反应详情

温度

95 °C

To 300 g of polyphosphoric acid (117% phosphoric acid) heated at 90° C. was added 0.7 g of copper phthalocyanine followed by 68.2 g of 2,5-dianilinoterephthalic acid. The mixture was heated at 120°-125° C. for two hours. After the melt was cooled to 95° C., the acid strength was adjusted to 112% by the dropwise addition of phosphoric acid. The resultant melt was stirred for 15 minutes and then slowly poured into 453 g of methanol at 24° C. During the drown, the temperature was allowed to increase to 55° C., with the temperature being controlled by external cooling and adjustment of melt addition rate. The slurry was heated at reflux (68°-72° C.) for one hour, diluted with water, and stirred at 60° C. for 30 minutes. The solid component was collected by filtration and washed with water until acid free. The resultant presscake was reslurried in water. After adjustment of the pH to greater than 7, 7.5 g of 50% sodium hydroxide was added and the resultant slurry was heated at 90° C. for one hour. The slurry was cooled, filtered, and washed with water until alkali free, then reslurried in water. After adjustment of the pH to greater than 8.5, 3.2 g of a cycloaliphatic carboxylic acid was added. The resultant slurry was heated at about 140°-145° C. for two hours in a closed system, cooled, acidified with phosphoric acid, and stirred. The solid component was collected by filtration and washed with water. The wet cake can be dried or used as is for specific applications. Here, the wet cake was dried in an oven at 60° C. to give approximately 54.0 g of quinacridone as a brilliant violet pigment.

1. temperatureThe mixture was heated at 120°-125° C. for two hours
2. temperatureto increase to 55° C., with the temperature
3. temperatureby external cooling
4. additionadjustment of melt addition rate
5. temperatureThe slurry was heated
6. temperatureat reflux (68°-72° C.) for one hour
7. stirringstirred at 60° C. for 30 minutes
8. filtrationThe solid component was collected by filtration
9. washwashed with water until acid free
10. additionAfter adjustment of the pH to greater than 7, 7.5 g of 50% sodium hydroxide was added
11. temperaturethe resultant slurry was heated at 90° C. for one hour
12. temperatureThe slurry was cooled
13. filtrationfiltered
14. washwashed with water until alkali free,
15. additionAfter adjustment of the pH to greater than 8.5, 3.2 g of a cycloaliphatic carboxylic acid was added
16. temperatureThe resultant slurry was heated at about 140°-145° C. for two hours in a closed system
17. temperaturecooled
18. stirringstirred
19. filtrationThe solid component was collected by filtration
20. washwashed with water
21. customThe wet cake can be dried
22. customHere, the wet cake was dried in an oven at 60° C.