Phthalonitrile → Dichlorotitanium phthalocyanine

Beteiligte Stoffe

Reaktionsbedingungen

Reaktionsschritte

First, 40 g of o-phthalodinitrile, 18 g of titanium tetrachloride and 500 ml of α-chloronaphthalene were heated and stirred in a nitrogen atmosphere at 200° C. to 250° C. for 3 hours to react the reactants and allowed to cool to 100° C. to 130° C., and then the reaction product was filtered off hot, washed with 200 ml of α-chloronaphthalene heated to 100° C. to obtain a crude product of dichlorotitanium-phthalocyanine. At room temperature, the crude product was washed with 200 ml of α-chloronaphthalene, and then washed with 200 ml of methanol, and further subjected to heat spray washing in 500 ml of methanol for 1 hour. After filtered, the resulting crude product was stirred and dissolved in 100 ml of concentrated sulfuric acid to filter off insolubles. The sulfuric acid solution was added to 3000 ml of water, and the resulting crystal was filtered off to be repeatedly subjected to heat spray washing with 500 ml of hot water until the pH thereof reached 6 to 7, and then filtered off again. The wet cake was treated with dichloromethane, washed with methanol, and then dried to obtain 32 g of a titanylphthalocyanine crystal showing an X-ray diffraction spectrum shown in FIG. 4 and having a structure represented by the following formula (I):

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