Formaldehyde → Formaldehyde;phenol

Participants

Reaction Steps

94.2 g of phenol (reagent-grade, available from Kanto Kagaku K.K.) and 80.6 g of 37%-formalin were placed in a separable flask equipped with a Dimroth condenser, and stirred for mixing therein, followed further by addition of 14.0 g of 20% sodium hydroxide aqueous solution and stirring for mixing. The resultant solution was reacted at a temperature of 85-95° C. for 6 hours on a mantle heater. After the reaction, the reaction product was cooled to room temperature to obtain 152 g of phenol-formaldehyde initial condensate. The initial condensate was placed in a vessel formed by a copper foil and cured at 150° C. for 12 hours in a drier (“EYELA NED-300”, available from Tokyo Rika Kiki K.K.) to obtain 95 g of a phenolic resin. Then, the phenolic resin was crushed to diameters of ca. 1-2 cm, heated to 600° C. at a rate of 200° C./h in a nitrogen gas atmosphere (normal pressure) and held at 600° C. for 1 hour for pre-calcination to obtain a carbon precursor. The carbon precursor was pulverized to form a powdery carbon precursor having an average particle size of 25 μm. Then, the powdery carbon precursor was charged in a vacuum calcination furnace, heated to 1100° C. at a rate of 5° C./min and held at 1100° C. for 1 hour for main calcination under a reduced pressure maintained at 1 kPa or below, followed by cooling to obtain a powdery carbonaceous material.

Provenance & Evidence