HRID845561

反应详情

EQUATION

反应方程式

HRID 845561 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

225 parts of polyphosphoric acid (P2O5 content 85.5%) are heated to 50° C. 3.75 parts of methanol are then added dropwise in the course of 10 minutes. After stirring for 30 minutes the mixture is raised to 100° C. and is stirred at this temperature for 2 hours. It is then raised to 120° C. On reaching this temperature 50 parts of 2,5-dianilinoterephthalic acid are added with stirring in the course of 1 hour. After the mixture has been stirred at 120° C. for a further hour 1 part of distearyldimethylammonium chloride is added, and the mixture is stirred at 120° C. for a further hour. The melt is then hydrolyzed with 300 parts of ice and 375 parts of water. The crude quinacridone is separated off by filtration and is washed with water until neutral. The water-moist crude quinacridone is suspended in 300 parts of water and 75 parts of 10% strength potassium hydroxide solution are added. The suspension thus obtained is bulked to 750 parts with water and is then boiled with stirring for 7 hours. The suspended particles are then filtered off and washed with water until neutral. The isolated neutral moist quinacridone is suspended in 300 parts of 80% strength isobutanol, the suspension is stirred at 150° C. in a sealed vessel for 5 hours, and the quinacridone is then isolated as described in Example 1. Drying produces 44.5 parts of bluish red pigment of the pure γ-crystal modification. To measure the gloss, a casting was prepared on plastic film and measured, both steps being carried out as described in Example 1. The gloss value is 52.1.

WORKUP

后处理

  1. stirringis stirred at this temperature for 2 hours
  2. temperatureIt is then raised to 120° C
  3. additionare added
  4. stirringwith stirring in the course of 1 hour
  5. additionis added
  6. stirringthe mixture is stirred at 120° C. for a further hour
  7. customThe crude quinacridone is separated off by filtration
  8. washis washed with water until neutral
  9. additionare added
  10. customThe suspension thus obtained
  11. stirringwith stirring for 7 hours
  12. filtrationThe suspended particles are then filtered off
  13. washwashed with water until neutral
  14. stirringthe suspension is stirred at 150° C. in a sealed vessel for 5 hours