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Designing a safer process for the reaction of TFA with sodium borohydride in THF by calorimetric technique

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Abstract

Reaction of TFA with sodium borohydride in THF is a loss of thermal control involving the evolution of Hydrogen gas. The investigation of the process by RC1e and ARSST showed that the criticality class of the reaction is dependant on the addition of TFA. Heat of reaction (Q r), adiabatic temperature rise (ΔT ad), and MTSR data are obtained from RC1e experiment. Exothermic onset temperature, Pressure rise, and self heat rate data are obtained from ARSST experiments. The correlation of these data was utilized to define the criticality class of the reaction under different conditions. The reaction with uncontrolled addition of TFA falls in the undesirable criticality class 5. Vent size data are obtained from the adiabatic calorimeter for undesirable reaction. The criticality class can be changed to class 2 with controlled addition. Accordingly, interlock system to control the undesired reaction and appropriate vent relief system are provided.

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Abbreviations

Q r :

Heat of reaction (kJ)

C p :

Specific heat of the reaction mass (kJ kg−1 K−1)

M r :

Quantity of the reaction mass (kg)

U :

Overall heat transfer coefficient (W m−2 K−1)

ΔT ad :

Adiabatic temperature rise (°C)

T cf :

Maximum temperature at cooling failure (°C)

T p :

Process temperature (°C)

T o :

Exotherm onset temperature (°C)

T f :

Final temperature (°C)

(dT/dt)max :

Maximum rate of temperature rise (°C min−1)

kPa:

Kilo Pascals

psig:

Pounds per square inch (gauge)

T D24 :

Temperature at which time to maximum rate adiabatic is 24 h (°C)

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Acknowledgements

We thank Mr. Sunil Kulkarni (Head, Corporate EHS), Dr. Ramesh Dandala (Head, API-R&D), and Dr. Hari Babu (COO) for their support and encouragement.

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Authors and Affiliations

  1. Process Safety Lab, Research & Development Center-API, Mylan Laboratories Limited (Formerly known as Matrix Laboratories Ltd), Plot No. 34A, ANRICH Industrial Estate, Bollaram, Jinnaram Mandal, Medak Dt., Andhra Pradesh, 502325, India

    Srinivasarao Veedhi

  2. Department of Environmental, Health and Safety, Research & Development Center-API, Mylan Laboratories Limited (Formerly known as Matrix Laboratories Ltd.), Plot No. 34A, ANRICH Industrial Estate, Bollaram, Jinnaram Mandal, Medak Dt., Andhra Pradesh, 502325, India

    Anil Sawant

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  1. Srinivasarao Veedhi
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  2. Anil Sawant
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Correspondence to Srinivasarao Veedhi.

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Veedhi, S., Sawant, A. Designing a safer process for the reaction of TFA with sodium borohydride in THF by calorimetric technique. J Therm Anal Calorim 111, 1093–1097 (2013). https://doi.org/10.1007/s10973-012-2514-0

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  • DOI: https://doi.org/10.1007/s10973-012-2514-0

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