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Device and method for preparing electronic ethylene carbonate by coupling crystallization with rectification

A technology coupled with ethylene carbonate and rectification, which is applied in the field of preparation of electronic grade reagents, can solve problems such as difficult balance between product purity and yield, unfavorable lithium-ion battery electrolyte, and poor lithium-ion battery, so as to ensure production operation Efficiency, high product purity, and easy maintenance

Pending Publication Date: 2017-12-22
FUZHOU UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The formation of alcohols and the hydrolysis of ethylene carbonate will have adverse effects on lithium-ion batteries
In addition, due to the hygroscopicity of ethylene carbonate, it contains a small amount of water while containing the above-mentioned impurities, which is unfavorable for the configuration of lithium-ion battery electrolyte, so ethylene carbonate must be processed and purified to reach electronic grade , to meet the requirements of high-quality lithium batteries
[0004] At present, rectification is mostly used for the purification of ethylene carbonate, but the existing operation process has problems such as high energy consumption, long operation cycle, low yield, and large material loss during the purification process.
Simply preparing electronic-grade ethylene carbonate by rectification, it is difficult to balance the purity and yield of the product, and the production cost is high
In addition, there is also a way to purify ethylene carbonate by adding alcohol and impurity removers such as ferric chloride, aluminum chloride, and molecular sieves. However, this method also has high requirements for operating conditions, long operating cycles, complicated operations, and high yield. Disadvantages such as low rate

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  • Device and method for preparing electronic ethylene carbonate by coupling crystallization with rectification
  • Device and method for preparing electronic ethylene carbonate by coupling crystallization with rectification

Examples

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Embodiment 1

[0058] Such as figure 1 As shown, the present embodiment provides a device for preparing electronic-grade ethylene carbonate coupled with crystallization and rectification, including a raw material storage tank 1, a falling film crystallizer 2, a rectification tower 3, a first product tank 4, a transition tank 5 and Second product tank 6.

[0059] The connection relationship of each device is as follows:

[0060] The raw material storage tank 1 is connected to the feed port 201 of the falling film crystallizer 2 through the feed pipeline 11, and a discharge main pipe 21 is arranged at the discharge port 202 of the falling film crystallizer 2, and the end of the discharge main pipe 21 is connected with a circulation pipeline 31. The first product pipeline 41 and the transition pipeline 51, the circulation pipeline 31 is connected to the feed port 201 of the falling film crystallizer 2, the first product pipeline 41 is connected to the first product tank 4, and the transition p...

Embodiment 2

[0080] This embodiment provides a method for preparing electronic-grade ethylene carbonate coupled with crystallization and rectification, including a crystallization process and a rectification process, and the crystallization process includes the following steps:

[0081] Crystallization: The ethylene carbonate material to be purified is transported from the raw material storage tank 1 to the falling film crystallizer 2, the material enters the falling film crystallizer 2 and flows in the falling film in the crystallization tube, and the temperature of the cooling medium is adjusted so that the material is Crystallize in the crystallization tube, stop feeding when the crystal layer reaches a certain thickness;

[0082] Sweating: Then gradually increase the temperature of the cooling medium to make the crystal layer sweat, and discharge the sweating residue into the transition tank 5;

[0083] Crystallization and melting: after sweating, further increase the temperature of th...

Embodiment 3

[0094] Different from Example 2 are the operating conditions of the crystallization process and the operating conditions of the rectifying process, and all the other are the same as Example 2.

[0095] In the present embodiment, the operating conditions of the crystallization process are:

[0096] The feed flow rate of ethylene carbonate is 200L / h, and the feed temperature is 42°C;

[0097] During the falling film crystallization process, the cooling step length is 1.5°C / h, the crystallization time is 6h, and the end point temperature of cooling crystallization is 33°C, followed by constant temperature for 2h;

[0098] The temperature rise step in the sweating process is 3°C / h, the sweating time is 3h, and the sweating end point temperature is 37°C;

[0099] The temperature during the melting of the crystals was 45°C.

[0100] The operating conditions of the rectification process are:

[0101] The vacuum distillation operation is adopted, the pressure inside the tower is 2....

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Abstract

The invention belongs to the technical field of preparation of an electronic reagent and relates to a device and a method for preparing electronic ethylene carbonate by coupling crystallization with rectification. The device for preparing electronic ethylene carbonate by coupling crystallization with rectification provided by the invention comprises a raw material storage tank, a falling film crystallizer, a rectifying column, a first product tank, a transition tank and a second product tank, wherein the raw material storage tank is connected with a feeding port of the falling film crystallizer; a discharging head pipe is arranged at a discharging port of the falling film crystallizer; the discharging head pipe is respectively connected with the feeding port of the falling film crystallizer, the first product tank and the transition tank; the transition tank is connected with the rectifying column; an outlet at the top of the rectifying column is connected with the second product tank; the outlet at the bottom of the rectifying column is connected with the raw material storage tank. According to the invention, the two technologies of falling film crystallization and rectification are coupled with each other, the deficiencies thereof are mutually made up, more efficient separating operation is realized, the prepared ethylene carbonate can reach ultra-clean high-purity electronic level, and meanwhile, the structure is simple, the operation is convenient, the energy consumption is low and the cost is low.

Description

technical field [0001] The invention belongs to the technical field of preparation of electronic-grade reagents, and relates to the preparation of electronic-grade ethylene carbonate, in particular to a device and method for preparing electronic-grade ethylene carbonate by coupling crystallization and rectification. Background technique [0002] Ethylene carbonate (EC) is an organic solvent and organic synthesis intermediate with excellent performance. It has the advantages of high boiling point, low toxicity and corrosion. It is soluble in water, acetone, ethanol and other solvents. Acrylonitrile, etc., can be used as spinning liquid on textiles; it can also be directly used as a solvent for removing acid gas and an additive for concrete. It can be used as a pharmaceutical component and raw material in medicine; it can also be used as a plastic foaming agent and a stabilizer for synthetic lubricating oil. What is particularly prominent is that ethylene carbonate is widel...

Claims

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Application Information

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IPC IPC(8): C07D317/38
CPCC07D317/38Y02E60/10
Inventor 杨臣柴士阳邱挺叶长燊王红星李玲黄智贤杨金杯陈锦溢王晓达林小城王清莲
Owner FUZHOU UNIVERSITY
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