Purification device and method of bis (trifluoromethanesulfonyl) imine

Abstract

The invention provides a bis (trifluoromethanesulfonyl) imine purification device which comprises a mixing kettle, the bottom of the mixing kettle is connected with a rectifying tower, the top of the rectifying tower is sequentially connected with a trifluoromethanesulfonyl chloride condenser and a bis-imine condenser, the bottom of the trifluoromethanesulfonyl chloride condenser is connected with a trifluoromethanesulfonyl chloride storage tank, and the bottom of the bis-imine condenser is connected with a bis-imine storage tank. The bottom of the diimine condenser is connected with a diimine storage tank; the invention also provides a method for purifying bis (trifluoromethanesulfonyl) imine by adopting the device, which comprises the following steps: adding crude bis (trifluoromethanesulfonyl) imine and high-purity water into the mixing kettle, stirring, then adding trifluoromethanesulfonyl chloride, introducing the uniformly mixed material into the rectifying tower, distilling off trifluoromethanesulfonyl chloride and water, then adjusting the parameters of the rectifying tower, and finally purifying the bis (trifluoromethanesulfonyl) imine. The high-quality bis (trifluoromethanesulfonyl) imine is obtained. According to the method, purification of bis (trifluoromethanesulfonyl) imine is completed by controlling the adding proportion of high-purity water, bis (trifluoromethanesulfonyl) imine and trifluoromethanesulfonyl chloride and rectification conditions.

Description

technical field [0001] The invention belongs to the technical field of fine chemicals, and in particular relates to a purification device and method of bis(trifluoromethanesulfonyl)imide. Background technique [0002] Bis(trifluoromethanesulfonyl)imide itself is an important acidic substance, which has very high practical value in chemistry. In organic chemistry, it is mainly used in acid-catalyzed reactions. In inorganic chemistry, it is mainly used to stabilize some inert ions, etc. In addition, bis(trifluoromethanesulfonyl)imide is an important material for synthesizing lithium bis(trifluoromethanesulfonyl)imide, and its purity determines the purity of lithium bis(trifluoromethanesulfonyl)imide. At present, the lithium battery industry has high requirements on the purity of lithium bis(trifluoromethanesulfonyl)imide, so it is required to prepare and purify high-purity bis(trifluoromethanesulfonyl)imide. [0003] As methods for preparing and purifying bis(trifluorometha...

AI Technical Summary

Problems solved by technology

Separating and purifying bis(trifluoromethylsulfonyl)imide from organic solvents has the disadvantages of poor operating environment, the danger of inflammability and explosion, high requirements for the purity of organic solvents, and the purity of obtained products cannot meet the requirements of high purity.

[0007] Chinese patent 201010617057.8 reports the ammonium salt or quaternary ammonium salt of perfluoroalkyl sulfonylimide and solvent to prepare perfluoroalkane with a concentration of 0.1% to 30%. ammonium or quaternary ammonium salt solution of sulfonylimide, and then undergo cationic transformation to obtain perfluoroalkylsulfonylimide acid solution, resulting in insufficient product purity

[0008] Chinese patent 201310616306.5 reported the reaction of bis(trifluoromethanesulfonyl)imide salt and sulfuric acid in the presence of silicon dioxide, high-purity nitrogen was introduced before the reaction, and purified by atmospheric distillation and rectification after the reaction Bis(trifluoromethanesulfonyl)imide, the purity obtained is higher, but involves more steps, and the removal efficiency of impurities is lower

[0009] Various methods for preparing and purifying bis(trifluoromethanesulfonyl)imide have been reported successively at home and abroad. acid, which cannot be removed only by vacuum distillation, and a variety of fluorosulfonylimide acids are solid at room temperature, which is prone to clogged pipes during acidolysis and distillation, which brings inconvenience to the operation

Using organic solvents for extraction and purification, high requirements for organic solvents, potential safety hazards, and poor operating environment

In addition, the purity of the product obtained by the above method can only reach 99%, which cannot meet the high purity requirements of the lithium battery industry.

Or the purity is higher, but more process steps are involved, and the removal efficiency of impurities is lower

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