Phthalonitrile → Dichlorotitanium phthalocyanine

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Reaction Steps

In this comparative example, α-titanyloxyphthalocyanine was prepared by the method disclosed in Japanese Patent Application Laying-open No. 62-134651. That is, a mixture of 40 g of phthalodinitrile, 18 g of titanium tetrachloride, and 500 cc of chloronaphthalene was stirred at the temperature of 240° C. to 2500° C. for 3 hours in nitrogenous atmosphere to completely react with each other. The mixture was filtrated after the reaction, and as a result dichlorotitanium phthalocyanine was obtained. The obtained dichlorotitanium was mixed with 300 cc of concentrated ammonium solution to obtain a mixture. Then the mixture was heat-refluxed for 1 hour and subjected to the purification by using a Soxhlet extractor. Consequently, titanyloxyphthalocyanine was obtained by drying the purified product. The resultant titanyloxyphthalocyanine was confirmed as α-type crystal having an X-ray diffraction spectrum which is the same as the one shown in FIG. 3.

Provenance & Evidence