Preparation method of tributylmethylphosphon bis(trifluoromethanesulfonyl)imide_Industrial additives

Background and overview[1]

Ionic liquid (ionic liqu plastic deodorant id) is a liquid substance composed entirely of ions. It is liquid at room temperature or low temperature (-97℃~100℃), so it is also called room temperature/low temperature molten salt (room/ low temperature molten salt), or liquid organic salt. There are many types of ionic liquids. According to different organic cations, ionic liquids can be divided into quaternary ammonium salts, quaternary phosphonium salts, nitrogen-containing heterocyclic onium salts, etc. Nitrogen-containing heterocyclic ionic liquids include imidazolium salts, Pyridinium salts, piperidine salts, pyrrolidine salts, etc. There are many kinds of anions that make up ionic liquids. Inorganic anions include F-, Cl-, Br-, I-, NO3-, CO32-, PF6-, BF4-, C2O42-, SO42-, PO43-, Al2Cl7-, etc., and organic anions Including CH3COO-, CF3SO3-, C4H9SO3-, CF3COO-, N(CF3SO2)2-, N(C2F5SO2)2-, N(C4F9SO2)2-, N[(CF3SO2) (C4F9SO2)]-, C(CF3SO2)3 -wait. Theoretically, there can be as many as 1018 types of ionic liquids. Tributylmethylphosphon bis(trifluoromethanesulfonyl)imide is one of them.

Preparation[1]

Tributylphosphine bis(trifluoromethanesulfonyl)imide is prepared as follows: Place 500g (2.48mol) tributylphosphine and 800mL dimethyl carbonate in a pressure vessel (replace the pressure vessel with nitrogen in advance air), react at 145°C and 1.4~1.5Mpa pressure for 8 hours to obtain a light yellow to brown solution. After cooling, a white solid precipitates; slowly add 418.69g (1.49mol) bis (1.49mol) while stirring at room temperature. The mL methanol solution of trifluoromethanesulfonyl)imide produces a large amount of antioxidant rd gas; then add 1.00g lithium bis(trifluoromethanesulfonyl)imide every 10 minutes until no more white precipitate is formed. Filter, distill the filtrate under reduced pressure to remove low-boiling matter, and dry it under vacuum conditions at 80°C for 6 hours to obtain 727.94g (two-step reaction yield of about 59%) colorless to light yellow methyltributylquaternaryphosphonium bis. (Trifluoromethanesulfonyl) imide salt.

Main reference materials

[1] CN201310532457.2 Preparation method of ionic liquid

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