반응 #514367

ord-1e11743c1dc648af83d1735ce9f92ae4

반응 방정식

O=C(O)c1cc(Nc2ccccc2)c(C(=O)O)cc1Nc1ccccc1
2,5dianilinoterephthalic acid
O=C(O)c1cc(Nc2cccc(Cl)c2)c(C(=O)O)cc1Nc1cccc(Cl)c1
2,5-di(3-chloroanilino)terephthalic acid
O=c1c2ccccc2[nH]c2cc3c(=O)c4ccccc4[nH]c3cc12
quinacridone

반응 조건

온도
125°CELSIUS
상세 조건
See reaction.notes.procedure_details.

실험 절차

450 parts of polyphosphoric acid containing 85.0% P2O5 are metered into a stirred vessel. Then 135 parts of 2,5dianilinoterephthalic acid and 15 parts of 2,5-di(3-chloroanilino)terephthalic acid are introduced at 125° C. with stirring and the mixture is heated at 125° C. for 1 hour during which ring closure takes place to form the quinacridone. The reaction midure is subsequently metered with stirring over 2 minutes (CG; 50%/min) into 2187.9 parts of 85% strength phosphoric acid at 140° C., during which it is hydrolyzed. During this hydrolysis the temperature rises to 155° C. The phosphoric acid concentration after the hydrolysis is 90%. Then 1768.9 parts of 40% strength phosphoric acid are added dropwise and the suspension is cooled to 120° C. The phosphoric acid concentration thereafter is 70%. The mixture is stirred at 120° C. for 1 hour. Subsequently the mixed crystal pigment is filtered off with suction at 110° C., washed with 70% strength phosphoric acid until the runoff is colorless, washed to neutrality with water, and dried at 80° C. This gives 132.8 parts of mixed crystal pigment (Pigment Violet 19, γII phase). At twice the Bragg angle, 2θ, X-ray spectrum shows three strong lines at 6.3°, 13.5° and 26.4°, four moderate lines at 16.6°, 20.6°, 24.0° and 28.3°, and one weak line at 30.3°. In the AM lacquer, transparent, pure and strongly colored coatings of deep hue are obtained. The rheology is evaluated as 3-4 and the viscosity is 4.5 s. The gloss measurement gives a value of 60.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US06312512B1uspto-grants-2001_11