Journal
INDUSTRIAL & ENGINEERING CHEMISTRY RESEARCH
Volume 62, Issue 3, Pages 1338-1349Publisher
AMER CHEMICAL SOC
DOI: 10.1021/acs.iecr.2c04631
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This study developed a two-step synthesis process for adiponitrile using a patented method. The Ni30Fe10/Al2O3-MgO(0.8:1.2)-700-2 catalyst showed high efficiency in the catalytic amination of 6-hydroxyhexanenitrile to adiponitrile. Under optimized conditions, the conversion rate of 6-hydroxyhexanenitrile reached 63.1% with a selectivity of 51.5% for adiponitrile, corresponding to a one-pass yield of 32.5%. The catalyst could be fully regenerated by high-temperature reduction with H2.
Adiponitrile, as an important bulk chemical, was synthesized in two steps: catalytic amination of epsilon-caprolactone to 6-hydroxyhexanenitrile over a ZnO catalyst through a patented process, followed by catalytic amination of 6-hydroxyhexanenitrile to adiponitrile. An Al2O3-MgO composite-supported bimetallic catalyst Ni30Fe10/Al2O3-MgO(0.8:1.2)-700-2 was found to be efficient in the catalytic amination of 6-hydroxyhexanenitrile to adiponitrile. Under the optimal reaction conditions, which are a reaction temperature of 300 degrees C, atmospheric pressure, 6-hydroxyhexanenitrile/NH3/H2 molar ratios of 1:5:2, and a residence time of 5 s, the conversion of 6-hydroxyhexanenitrile reached 63.1% with an adiponitrile selectivity of 51.5%, corresponding to a one-pass adiponitrile yield of 32.5%. The characterization results revealed that Ni and Fe are present in the form of Ni3Fe alloy nanoparticles with diameters of 8 to 16 nm in the catalyst Ni30Fe10/Al2O3-MgO(0.8:1.2)-700-2. The good catalysis of Ni30Fe10/Al2O3-MgO(0.8:1.2)-700-2 could be ascribed to the synergetic effect between the two metals in the Ni3Fe alloy and a suitable magnesium-to-aluminum molar ratio in the catalyst. Catalyst deactivation took place due to the deposition of carbonaceous substances on the surface of the catalyst in a catalytic run, and the deactivated catalyst could be regenerated fully by high-temperature reduction with H2.
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