in the upper and lower layers respectively. The input end of the evaporator is connected to the discharge pipe of the deacidification tower, and the output pipe of the evaporator is connected to the interior of the membrane filter. A drain pipe is also provided on one side of the membrane filter. The deacidification tower is also equipped with a heating component, which is connected to the interior of the evaporator through a pipe.

[0007] Based on the above technical solution, the present invention can be further improved as follows.

[0008] Furthermore, the input end of the evaporator is also provided with a filter element, which is cylindrical and has an inverted conical filter element inside. The outer wall of the filter element is surrounded by several filter holes and covered with a filter membrane.

[0009] Further, the top of the filter core extends upward and is provided with an interface at the top end, the interface is in communication with the discharge pipe of the deacidification tower, the bottom of the filter core extends downward and is provided with a discharge pipe, the discharge pipe extends downward and is provided with a solenoid valve inside, and the input end of the evaporator is in communication with the side wall of the filter through a pipeline.

[0010] Further, the inside of the filter is further provided with a preheating pipe, the main body of the preheating pipe is arranged in a spiral shape and is arranged at the periphery of the filter core, one end of the preheating pipe is in communication with the inside of the evaporator, and the other end extends to the outside and is connected to the recovery container.

[0011] Further, the heat supplement assembly comprises a heat supplement device arranged on one side inside the dehydration assembly, the output end of the heat supplement device is provided with a circulating pump, the circulating pipe of the circulating pump extends outward and is in communication with the evaporator, and the input end of the heat supplement device is in communication with the top end of the evaporator through a pipeline and is provided with a valve.

[0012] Further, the top of the evaporator is further provided with a shell side inlet, the shell side inlet is in communication with the bottom of the membrane filter, and the shell side inlet is further provided with a temperature sensor.

[0013] Further, a plurality of filter cartridges are vertically arranged inside the membrane filter, the filter cartridges are covered with a permeation gasification membrane, the output pipe of the evaporator is in communication with the top end of each filter cartridge through a mesh branch, and each filter cartridge is correspondingly provided with a backflow pipe at the bottom, the other ends of the plurality of backflow pipes are collected at the shell side inlet, and the other end of the membrane filter is further provided with a drain pipe.

[0014] Further, a gas valve is arranged at the connection between each filter cartridge and the output pipe of the evaporator.

[0015] Further, a heat pump is further arranged on the output pipe of the evaporator.

[0016] Further, a flow meter is further arranged on the feed inlet of the deacidification tower.

[0017] Compared with the prior art, the technical scheme of the present application has the following beneficial technical effects:

[0018] The present application is improved based on the existing excess alcohol dehydration recovery device, the material after deacidification is heated by the evaporator to become gaseous, then the steam is pressurized again by the heat pump and transported to the inside of the membrane filter, the water in the steam state material is separated by the permeation gasification membrane to obtain anhydrous alcohol product, in this process, the anhydrous alcohol steam in the evaporator can be effectively utilized twice, so only the heat pump needs to be powered, which can effectively avoid waste of steam, and in this process, the whole device can be continuously and uninterruptedly operated, greatly improving the recovery efficiency. Attached Figure Description

[0019] Fig. 1 This is a schematic diagram of the entire dehydration and recovery device in this embodiment;

[0020] Fig. 2 This is a schematic diagram of the filter element in this embodiment;

[0021] Fig. 3 This is a schematic diagram of the membrane filter and filter cartridge in this embodiment;

[0022] The components include: 1. Deacidification tower; 2. Dehydration assembly; 21. Evaporator; 22. Membrane filter; 23. Filter element; 231. Preheating pipe; 232. Filter cartridge; 24. Filter cylinder; 25. Return pipe; 26. Drain pipe; 3. Heat replenishment assembly; 31. Heat replenisher; 32. Circulation pump; 33. Circulation pipe; 4. Heat pump. Detailed Implementation

[0023] To facilitate understanding of this application, a more complete description will be provided below with reference to the accompanying drawings, which illustrate embodiments of the present application. However, the present application can be implemented in many different forms and is not limited to the embodiments described herein. Rather, these embodiments are provided so that the disclosure of this application will be thorough and complete.

[0024] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the application.

[0025] Combination Figs. 1-3 As shown, an apparatus for dehydrating and recovering excess alcohol from an esterification reaction includes:

[0026] Deacidification tower 1 is mainly used to remove acidic components from the recovered liquid so that the acid-removed mixture can be further separated using a large number of inorganic molecular sieve membranes.

[0027] The dehydration component 2, consisting of an evaporator 21 and a membrane filter 22, is located on one side of the deacidification tower 1. It separates the water in the recovery liquid through heating and filtration, thereby achieving efficient recovery of anhydrous alcohol.

[0028] Specifically, in this embodiment, during the acid removal process, the acid removal tower 1 mainly uses acid-base neutralization to remove the acidity in the recovered liquid, which will result in precipitation. In order to facilitate the subsequent further processing of the recovered liquid, it is necessary to filter the recovered liquid after acid removal in advance.

[0029] The existing filtering mode has simple structure, directly uses the filter screen to realize, but the amount of recovery liquid is relatively large, each time of filtering separation, part of impurities will be blocked on the filter screen, if not timely discharge, will seriously affect the subsequent conveying effect, therefore, the staff needs to carry out regular cleaning, cannot carry out continuous work.

[0030] Based on the above structure requirements, in the embodiment, a filter 23 is directly arranged at the input end of the evaporator 21, which is in cylindrical structure, and a reverse tapered filter core 232 is arranged inside, the inner wall of the filter core 232 is covered with a filter membrane, the top end and the bottom end of the filter core 232 extend to the outside of the filter 23 and form interfaces and impurity discharge pipes at both ends respectively, the interface is in communication with the discharge pipe on the deacidification tower 1, therefore, the recovery liquid in the deacidification tower 1 can directly enter the inside of the filter 23 and separate the impurities in the liquid through the filter membrane, after separation, the solid impurities will be retained in the inside of the filter core 232, the electromagnetic valve on the impurity discharge pipe is opened regularly, so as to discharge the impurities.

[0031] In the above structure, the filter structure does not need the staff to stop for maintenance operation, only needs to control the on-off of the electromagnetic valve on the impurity discharge pipe to realize the automatic impurity discharge function, which is very convenient to use.

[0032] In addition, it also needs to be preheated before entering the dewatering assembly 2, in order to effectively utilize the anhydrous alcohol steam waste heat in the inside of the dewatering assembly 2, in the embodiment, a preheating pipe 231 is arranged in the inside of the filter 23, which is arranged in spiral shape, and the two ends thereof extend to the inside of the dewatering assembly 2 respectively, and a liquid pump is arranged at the connection position, which is used for input and output of the high temperature steam after condensation, therefore, in the filtering and separating process, a large amount of recovery liquid will be in contact with the preheating pipe 231 first, so as to achieve the preheating effect, and does not need to consume extra steam, effectively utilizes the latent heat carried by the high temperature steam after condensation, and the anhydrous alcohol after condensation is more convenient to recycle and store.

[0033] The input end of the evaporator 21 is in communication with the output end of the above filter 23, which is used for evaporating the filtered solution into gaseous state, and then inputting into the inside of the output end input membrane filter 22, and separating the water vapor by the filter membrane, so as to obtain the anhydrous alcohol under high temperature gaseous state, so as to recycle and utilize it separately.

[0034] In the above structure, one side of the evaporator 21 is also equipped with a heat supplement assembly 3, which includes a heat supplement device 31 (i.e. an electric heater, and is externally connected with a steam input pipe, which uses a circulating method to reheat high-temperature steam, and cooperates with an external steam pipe to supplement a certain amount of internal steam), a circulating pump 32 and a circulating pipe 33, the input end of the circulating pipe 33 is in communication with the top end side wall of the evaporator 21, the output end is in communication with the bottom end side wall of the evaporator 21, and a remotely controllable valve is also arranged on the input end, and the circulating pump 32 and the heat supplement device 31 are both installed on the circulating pipe 33, and the circulating pump 32 is mainly used to control the speed of its circulating heating.

[0035] In addition, after the recovered liquid is heated and evaporated into a gaseous state, the heat pump 4 is used to input it into the membrane filter 22, in order to separate the water in the recovered liquid in a gaseous state, a plurality of filter cartridges 24 are also vertically arranged in the membrane filter 22, and a permeation gasification membrane is arranged on the filter cartridge 24, and the output pipe of the evaporator 21 is in communication with the top end of each filter cartridge 24 through a mesh branch, and each filter cartridge 24 is correspondingly equipped with a reflux pipe 25 at the bottom, and the other end of the reflux pipe 25 is in communication with the shell side inlet, so that when the high-temperature steam in the gaseous state is input into the filter cartridge 24, it will quickly diffuse, especially the water vapor will directly pass through the permeation gasification membrane on the surface of the filter cartridge 24, and the recovered liquid gas will be blocked by the permeation gasification membrane, the water vapor is drawn by the air blower and cooperates with the condenser to condense the water vapor, and then is discharged along the drain pipe 26 on the membrane filter 22, and the anhydrous alcohol steam remaining in the filter cartridge 24 is directly injected into the shell side inlet of the evaporator 21 through the reflux pipe 25 at the bottom, so that the anhydrous alcohol steam is used as a heat source for evaporating new recovered liquid, and after preliminary condensation, it can also be used as a heat source in the preheating structure, so that the heat in the whole process is recycled to a high degree, and in the whole process, a certain amount of hot steam is added through the heat supplement device 31 when the equipment is started, and then it can be closed and continuously work, and will not affect the operation of the whole equipment.

[0036] In the above structure, the plurality of filter cartridges 24 can also be individually disassembled, which facilitates the periodic replacement of the filter membranes by the staff, and during the maintenance process, the equipment does not need to be shut down, only the corresponding valve needs to be closed, which greatly improves the convenience of maintenance and does not affect the recovery work efficiency of the whole equipment.

[0037] At the connection of the shell side inlet at the top of the reflux pipe 25 and the evaporator 21, a temperature sensor should also be equipped to monitor the filtered anhydrous alcohol vapor temperature in real time, so that the staff can adjust the internal vapor temperature of the evaporator 21 through the heat supplement device 31. In addition, a flow meter is also arranged at the feed inlet of the deacidification tower 1 to count the input, and the recovery ratio of the entire device is calculated by comparing the recovered anhydrous alcohol product, so as to facilitate the staff to improve the recovery process later.

[0038] Finally, it should be pointed out that: the above examples are only used to illustrate the technical solutions of the present application, and not to limit them; although the present application has been described in detail with reference to the foregoing examples, those skilled in the art should understand that: it can still modify the technical solutions recorded in the foregoing examples, or make equivalent replacement for part or all of the technical features; and these modifications or replacements do not make the essence of the corresponding technical solutions deviate from the technical solutions of the embodiments of the present application.

Claims

1. An apparatus for recovering excess alcohol from an esterification reaction by dehydration, characterized by comprising: The application relates to a deacidification and dehydration device, which comprises a deacidification tower (1) and a dehydration assembly (2), the feed inlet of the deacidification tower (1) is communicated with a raw material pipe, the dehydration assembly (2) is divided into an evaporator (21) and a membrane filter (22), the input end of the evaporator (21) is communicated with a discharge pipe of the deacidification tower (1), the output pipe of the evaporator (21) is communicated with the inside of the membrane filter (22), and a drain pipe (26) is further arranged on one side of the membrane filter (22); a heat supplement assembly (3) is further arranged in the deacidification tower (1), and the heat supplement assembly (3) is communicated with the inside of the evaporator (21) through a pipeline.

2. The esterification reaction excess alcohol dehydration recovery apparatus according to claim 1, characterized by A filter piece (23) is further arranged on the input end of the evaporator (21), the filter piece (23) is in a cylindrical shape and internally provided with a reverse conical filter core (232), a plurality of filter holes are arranged around the outer side wall of the filter core (232), and a filter film is covered on the surface.

3. The esterification reaction excess alcohol dehydration recovery apparatus according to claim 2, characterized by The top of the filter core (232) extends upwards and is provided with an interface at the top end, the interface is communicated with the discharge pipe of the deacidification tower (1), the bottom of the filter core (232) extends downwards and is provided with a foreign matter discharge pipe, the foreign matter discharge pipe extends downwards and is internally provided with an electromagnetic valve, and the input end of the evaporator (21) is communicated with the side wall of the filter piece (23) through a pipeline.

4. The esterification reaction excess alcohol dehydration recovery apparatus according to claim 3, characterized by A preheating pipe (231) is further arranged in the filter piece (23), the main body of the preheating pipe (231) is arranged in a spiral shape around the periphery of the filter core (232), one end of the preheating pipe (231) is communicated with the inside of the evaporator (21), and the other end extends to the outside and is externally connected to a recovery container.

5. The excess alcohol dehydration recovery apparatus for esterification reaction according to claim 4, characterized by The heat supplement assembly (3) comprises a heat supplement device (31) arranged on one side in the dehydration assembly (2), a circulating pump (32) is arranged on the output end of the heat supplement device (31), a circulating pipe (33) of the circulating pump (32) extends outwards and is communicated with the evaporator (21), and the input end of the heat supplement device (31) is communicated with the top end of the evaporator (21) through a pipeline and is provided with a valve.

6. The esterification reaction excess alcohol dehydration recovery apparatus according to claim 5, characterized by A shell side inlet is further arranged on the top of the evaporator (21), the shell side inlet is communicated with the bottom of the membrane filter (22), and a temperature sensor is further arranged on the shell side inlet.

7. The apparatus for recovering excess alcohol from an esterification reaction according to claim 1, wherein A plurality of filter cartridges (24) are vertically arranged in the membrane filter (22), the filter cartridges (24) are covered with permeation gasification membranes, the output pipe of the evaporator (21) is communicated with the top end of each filter cartridge (24) through a mesh branch, each filter cartridge (24) is correspondingly provided with a backflow pipe (25) at the bottom, the other ends of the backflow pipes (25) are gathered at the shell side inlet, and a drain pipe (26) is further arranged at the other end of the membrane filter (22).

8. The esterification reaction excess alcohol dehydration recovery apparatus according to claim 7, characterized by An air valve is arranged at the connection between each filter cartridge (24) and the output pipe of the evaporator (21).

9. The esterification reaction excess alcohol dehydration recovery apparatus according to claim 8, characterized by A heat pump (4) is further arranged on the output pipe of the evaporator (21).

10. The apparatus for recovering excess alcohol from an esterification reaction according to claim 1, wherein A flowmeter is further arranged on the feed inlet of the deacidification tower (1).

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