反应详情

温度

15 °C

52.0 g of 1,4-diaminoanthraquinone (92% pure) and 47.0 g of 1-aminoanthraquinone (98% pure) are dissolved in 512 g of 96% strength H2SO4 and this solution is added dropwise, with efficient stirring, to 460 g of water within 30 minutes. After cooling to about 15° C., 110.0 g of potassium peroxodisulphate are added, with efficient stirring, within about 3 hours and the mixture is allowed to warm slowly to 20° C. The melt is stirred at about 20° C. for 2-3 hours and then added to a mixture of 600 ml of water and 150 ml of 40% strength NaHSO3 solution and, after addition of a defoamer, the mixture is heated to 80°-90° C. in 30 minutes. After 30 minutes at 80°-90° C., the solid is filtered off hot with suction, washed with water to neutrality and dried at 100° C. 97.4 g of 4,4'-diamino-1,1'-dianthrimide (81% pure), corresponding to 86% of theory, were obtained.

1. temperatureto warm slowly to 20° C
2. additionafter addition of a defoamer
3. temperaturethe mixture is heated to 80°-90° C. in 30 minutes
4. waitAfter 30 minutes at 80°-90° C.
5. filtrationthe solid is filtered off hot with suction
6. washwashed with water to neutrality
7. customdried at 100° C