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Purification method and purification device of electronic-grade ethylene carbonate

A technology of ethylene carbonate and purification method, applied in the direction of organic chemistry, etc., can solve the problems of low primary crystallization yield, low crystallization raw material purity, battery capacity attenuation, etc., and achieves the effect of small discoloration, low impurity content, and improved battery life.

Active Publication Date: 2020-04-14
DONGYING HI TECH SPRING CHEM IND
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Problems solved by technology

However, due to the low purity of the crystallization raw material used in this method, the removal rate of impurities entering the crystallizer for separation and purification is low. In order to obtain high-purity products, the amount of raffinate and sweating liquid is large, resulting in a low yield of primary crystallization. Sweat and residual fluid need to undergo multiple cycles of crystallization, which consumes a lot of energy
At the same time, due to the low removal rate of impurities during the reaction process, it is easy to change color under aerobic and high temperature conditions, which will cause the capacity of the battery to decay when it enters the electrolyte product, and the cycle life will be reduced

Method used

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  • Purification method and purification device of electronic-grade ethylene carbonate

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Effect test

Embodiment 1

[0057] (1) Seeding and cooling crystallization: Under the protection of inert gas, take the crude ethylene carbonate produced from the side line of the first rectification tower (the crude ethylene carbonate with a mass fraction of 99.98%) and add it from the top of the falling film crystallizer, and then The material rate is 1.5 t / h. After the feeding is completed, the material circulation pump is turned on, the cooling system is turned on, and a cold source of 20°C is used to stimulate the material to crystallize. When the material temperature drops to 31~32°C, it rebounds. The rebound temperature is After cooling down to the final temperature, seeding ends. After the seeding is completed, switch the temperature control plate heat exchanger, and pass steam to quickly raise the temperature of the circulating water to 36°C, and then keep the temperature constant after the temperature rises to 36°C (the time from the temperature rise to the end of the constant temperature is 25 ...

Embodiment 2

[0068] (1) Seeding and cooling crystallization: Under the protection of inert gas, take the crude ethylene carbonate produced from the side line of the first rectification tower (the crude ethylene carbonate with a mass fraction of 99.95%) and add it from the top of the falling film crystallizer, and carry out The material rate is 2.0 t / h. After the feeding is completed, turn on the material circulation pump, turn on the cooling system, and use a cold source of 25°C to stimulate the crystallization of the material. When the material temperature reaches 31~32°C, stop seeding when the temperature rebounds , after the seeding is completed, switch the temperature control plate heat exchanger, and pass steam to quickly raise the temperature of the circulating water to 36.5°C, and then keep the temperature constant after the temperature rises to 36.5°C (the time from the temperature rise to the end of the constant temperature is 25min, and the explosion generated The excess crystals ...

Embodiment 3

[0077] (1) Seeding and cooling crystallization: under the protection of an inert gas, take part of the crude ethylene carbonate produced from the side line of the first rectification tower (the crude ethylene carbonate with a mass fraction of 99.90%) and add it from the top of the falling film crystallizer. The feeding rate is 5.0t / h. After the feeding is completed, turn on the material circulation pump, turn on the cooling system, and use a cold source of 28°C to stimulate the crystallization of the material for 60 minutes. When the temperature of the material reaches 31~32°C, stop when the temperature rebounds After the seeding is completed, switch the temperature control plate heat exchanger, and pass steam to quickly raise the temperature of the circulating water to 36°C, and then keep the temperature constant after the temperature rises to 36°C (the time from the temperature rise to the end of the constant temperature is 30 minutes, and the The excess crystals produced by ...

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Abstract

The invention discloses a purification method and a purification device of electronic-grade ethylene carbonate, and belongs to the technical field of preparation of electronic-grade reagents. The purification method comprises the following steps: 1) seeding ethylene carbonate with a purity of 99.90%-99.98%; 2) after seeding is finished, raising the temperature to 36-37 DEG C, and keeping the constant temperature for 0.5-3 hours; 3) cooling and crystallizing after the temperature maintenance is finished; 4) carrying out heating-sweating on the crystals in a gradual heating manner, and carryingout the next round of crystallization on the obtained sweating water; 5) after sweating is finished, raising the temperature to melt the sweating crystals to obtain a first product with a purity of more than 99.995%; and 6) rectifying the non-crystallized mother liquor twice to obtain a second product with a purity of more than 99.990%. According to the purification method provided by the invention, electronic-grade ethylene carbonate with a purity of more than 99.995% can be obtained, meanwhile, sweating liquid is returned to a falling-film crystallizer, the raw material liquid is recycled, and the total yield is improved.

Description

technical field [0001] The invention relates to the technical field of preparation of electronic grade reagents, in particular to a purification method of electronic grade ethylene carbonate and a purification device thereof. Background technique [0002] Ethylene carbonate, also known as 1,3-dioxolane-2 ketone, ethylene carbonate, ethylene glycol carbonate, molecular formula C 3 h 4 o 3 , abbreviated as EC. Ethylene carbonate is an organic solvent and organic synthesis intermediate with excellent performance. It has the characteristics of high boiling point, low toxicity and corrosion. It is soluble in water, benzene, acetone and other solvents, and can dissolve polyvinyl chloride, polyacrylonitrile, etc. . Ethylene carbonate can be used as a spinning solution for textiles; it can also be directly used as a solvent for removing acid gases and as an additive for concrete; it can be used as a component and raw material of raw materials in the pharmaceutical field; it can ...

Claims

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Application Information

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IPC IPC(8): C07D317/38
CPCC07D317/38
Inventor 燕增伟吴雷雷张生安杜桂强宋云瑞郝小军张庆博
Owner DONGYING HI TECH SPRING CHEM IND
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