The fabrication of a catalytic microreactor for the reaction of undiluted carbonyl difluoride and elemental fluorine to synthesize trifluoromethyl hypofluorite, CF3OF, on CsF catalyst supported on F2-passivated nanosctructured Ni coating was studied. The nanosctructured Ni support for catalyst immobilization was electrodeposited by a two-step procedure, consisting of a low current density step followed by a brief high current density one, for a hierarchical differentiation of structural features. An aqueous solution of NiCl2with diethanolamine, as crystal modifier, and sodium lauryl sulphate, as anti-pitting agent, was used as electrolyte. Constant-pH Ni electrocrystallization was performed on H2SO4-etched Cu substrates in a range of pH from 1 to 4 via a HCl/H3BO3based buffer. Passivation was carried out under up to 300 mbar of undiluted F2. XRD, XPS, SEM, AFM, and static contact angle measurements were performed. Ni coatings obtained from pH 3 electrolytes were selected for microreactor fabrication on the basis of characterization data, due to the reproducibility and homogeneity of the structured Ni layers. The catalytic microreactor allowed the quantitative production of CF3OF from pure reactants, on demand, and removing any criticality relative to thermal and safety control of the synthesis. The CF3O-group selective transfer ability of the synthetized hypofluorite has raised interest in pharmaceutical and agrochemical industries in recent years.

Catalytic microreactor with electrodeposited hierarchically nanostructured nickel coatings for gas-phase fluorination reactions

Sansotera, Maurizio;Baggioli, Alberto;Ieffa, Simona;Magagnin, Luca;Navarrini, Walter
2018

Abstract

The fabrication of a catalytic microreactor for the reaction of undiluted carbonyl difluoride and elemental fluorine to synthesize trifluoromethyl hypofluorite, CF3OF, on CsF catalyst supported on F2-passivated nanosctructured Ni coating was studied. The nanosctructured Ni support for catalyst immobilization was electrodeposited by a two-step procedure, consisting of a low current density step followed by a brief high current density one, for a hierarchical differentiation of structural features. An aqueous solution of NiCl2with diethanolamine, as crystal modifier, and sodium lauryl sulphate, as anti-pitting agent, was used as electrolyte. Constant-pH Ni electrocrystallization was performed on H2SO4-etched Cu substrates in a range of pH from 1 to 4 via a HCl/H3BO3based buffer. Passivation was carried out under up to 300 mbar of undiluted F2. XRD, XPS, SEM, AFM, and static contact angle measurements were performed. Ni coatings obtained from pH 3 electrolytes were selected for microreactor fabrication on the basis of characterization data, due to the reproducibility and homogeneity of the structured Ni layers. The catalytic microreactor allowed the quantitative production of CF3OF from pure reactants, on demand, and removing any criticality relative to thermal and safety control of the synthesis. The CF3O-group selective transfer ability of the synthetized hypofluorite has raised interest in pharmaceutical and agrochemical industries in recent years.
JOURNAL OF FLUORINE CHEMISTRY
Electrodeposition; Fluorination; Hierarchically nanostructured Ni; Hypofluorite; Microreactor; Passivation; Biochemistry; Environmental Chemistry; Physical and Theoretical Chemistry; Organic Chemistry; Inorganic Chemistry
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Utilizza questo identificativo per citare o creare un link a questo documento: http://hdl.handle.net/11311/1063566
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