Phthalonitrile → Phthalocyanine

Participants

Reaction Conditions

Reaction Steps

Phthalonitrile (1100 grams) and titanium tetrachloride (813 grams) were suspended in 6800 ml of 1-chloronaphthalene and heated to 215°-220° C. and maintained for 2.5 hours at this temperature. The reaction mixture was cooled to 140° C., and the dark solid was collected, and washed with acetone, and methanol. After drying, the dark blue solid (1090 grams) was refluxed five times for two hours in 10 liters of distilled water, filtered, to yield crude titanyl phthalocyanine. The x-ray diffraction spectrum (FIG. 1) exhibited major peaks of the Bragg angle at 7.5°, 8.3°, 10.5°, 12.7°, 14.2°, 14.6°, 18.9°, 22.1°, 24.3°, 26.1°, 29.9° (all +/-0.2°).

Provenance & Evidence