Bis(fluorosulfonyl)amide Salt Production via Thin-Film Evaporation
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Solution Overview
Problem
Existing methods for producing bis(fluorosulfonyl)amide alkali metal salt powders face challenges in achieving high purity while minimizing yield reduction due to thermal decomposition, as the interaction between the salt and good solvents hinders precipitation, leading to lower yields.
Innovation Solution
A method involving distillation using a thin-film evaporator with a poor solvent added to a solution of bis(fluorosulfonyl)amide alkali metal salt in a good solvent, where the equilibrium vapor pressure of the good solvent is higher than that of the poor solvent, and a specific thin-film evaporator design with a rotor blade for efficient evaporation and precipitation.
Engineering Contradictions & Design Principles
Engineering Contradiction Analysis
1Manufacturing precision
If a solution of fluorosulfonyl imide alkali metal salt is concentrated by distilling off reaction solvent in the presence of both reaction solvent and poor solvent, then the fluorosulfonyl imide alkali metal salt can be obtained, but thermal decomposition occurs when heated over a long term leading to reduced yield
Solution Approach 1:
The patent applies preliminary action by conducting distillation under reduced pressure at a lower temperature regime before complete concentration occurs. This preliminary removal of reaction solvent at controlled conditions prevents thermal decomposition that would occur during prolonged heating, thereby maintaining high yield while achieving the necessary concentration for salt precipitation.
Solution Approach 2:
The patent changes the pressure parameter by conducting distillation under reduced pressure rather than atmospheric pressure. This parameter change allows the distillation process to occur at lower temperatures, preventing thermal decomposition of the fluorosulfonyl imide alkali metal salt while still achieving effective solvent removal and salt precipitation.
2Ease of manufacture
If the reaction solvent is previously removed using a thin-film evaporator before the concentration step, then the concentration process is simplified, but the interaction between salt and good solvent hinders precipitation leading to lower yield
Solution Approach 1:
The patent extracts the reaction solvent from the solution using distillation under reduced pressure, separating it from the fluorosulfonyl imide alkali metal salt and poor solvent mixture. This extraction approach allows controlled removal of the good solvent while maintaining conditions that promote salt precipitation, avoiding the yield loss associated with simple concentration methods.
3Device complexity
If conventional distillation methods are used to concentrate the solution, then the process is simpler, but only viscosity increases and precipitation is unlikely to occur
Solution Approach 1:
The patent changes the pressure parameter by conducting distillation under reduced pressure, which fundamentally alters the evaporation and precipitation behavior. This parameter change enables effective solvent removal and salt precipitation to occur simultaneously, overcoming the limitation of conventional distillation where only viscosity increases without precipitation.
Applied Scientific Principles
This section explains which scientific principles are used to turn an abstract innovation direction into a practical engineering solution.
Function Achieved in This Case
This method effectively produces bis(fluorosulfonyl)amide alkali metal salt powder with high purity in a shorter time while preventing yield reduction from thermal decomposition, by ensuring the good solvent is vaporized and the poor solvent remains for precipitation, enhancing separation efficiency.
Implementation Method 1
conducting distillation using a thin-film evaporator while adding a poor solvent to a solution formed by dissolving the bis(fluorosulfonyl)amide alkali metal salt in a good solvent
Implementation Method 2
conducting distillation using a thin-film evaporator while adding a poor solvent to a solution
Implementation Method 3
a stirring apparatus comprises a vertical rotation axis and a rotor blade capable of pumping up a liquid accumulated on a bottom part of the vessel by a centrifugal force and squirting the pumped-up liquid on an upper part of the wall inside the vessel
Implementation Method 4
the squirted liquid naturally flows down along the wall inside the vessel, during which evaporation of the liquid is caused
Data Source
AI summary
An object of the present invention is to provide a method for producing a bis(fluorosulfonyl)amide alkali metal salt powder having high purity while suppressing reduction in yield due to thermal decomposition, etc. The method for producing a bis(fluorosulfonyl)amide alkali metal salt powder according to the present invention comprises precipitating a bis(fluorosulfonyl)amide alkali metal salt by conducting distillation using a thin-film evaporator while adding a poor solvent for the bis(fluorosulfonyl)amide alkali metal salt such as an aromatic hydrocarbon solvent and a linear or branched aliphatic hydrocarbon solvent to a solution formed by dissolving the bis(fluorosulfonyl)amide alkali metal salt in a good solvent for the bis(fluorosulfonyl)amide alkali metal salt such as an ester solvent and nitrile solvent.

