Method for preparing electronic grade ethylene carbonate by falling film crystallization

A technology of ethylene carbonate and falling film crystallization, applied in circuits, electrical components, secondary batteries, etc., can solve the problems of unfavorable lithium-ion battery electrolyte, high operating conditions, and poor lithium-ion batteries, and achieve considerable economic benefits , Reduce energy consumption, increase output and product purity

Active Publication Date: 2018-01-26
TIANJIN UNIVERSITY OF SCIENCE AND TECHNOLOGY
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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 large energy consumption and long operation cycle.
In addition, there is also a way to purify ethylene carbonate by adding alcohol and impurities removal agents such as ferric chloride, aluminum chloride, molecular sieve or activated carbon, but this method also has high requirements for operating conditions, complicated operations, and low yields and high cost issues

Method used

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  • Method for preparing electronic grade ethylene carbonate by falling film crystallization
  • Method for preparing electronic grade ethylene carbonate by falling film crystallization

Examples

Experimental program
Comparison scheme
Effect test

Embodiment approach

[0066] As an optional implementation, the method includes the following steps:

[0067] (a) Preheating: Preheat the ethylene carbonate raw material to 39-50°C, keep the temperature constant for 10-60 minutes, and then use a pump to transport the raw material to the crystallizer;

[0068] (b) Feeding: raw materials are fed from the top of the crystallizer, so that the raw materials are circulated between the crystallizer and the raw material storage tank at a flow rate of 100t / h~300t / h, and the temperature of the crystallizer is controlled at 25~35°C;

[0069] (c) Cooling crystallization: crystallize by gradually cooling down, so that ethylene carbonate forms a crystal layer on the wall of the crystallizer, the cooling step is 0.5 ° C / h ~ 3 ° C / h, the cooling end temperature is 15 ~ 35 ° C, crystallization Stop feeding after 2-13 hours, then keep the temperature for 1-3 hours, discharge the uncrystallized ethylene carbonate residual liquid from the material outlet of the cr...

Embodiment 1

[0077]The present embodiment provides a method for preparing electronic-grade ethylene carbonate by falling film crystallization, comprising the following steps:

[0078] (a) add ethylene carbonate raw material from crystallizer top with pump, make ethylene carbonate circulate between crystallizer and ethylene carbonate raw material storage tank by 100t / h flow rate, crystallizer wall temperature temperature drops to 35 ℃;

[0079] (b) Carry out crystallization by gradually lowering the temperature, so that ethylene carbonate forms a crystal layer on the wall of the crystallizer, and the temperature at the end point of cooling is 30°C. Stop feeding after 2 hours of crystallization, and then keep the temperature for 1 hour, and remove the uncrystallized ethylene carbonate residual liquid It is discharged from the material outlet of the crystallizer and transported to the recovery device;

[0080] (c) The crystal layer is melted by heating and sweating in two steps, and the sweat...

Embodiment 2

[0083] The present embodiment provides a method for preparing electronic-grade ethylene carbonate by falling film crystallization, comprising the following steps:

[0084] (a) ethylene carbonate raw material is added from crystallizer top with pump, makes ethylene carbonate circulate between crystallizer and ethylene carbonate raw material storage tank by 200t / h flow rate, and crystallizer wall temperature temperature drops to 30 ℃;

[0085] (b) Carry out crystallization by gradually lowering the temperature, so that ethylene carbonate forms a crystal layer on the wall of the crystallizer. The end point temperature of cooling is 26° C., stop feeding after 5 hours of crystallization, and then keep the temperature for 2 hours to remove the uncrystallized ethylene carbonate residue. It is discharged from the material outlet of the crystallizer and transported to the recovery device;

[0086] (c) The crystal layer is melted by heating and sweating in three steps, and the sweating ...

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Abstract

The invention belongs to the technical field of preparation of electronic grade reagents and relates to a method for preparing electronic grade ethylene carbonate by falling film crystallization. Themethod comprises gradual cooling crystallization, stepwise heating sweating, complete melting and secondary crystallization and realizes recovery and treatment on the falling film crystallization residue liquid and sweating residue liquid so that energy consumption is reduced, a falling film crystallization yield and product purity are improved and product purity, product yield and comprehensive device economic benefits are maximized. Compared with the existing method using alcohol removing agent/impurity removing agent or distillation purification, the method is economical and has better effects and considerable economic benefits.

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 method for preparing electronic-grade ethylene carbonate by falling film crystallization. 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 widely used in the lithium-ion b...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D317/38H01M10/0569
CPCY02E60/10
Inventor 王红星柴士阳盖晓龙刘伯潭
Owner TIANJIN UNIVERSITY OF SCIENCE AND TECHNOLOGY
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