Formaldehyde → Formaldehyde;phenol
Reaction equation
[C:1]1([OH:7])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.C=O.O.N>>[CH2:1]=[O:7].[C:1]1([OH:7])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1Participants
Procedure
48.0 g of phenol and 82.6 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 3.8 g of 29% ammonia water and stirring for mixing. The resultant solution was reacted at a temperature of 70-80° C. for 6.5 hours on a mantle heater. After the reaction, the reaction product was cooled to room temperature to obtain 78 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 to obtain 60 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 1200° C. at a rate of 5° C./min and held at 1200° 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.
Workup
- customequipped with a Dimroth condenser
- additionfor mixing
- stirringstirring
- additionfor mixing
- customAfter the reaction
Sources & evidence
- ORD record
- ord-86df9ca8ff4543ce885462fc8e98be2b
- Source dataset
- uspto-grants-2003_05
- Patent number
- US06569570B2
Reaction notes
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