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  • 1
    Electronic Resource
    Electronic Resource
    Springer
    Journal of thermal analysis and calorimetry 49 (1997), S. 1625-1633 
    ISSN: 1572-8943
    Keywords: Grignard reaction ; process development ; process safety ; reaction calorimetry
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract A Grignard reaction of reactantA and phenyl magnesium chloride is used to make a pharmaceutical intermediate at the production scale. The elimination of protecting groups onA was proposed as a means to reduce synthesis costs. This new synthesis route, however, had process efficiency and safety issues associated with it: (1) build-up of unreactedA in the reactor, (2) influence ofA's particle size on the reaction rate, (3) the sensitivity of the reaction rate to the reaction temperature and to the (changing) solvent composition, and (4) the highly exothermic nature of the reaction. The Mettler RC1 Reaction Calorimeter was used to quantify the influence of solvent composition, temperature, and particle size on the reaction rate. Results indicated a dramatic effect of solvent composition and reaction temperature on the reaction rate; for example, over a temperature range of just 30°C, the reaction time decreased from more than a day to just a few minutes. At such high reaction rates, the vessel jacket could not remove the reaction heat sufficiently and the internal temperature rose adiabatically. These results were used to make process design and operation recommendations for safe and efficient plant operation with this modified Grignard reaction system.
    Type of Medium: Electronic Resource
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  • 2
    Electronic Resource
    Electronic Resource
    New York, NY [u.a.] : Wiley-Blackwell
    Process Safety Progress 14 (1995), S. 71-76 
    ISSN: 1066-8527
    Keywords: Chemistry ; Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Process Engineering, Biotechnology, Nutrition Technology
    Notes: An ARCTM or similar experimental apparatus provides the transient temperature history of a chemical system under adiabatic conditions. The information obtained has several applications in the design and operation of industrial systems. Of particular interest is use of the adiabatic kinetic data to define “intervention strategies” based on “allowable response times” during an emergency.The time-temperature behavior of industrial reactors can be simulated over a limited temperature range by matching the “thermal inertia” (or φ-factor) of the experimental system to that of the full-scale system. This approach is applicable even for complex reactions, minimizes the extrapolation of data, and allows the use of simple models for data interpretation. Simulation results directly give the time available to respond in the event of a thermal runaway; this in turn defines the design requirements for an intervention scheme (e.g., emergency cooling, blow down, quench, etc.). The chosen intervention system can be tested experimentally prior to and/or during process start-up.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
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