Method for removing moisture and chloride ions in fluoroethylene carbonate

A technology for fluoroethylene carbonate and crude ethylene carbonate, applied in the field of purification, can solve the problems of large fluctuations in chloride ion content, lack of chlorine ion removal process, high moisture content, etc., to avoid large area of ​​crystal sticking to the wall and avoid energy consumption Larger, uniform particle size effect

Pending Publication Date: 2021-12-28
ZHUHAI LEE & MAN MATERIALS SCI CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But this method has the following disadvantages: the first is that due to the high boiling point of fluoroethylene carbonate itself, the energy consumption of the multi-stage rectification method is very large, which is not conducive to the energy saving and emission reduction of enterprises; the second is that the residual moisture content is relatively high high
[0004] Most of the preparation methods about fluoroethylene carbonate reported at present are obtained by fluorination reaction between chloroethylene carbonate and potassium fluoride. This preparation method will inevitably cause obvious residual chloride ions in the product. Post-treatment Most of the purification methods used in purification are directly distilling the crude product, lac

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] In a 200L reactor, 108kg of crude fluoroethylene carbonate and 72kg of anhydrous dimethyl carbonate were added, and then 10.8kg of calcium hydride was added for stirring reaction, and the stirring speed of the stirring blade was set at 350rpm. The Karl Fischer water measurement method is used for on-line monitoring to measure the water content, and the pH meter is used to monitor the pH value on-line. When the water content is less than or equal to 20ppm and the pH is neutral, stop stirring, let stand for 2 hours and wait for the solid-liquid separation, then transfer the supernatant liquid to a centrifuge for centrifugation, and then transfer the obtained centrifuged liquid to a filter for filtration. The obtained clear liquid is transported to a temperature-controllable crystallization tank. Start the stirring system, the stirring rate is 250rpm, the temperature control system is set to drop from the initial 30°C to the end point 8°C, and the temperature drop time is ...

Embodiment 2

[0025] The operation of this example is basically the same as that of Example 1, except that the dissolved organic solvent of this example is changed to toluene. The final weight of the product obtained in this embodiment is 97.4kg. Yield: 90.2%. Take the liquid for analysis. GC-MS purity 99.95%. Trace detection results: ICP-OES (ppm): K + =3.422ppm, Na + =4.274ppm, Fe 2+ = 0.186ppm, Ca 2 + = 8.071ppm; Mg 2+ = 0.314ppm; IC: F － = 1.34ppm, Cl － =5.33ppm, NO 3 － =3.51ppm, SO 4 2- = 1.23ppm, PO 4 3- = 1.86ppm. KF: H 2 O=7.88ppm.

Embodiment 3

[0027] The operation of this embodiment is basically the same as that of Embodiment 1, except that the alkaline desiccant of this embodiment is lithium hydride. The final weight of the product obtained in this embodiment is 96.2kg. Yield: 89.1%. Take the liquid for analysis. GC-MS purity 99.95%. Trace detection results: ICP-OES (ppm): K + = 1.902ppm, Na + =8.218ppm, Fe 2+ = 0.093ppm, Ca 2 + = 1.933ppm; Mg 2+ = 0.163ppm; IC: F － =4.14ppm, Cl － =8.05ppm, NO 3 － =4.71ppm, SO 4 2- =5.03ppm, PO4 3- = 0.93 ppm. KF: H 2 O = 9.01 ppm.

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Abstract

The invention discloses a method for removing water and chloride ions in fluoroethylene carbonate, which comprises the following steps of: removing water by using an alkaline drying agent until the water content is less than or equal to 30ppm, so that no metal cation pollution is generated after the reaction, removing the chloride ions, and dynamically cooling and crystallizing, so that the obtained crystal is uniform in size and can be prevented from being adhered to the wall in a large area; the method is easy to operate in the subsequent filtering process, heating is not adopted in the whole water removal process, operation is easy and convenient, and the problems that a traditional heating distillation method is large in energy consumption, tedious in step, low in efficiency and high in water content are solved.

Description

Technical field: [0001] The invention relates to the technical field of purification, in particular to a method for removing moisture and chloride ions in fluoroethylene carbonate. Background technique: [0002] Fluoroethylene Carbonate (FEC) as a lithium battery electrolyte additive, not only can form a tight structure layer without increasing the electrolyte impedance, but also can prevent the electrolyte from further decomposition, has good high and low temperature performance and anti- Inflatable function. At the same time, it can also promote the formation of SEI film, improve the cycle performance of the battery, and improve the overall performance of the electrolyte. [0003] In order to obtain higher purity fluoroethylene carbonate, the industry usually adopts the method of multi-stage rectification to carry out purification. But this method has the following disadvantages: the first is that due to the high boiling point of fluoroethylene carbonate itself, the ener...

Claims

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Application Information

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IPC IPC(8): C07D317/42
CPCC07D317/42
Inventor 辛伟贤梁海波谢文健陈新滋
Owner ZHUHAI LEE & MAN MATERIALS SCI CO LTD
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