反应 #1153151

ord-2e527bc5452b459e9b2815316c530f33

反应方程式

Cc1ccc(Nc2cc(C(=O)O)c(Nc3ccc(C)cc3)cc2C(=O)O)cc1
2,5-di(4-toluidino)terephthalic acid
O=C(O)c1cc(Nc2ccc(Cl)cc2)c(C(=O)O)cc1Nc1ccc(Cl)cc1
2,5-di(4-chloroanilino)terephthalic acid
O=c1c2ccccc2[nH]c2cc3c(=O)c4ccccc4[nH]c3cc12
quinacridone

反应条件

温度
125°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    workup.ADDITIONDuring this addition the temperature
  2. 2
    其他rises to 120° C
  3. 3
    workup.STIRRINGstirred at 125° C. for 1 hour

实验过程

A stirred vessel is charged with 1000 parts of polyphosphoric acid containing 85.0% P2O5. Then 75 parts of 2,5-di(4-toluidino)terephthalic acid and 60 parts of 2,5-di(4-chloroanilino)terephthalic acid are introduced at 90° C. with stirring over 25 minutes. During this addition the temperature rises to 120° C. The mixture is heated to 125° C. and stirred at 125° C. for 1 hour, and ring closure takes place to form the quinacridone. The reaction mixture is subsequently metered into a static mixer, model Kenics KMR (length: 10 cm, diameter: 9 mm, 8 elements, supplier: H. Ott, Neckargmünd) with a throughput of 3.3 parts by volume per hour in a volume flow of 27 parts by volume per hour of 70% strength phosphoric acid at 95° C. and is hydrolyzed in 0.9 second (a precipitate is formed). During hydrolysis, the temperature rises to 118° C. Following the hydrolysis the phosphoric acid strength is 77.7%. This gives 4905 parts of crude pigment suspension. After cooling to 60° C., the crude pigment suspension is filtered off with suction, washed to neutrality with water and dried at 80° C.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US06241814B1uspto-grants-2001_06