Bis(halosulfonyl)amine Production via Dynamic Temperature Control
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Solution Overview
Problem
The existing methods for producing bis(halosulfonyl)amine require high temperatures, leading to rapid gas generation and excessive loss of halogenating agents, making them unsuitable for industrial production.
Innovation Solution
A method involving heating a mixture of sulfamic acid and halosulfonic acid to 50°C to 140°C, with gradual addition of a halogenating agent like thionyl chloride, controlling the reaction rate to prevent rapid gas generation and optimizing the temperature to maintain a constant rate throughout the reaction.
Engineering Contradictions & Design Principles
Engineering Contradiction Analysis
1Productivity
If the temperature is raised to 80°C or higher to complete the reaction, then the reaction completion is improved, but the thionyl chloride evaporates and is eliminated from the reaction system
Solution Approach 1:
The patent applies dynamic temperature control by dividing the reaction into two stages: initially maintaining a lower temperature (0°C to 50°C) to prevent thionyl chloride evaporation, then raising the temperature (50°C to 140°C) in the later stage to ensure reaction completion. This dynamic adjustment of temperature throughout the reaction process resolves the contradiction between preventing substance loss and achieving complete reaction.
Solution Approach 2:
The patent applies preliminary action by first mixing sulfamic acid and halosulfonic acid at a lower temperature before adding the halogenating agent, and maintaining this lower temperature during the initial reaction phase. This preliminary temperature control prevents thionyl chloride evaporation before the reaction fully progresses, thereby preventing substance loss while still allowing complete reaction later.
2Loss of substance
If the temperature is lowered early in the reaction to prevent thionyl chloride evaporation, then the loss of thionyl chloride is reduced, but a large amount of gas may be generated rapidly when switching to the final reaction temperature
Solution Approach 1:
The patent applies dynamic temperature control to gradually raise the temperature from the initial lower stage (0°C to 50°C) to the final higher stage (50°C to 140°C). This gradual temperature transition prevents rapid gas generation that would occur with sudden temperature switching, while still achieving the necessary temperature for complete reaction and preventing thionyl chloride loss.
Solution Approach 2:
The patent applies periodic action by dividing the temperature control into distinct periods: an initial period at lower temperature to prevent evaporation, followed by a temperature raising period to ensure reaction completion. This periodic temperature management prevents both thionyl chloride loss and rapid gas generation by controlling the reaction rate throughout different stages.
3Productivity
If excess thionyl chloride is added to compensate for evaporation, then the reaction completion is improved, but the amount of halogenating agent used increases
Solution Approach 1:
The patent applies dynamic temperature control to maintain lower temperature (0°C to 50°C) during the phase when thionyl chloride is most vulnerable to evaporation, then raises temperature (50°C to 140°C) when the reaction is already progressing. This dynamic approach ensures reaction completion while minimizing thionyl chloride evaporation, thereby reducing the need for excess agent addition.
Solution Approach 2:
The patent applies preliminary action by establishing optimal temperature conditions before adding the halogenating agent and maintaining these conditions during the critical initial reaction phase. This preliminary temperature control prevents thionyl chloride evaporation from occurring in the first place, eliminating the need to compensate with excess agent addition.
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 approach inhibits rapid gas generation and reduces the amount of halogenating agent used, enabling high-yield industrial production of bis(halosulfonyl)amine.
Implementation Method 1
heating a mixture containing sulfamic acid and a halosulfonic acid to a temperature of 50°C to 140°C, followed by adding a halogenating agent thereto
Implementation Method 2
If the temperature of a mixture containing thionyl chloride is raised to 80°C or higher, the thionyl chloride evaporates and is eliminated from the reaction system
Data Source
AI summary
The present invention provides an industrially advantageous method for producing bis(halosulfonyl)amine that makes it possible to inhibit the rapid generation of gas and reduce the amount of halogenating agent used by controlling the reaction rate among sulfamic acid, the halogenating agent and a halosulfonic acid to nearly a constant rate from the initial stage to the final stage of the reaction. The method for producing bis(halosulfonyl)amine of the present invention allows the obtaining of a bis(halosulfonyl)amine such as N-(fluorosulfonyl)-N-(chlorosulfonyl)amine or bis (chlorosulfonyl)amine by a production method that includes heating a mixture containing sulfamic acid and a halosulfonic acid to a temperature higher than room temperature, adding a halogenating agent thereto, and allowing to react while adjusting to a prescribed temperature.