تفاعل #514376

ord-96434a85c5c74e248b9d0843f0c71406

ظروف التفاعل

درجة الحرارة
125°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.ADDITIONDuring this addition the temperature
  2. 2
    أخرىrises to 115° C
  3. 3
    workup.STIRRINGstirred at 125° C. for 1 hour during which ring closure

الإجراء التجريبي

1000 parts of polyphosphoric acid containing 83.0% P2O5 are metered into a stirred vessel. Then 180 parts of 2,5-dianilinoterephthalic acid and 20 parts of 2,5-di(3-chloroanilino) terephthalic acid are introduced at 90° C. with stirring over 60 minutes. During this addition the temperature rises to 115° C. The mixture is heated to 125° C. and stirred at 125° C. for 1 hour during which ring closure takes place to form the quinacridone. The reaction mixture is subsequently metered into a static mixer ®Kenics KMR (length 10 cm, diameter 9 mm, 8 elements, supplier: H. Ott, Neckargmüind) with a volume flow of 2.1 parts by volume per hour, into a volume flow of 44.5 parts by volume per hour of 85% strength phosphoric acid at 140° C., and is hydrolyzed in 0.34 second with the formation of a precipitate. The phosphoric acid concentration after the hydrolysis is 93%. This gives 6445 parts of crude pigment suspension. 6279 parts of crude pigment suspension are cooled to 120° C. and 4479 parts of 40% strength phosphoric acid at 25° C. are run in with stirring. Following the addition of phosphoric acid, the phosphoric acid concentration is 70%. The mixture is stirred at 120° C. for 3 hours. Subsequently, the crude mixed crystal pigment is diluted with 10,000 parts of water, filtered off with suction, washed to neutrality with water and dried at 80° C. This gives 102.6 parts of crude mixed crystal pigment.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US06312512B1uspto-grants-2001_11