HRID972046

反应详情

EQUATION

反应方程式

HRID 972046 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
70 °C

PROCEDURE

实验过程

Water (17 L) was added to stearyl phosphate (molar ratio of diester/monoester=1/7.7; acid value, 278.6 mg KOH/g) (1 kg) while heating at 70° C., whereby the stearyl phosphate was dispersed uniformly. An aqueous solution of sodium hydroxide (500 g/L) (398 ml) was dropwise added to the mixture while keeping the said temperature. When the addition was finished, the mixture showed a pH of about 11. Further, stirring was continued at 70° C. for 60 minutes. An aqueous solution of calcium nitrate (200 g/L) (2083 ml) was gradually added at a temperature of 60° to 70° C. After the addition was finished, the mixture was stirred at 60° C. for 60 minutes. On confirming that the remaining calcium ion in water became constant, the reaction was finished. The product was collected, washed with water, filtered, dried at 75° C. for 72 hours and pulverized by the aid of a hammer mill to give calcium stearyl phosphate (1029 g). Yield, 94%. M.P., >250° C. Apparent specific volume, 5.5 ml/g. Elementary analysis: calcd, P=7.5%, Ca=9.1%; found, P=7.3%, Ca=9.0%.

WORKUP

后处理

  1. additionWhen the addition
  2. additionAfter the addition
  3. stirringthe mixture was stirred at 60° C. for 60 minutes
  4. customThe product was collected
  5. washwashed with water
  6. filtrationfiltered
  7. customdried at 75° C. for 72 hours