Phthalonitrile → Dichlorotitanium phthalocyanine

Participants

Reaction Conditions

Reaction Steps

40 g of o-phthalodinitrile, 18 g of titanium tetrachloride and 500 ml of α-chloronaphthalene were reacted by heating and agitating in a nitrogen atmosphere at 200 to 250° C. for 3 hours, and after standing to cool to 100 to 130° C., filtered under hot, and the reaction product was washed with 200 ml of α-chloronaphthalene heated to 100° C. to obtain a crude product of dichlorotitanium phthalocyanine. The crude product was washed at room temperature with 200 ml of α-chloronaphthalene and then with 200 ml of methanol, and was further washed by suspending under hot in 500 ml of methanol for 1 hour. The crude product obtained by filtering was repeatedly washed by suspending under hot in 500 ml of water until the pH became 6 to 7, and it was dried to obtain TiOPc crystals. When the crystals were subjected to X-ray diffractiometry, the spectrum shown in FIG. 3 was obtained. It is understood from FIG. 3 that the crystals are crystalline TiOPc called Y type disclosed in JP-A 64-17066 having a maximum diffraction peak at a Bragg angle (2θ±0.2°) of 27.3° and diffraction peaks at Bragg angles (2θ±0.2°) of 9.5°, 9.7°, 11.7°, 15°, 23.5° and 24.1°.

Provenance & Evidence