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This chapter provides a description of necessary infrastructure for operation of lab-scale, high-pressure reactors. Furthermore, practical hints to improve the selection of the proper design and operation of a reactor vessel, with a focus on material selection and optimization concerning gas–liquid mass transport and heat removal, are discussed. The discussion is directed to improving reaction yields in order to approach the kinetic regime. For the risk assessment of liquid-phase hydrogenation, the hydrogen specific risks need to be considered, especially under the more severe reaction conditions, which are often required for conversion of biomass. Herein, a discussion of a variety of important safety parameters for the operation of larger autoclaves (≥ 500 mL), is given at an introductory level.

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