CN220176831U - Experimental device for synthesizing diethyl carbonate by transesterification of ethylene carbonate and ethanol - Google Patents

Experimental device for synthesizing diethyl carbonate by transesterification of ethylene carbonate and ethanol Download PDF

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Publication number
CN220176831U
CN220176831U CN202321408752.2U CN202321408752U CN220176831U CN 220176831 U CN220176831 U CN 220176831U CN 202321408752 U CN202321408752 U CN 202321408752U CN 220176831 U CN220176831 U CN 220176831U
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pipeline
ethanol
diethyl carbonate
experimental device
reaction
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阎子祯
郭建军
刘晨旭
张延让
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Shenghua New Energy Technology Dongying Co Ltd
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Shenghua New Energy Technology Dongying Co Ltd
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    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
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Abstract

The utility model relates to an experimental device for synthesizing diethyl carbonate by transesterification of ethylene carbonate and ethanol. The technical proposal is as follows: the lower extreme of blending tank is connected to the pre-reactor through pipeline and pre-heater, and the export of pre-reactor is connected to the reaction rectifying column through the pipeline, the lower extreme of reaction rectifying column is equipped with the cauldron end reboiler, and the top of reaction rectifying column is connected to the ethanol recovery jar through pipeline, first control valve and condenser, the bottom of reaction rectifying column is connected to the crude product jar of diethyl carbonate through the pipeline. The beneficial effects are that: the utility model solves the defect that the existing catalyst sodium ethoxide of a diethyl carbonate synthesis device is sensitive to the reaction environment, provides sodium methoxide with mild reaction conditions and relatively stable reaction environment as a catalyst, and provides a new thought for synthesizing diethyl carbonate by relatively stably generating transesterification reaction in a reaction rectifying tower under the catalysis of sodium methoxide through experiments.

Description

Experimental device for synthesizing diethyl carbonate by transesterification of ethylene carbonate and ethanol
Technical Field
The utility model relates to a diethyl carbonate preparation experimental device, in particular to a diethyl carbonate synthesis experimental device by transesterification of ethylene carbonate and ethanol.
Background
Diethyl carbonate (DEC for short) is an important compound in carbonic ester, and is a recognized green and environment-friendly chemical product. The ethyl, carbonyl, ethoxy and carboethoxy in the molecular structure have various reactivity, are important organic synthesis intermediates, and meanwhile, the DEC is used as an important solvent, so that the DEC has high industrial application value in the preparation of lithium battery electrolyte, the production of resin, nitrocellulose and cellulose ether.
In recent years, the demand for diethyl carbonate DEC has increased in the fields of lithium battery electrolytes, resins, medicines, printing and dyeing, and the development of the diethyl carbonate industry and the development of synthesis processes have been continuously promoted. The diethyl carbonate mainly comprises a phosgene method, an ester exchange method, an ethanol oxidative oxo-synthesis method and the like, wherein the ester exchange method is used for industrialization of the diethyl carbonate due to mild reaction conditions and high reaction speed. The Chinese patent number is CN201811194271.X, the patent name is "homogeneous production process of high-purity diethyl carbonate for lithium batteries", and the production process of high-purity diethyl carbonate for lithium batteries is synthesized in one step by taking ethylene carbonate (or propylene carbonate) and ethanol as reaction raw materials. However, the catalyst adopted by the method is soluble strong alkali sodium ethoxide, and the sodium ethoxide is solid powder, and has the defect of sensitivity to reaction environment.
Because the activity of the catalyst determines the degree of reaction progress, the transesterification catalyst is mainly divided into two types, i.e. homogeneous phase and heterogeneous phase, wherein liquid sodium methoxide is not applied to transesterification synthesis of ethylene carbonate and ethanol, so that in order to realize full utilization of sodium methoxide in transesterification reaction and improve the product yield, an experimental device for synthesizing diethyl carbonate by transesterification of ethylene carbonate and ethanol is necessary to design.
Disclosure of Invention
The utility model aims at overcoming the defects in the prior art, and provides an experimental device for synthesizing diethyl carbonate by transesterification of ethylene carbonate and ethanol.
The utility model relates to an experimental device for synthesizing diethyl carbonate by transesterification of ethylene carbonate and ethanol, which adopts the technical scheme that: including compounding jar (1), pre-reactor (2), pre-reactor (3), kettle bottom reboiler (5), reaction rectifying column (6), condenser (7), ethanol recovery jar (8), diethyl carbonate crude tank (9), the upper end of compounding jar (1) is equipped with ethylene carbonate feed inlet (1.1), ethanol feed inlet (1.2) and sodium methoxide feed inlet (1.3), the lower extreme of compounding jar (1) is connected to pre-reactor (3) through pipeline and pre-heater (2), the export of pre-reactor (3) is connected to reaction rectifying column (6) through the pipeline, the lower extreme of reaction rectifying column (6) is equipped with kettle bottom reboiler (5), and the top of reaction rectifying column (6) is connected to ethanol recovery jar (8) through pipeline and condenser (7), the bottom of reaction rectifying column (6) is connected to diethyl carbonate crude tank (9) through the pipeline.
Preferably, the lower end of the mixing tank (1) is connected to the lower end of the preheater (2) through a pipeline and a feed pump (4), the upper end of the preheater (2) is connected to the lower end of the pre-reactor (3) through a pipeline, and the upper end of the pre-reactor (3) is connected to one side of the reactive rectifying tower (6) through a pipeline.
Preferably, the top of the reaction rectifying tower (6) is connected to a tube side inlet of a condenser (7) through a pipeline, and a tube side outlet of the condenser (7) is connected to an ethanol recovery tank (8) through a pipeline; the shell side inlet of the condenser (7) is connected to the condensate water inlet pipe, and the shell side outlet of the condenser (7) is connected to the condensate water return pipe.
Preferably, the top of the reactive rectifying tower (6) is connected to a connecting pipe line of an ethanol feed inlet (1.2) at the top of the mixing tank (1) through a circulating pipe line (1.4) and a second control valve (11).
Preferably, a third control valve (12) is arranged on the connecting pipe line of the ethanol feed inlet (1.2).
Preferably, a fourth control valve (13) is arranged on a pipeline at the bottom outlet of the reaction rectifying tower (6).
The beneficial effects of the utility model are as follows: according to the utility model, ethylene glycol EG, diethyl carbonate (DEC) and a small amount of unreacted ethylene carbonate are gathered at the tower bottom of the reaction rectifying tower after ethylene carbonate, ethanol ester and sodium methoxide are fully mixed and enter the reaction rectifying tower to undergo transesterification; the method solves the defect that the existing catalyst sodium ethoxide of the diethyl carbonate synthesis device is sensitive to the reaction environment, provides a sodium methoxide with mild reaction conditions and relatively stable reaction environment as a catalyst, and provides a new thought for the synthesis of diethyl carbonate through relatively stable transesterification reaction in a reaction rectifying tower under the catalysis of sodium methoxide through experiments.
Drawings
Fig. 1 is a schematic structural view of embodiment 1 of the present utility model;
fig. 2 is a schematic structural view of embodiment 2 of the present utility model;
in the upper graph: mixing tank 1, preheater 2, pre-reactor 3, feed pump 4, kettle bottom reboiler 5, reaction rectifying column 6, condenser 7, ethanol recovery tank 8, diethyl carbonate crude product tank 9, first control valve 10, second control valve 11, third control valve 12, fourth control valve 13, ethylene carbonate feed inlet 1.1, ethanol feed inlet 1.2 and sodium methoxide feed inlet 1.3, circulation line 1.4.
Detailed Description
The preferred embodiments of the present utility model will be described below with reference to the accompanying drawings, it being understood that the preferred embodiments described herein are for illustration and explanation of the present utility model only, and are not intended to limit the present utility model.
Embodiment 1, referring to fig. 1, an experimental device for synthesizing diethyl carbonate by transesterification of ethylene carbonate and ethanol according to the present utility model comprises a mixing tank 1, a preheater 2, a pre-reactor 3, a kettle bottom reboiler 5, a reaction rectifying tower 6, a condenser 7, an ethanol recovery tank 8 and a crude diethyl carbonate tank 9, wherein the upper end of the mixing tank 1 is provided with an ethylene carbonate feed inlet 1.1, an ethanol feed inlet 1.2 and a sodium methoxide feed inlet 1.3, the lower end of the mixing tank 1 is connected to the pre-reactor 3 through a pipeline and the preheater 2, the outlet of the pre-reactor 3 is connected to the reaction rectifying tower 6 through a pipeline, the lower end of the reaction rectifying tower 6 is provided with a kettle bottom reboiler 5, the top of the reaction rectifying tower 6 is connected to the ethanol recovery tank 8 through a pipeline, a first control valve 10 and the condenser 7, and the bottom of the reaction rectifying tower 6 is connected to the crude diethyl carbonate tank 9 through a pipeline.
Wherein, the lower end of the mixing tank 1 is connected to the lower end of the preheater 2 through a pipeline and a feed pump 4, the upper end of the preheater 2 is connected to the lower end of the pre-reactor 3 through a pipeline, and the upper end of the pre-reactor 3 is connected to one side of the reactive rectifying tower 6 through a pipeline.
The top of the reactive rectifying tower 6 is connected to a tube side inlet of a condenser 7 through a pipeline, and a tube side outlet of the condenser 7 is connected to an ethanol recovery tank 8 through a pipeline; the shell side inlet of the condenser 7 is connected to a condensate water inlet pipe, and the shell side outlet of the condenser 7 is connected to a condensate water return pipe.
In addition, the top of the reactive rectifying tower 6 is connected to the connecting pipe line of the ethanol feed inlet 1.2 at the top of the mixing tank 1 through the circulating pipeline 1.4 and the second control valve 11, so that ethanol can be conveniently controlled to be fed into the mixing tank 1 along the circulating pipeline 1.4 for recycling, and in addition, the mixing tank is internally provided with a stirrer, so that raw materials can be mixed more uniformly.
The connecting pipeline of the ethanol feed inlet 1.2 is provided with a third control valve 12, so that the ethanol can be conveniently controlled to be fed into the mixing tank 1 for recycling.
A fourth control valve 13 is arranged on a pipeline at the bottom outlet of the reaction rectifying tower 6, so that the crude diethyl carbonate can be conveniently controlled to enter the crude diethyl carbonate tank 9.
The reaction rectifying tower 6 has a tower diameter of 100mm, a tower height of 1m and a tower plate number of 20; the pressure is normal pressure; the feeding temperature is 50 ℃; the temperature of the tower top is 80 ℃; the temperature of the tower kettle is 130 ℃; the temperature outlet of the reboiler 5 at the bottom of the kettle is 135 ℃.
In the use of the present utility model,
ethylene carbonate EC and ethanol EA are used as raw materials, diethyl carbonate is prepared by testing under the catalysis of sodium methoxide, and the raw materials are fed into a tower: in order to improve the reaction effect, a preheater 2 and a pre-reactor 3 are additionally arranged in front of the reaction rectifying tower, and then the mixture is sent into the reaction rectifying tower 6, the ethylene carbonate EC and the ethanol EA are subjected to transesterification under the action of sodium methoxide as a catalyst to obtain a mixture, ethylene glycol EG, diethyl carbonate DEC and a small amount of unreacted ethylene carbonate EC are gathered in the tower kettle of the reaction rectifying tower 6 along with the progress of transesterification, the mixture is gasified again through a kettle bottom reboiler 5 arranged in the tower kettle to enter the reaction rectifying tower 6, the finally obtained tower kettle mixture enters the next separation stage, the ethanol EA of light components is extracted from the top, and the balance is continuously established in the tower of the reaction rectifying tower 6 along with the progress of rectification and reaction, so that the mixture is in a relatively stable state in the tower, thereby being beneficial to the full utilization of sodium methoxide.
Embodiment 2, referring to fig. 2, the experimental device for synthesizing diethyl carbonate by transesterification of ethylene carbonate and ethanol according to the present utility model comprises a mixing tank 1, a feed pump 4, a kettle bottom reboiler 5, a reaction rectifying tower 6, a condenser 7, an ethanol recovery tank 8, and a crude diethyl carbonate tank 9, wherein the upper end of the mixing tank 1 is provided with an ethylene carbonate feed inlet 1.1, an ethanol feed inlet 1.2 and a sodium methoxide feed inlet 1.3, the lower end of the mixing tank 1 is connected to the reaction rectifying tower 6 through a pipeline and the feed pump 4, the lower end of the reaction rectifying tower 6 is provided with the kettle bottom reboiler 5, the top of the reaction rectifying tower 6 is connected to the ethanol recovery tank 8 through a pipeline, a first control valve 10 and the condenser 7, and the bottom of the reaction rectifying tower 6 is connected to the crude diethyl carbonate tank 9 through a pipeline.
The difference from example 1 is that: the preheater 2 and the pre-reactor 3 were omitted, and the experimental setup of this example was simplified, but the experimental purposes of the present utility model could also be achieved.
The above description is of the preferred embodiments of the present utility model, and any person skilled in the art may modify the present utility model or make modifications to the present utility model with the technical solutions described above. Therefore, any simple modification or equivalent made according to the technical solution of the present utility model falls within the scope of the protection claimed by the present utility model.

Claims (6)

1. An experimental device for synthesizing diethyl carbonate by transesterification of ethylene carbonate and ethanol is characterized in that: including compounding jar (1), pre-reactor (2), pre-reactor (3), kettle bottom reboiler (5), reaction rectifying column (6), condenser (7), ethanol recovery jar (8), diethyl carbonate crude tank (9), the upper end of compounding jar (1) is equipped with ethylene carbonate feed inlet (1.1), ethanol feed inlet (1.2) and sodium methoxide feed inlet (1.3), the lower extreme of compounding jar (1) is connected to pre-reactor (3) through pipeline and pre-heater (2), the export of pre-reactor (3) is connected to reaction rectifying column (6) through the pipeline, the lower extreme of reaction rectifying column (6) is equipped with kettle bottom reboiler (5), and the top of reaction rectifying column (6) is connected to ethanol recovery jar (8) through pipeline and condenser (7), the bottom of reaction rectifying column (6) is connected to diethyl carbonate crude tank (9) through the pipeline.
2. The experimental device for synthesizing diethyl carbonate by transesterification of ethylene carbonate and ethanol according to claim 1, wherein the experimental device is characterized in that: the lower extreme of compounding jar (1) be connected to the lower extreme of pre-heater (2) through pipeline and feeding pump (4), the upper end of pre-heater (2) is connected to the lower extreme of pre-reactor (3) through the pipeline, the upper end of pre-reactor (3) is connected to one side of reaction rectifying column (6) through the pipeline.
3. The experimental device for synthesizing diethyl carbonate by transesterification of ethylene carbonate and ethanol according to claim 2, wherein the experimental device is characterized in that: the top of the reaction rectifying tower (6) is connected to a tube side inlet of a condenser (7) through a pipeline, and a tube side outlet of the condenser (7) is connected to an ethanol recovery tank (8) through a pipeline; the shell side inlet of the condenser (7) is connected to the condensate water inlet pipe, and the shell side outlet of the condenser (7) is connected to the condensate water return pipe.
4. The experimental device for synthesizing diethyl carbonate by transesterification of ethylene carbonate and ethanol according to claim 3, wherein the experimental device is characterized in that: the top of the reactive rectifying tower (6) is connected to a connecting pipe line of an ethanol feed inlet (1.2) at the top of the mixing tank (1) through a circulating pipeline (1.4) and a second control valve (11).
5. The experimental device for synthesizing diethyl carbonate by transesterification of ethylene carbonate and ethanol according to claim 4, wherein the experimental device is characterized in that: and a third control valve (12) is arranged on the connecting pipeline of the ethanol feed inlet (1.2).
6. The experimental device for synthesizing diethyl carbonate by transesterification of ethylene carbonate and ethanol according to claim 5, wherein the experimental device is characterized in that: a fourth control valve (13) is arranged on a pipeline at the bottom outlet of the reaction rectifying tower (6).
CN202321408752.2U 2023-06-05 2023-06-05 Experimental device for synthesizing diethyl carbonate by transesterification of ethylene carbonate and ethanol Active CN220176831U (en)

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CN202321408752.2U CN220176831U (en) 2023-06-05 2023-06-05 Experimental device for synthesizing diethyl carbonate by transesterification of ethylene carbonate and ethanol

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Application Number Priority Date Filing Date Title
CN202321408752.2U CN220176831U (en) 2023-06-05 2023-06-05 Experimental device for synthesizing diethyl carbonate by transesterification of ethylene carbonate and ethanol

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CN220176831U true CN220176831U (en) 2023-12-15

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