Phthalonitrile → Dichlorotitanium phthalocyanine

Temperature

225 °C

40 g of o-phthalodinitrile, 18 g of titanium tetrachloride, 500 ml of α-chloronaphthalene were reacted by heating and stirring at 200 to 250° C. for 3 hours in a nitrogen atmosphere, and after standing to cool to a temperature of from 100 to 130° C., the mixture was filtered under hot. 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 with 200 ml of a-chloronaphthalene at room temperature, and after further washing with 200 ml of methanol, the crude product was further washed by suspending under heating in 500 ml of methanol for 1 hour. After filtration, the resulting crude product was dissolved by stirring in 100 ml of concentrated sulfuric acid, and insoluble matters were removed by filtration. The sulfuric acid solution was poured into 3,000 ml of water, and deposited crystals were filtered. The crystals were repeatedly washed by suspending under heating in 500 ml of water until pH became 6 to 7, and then filtered to obtain a wet cake. The wet cake was treated with monochlorobenzene, and the subjected to a methanol treatment and then a cyclohexane treatment, followed by drying to obtain a first crystalline substance.

1. temperatureby heating
2. temperatureto cool to a temperature of from 100 to 130° C.
3. filtrationthe mixture was filtered under hot
4. washThe reaction product was washed with 200 ml of α-chloronaphthalene
5. temperatureheated to 100° C.

ORD record

ord-7b6b2b04622f4650b0e986dd2cb19700

Source dataset

uspto-grants-2001_09

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06291120B1