反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 85 °C
PROCEDURE
实验过程
Water (20 L) was added to stearyl phosphate (molar ratio of diester/monoester=1/0.25; acid value, 121.9 mg KOH/g) (1 kg) while heating at 85° C., whereby the stearyl phosphate was dispersed uniformly. An aqueous solution of sodium hydroxide (500 g/L) (174 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 85° C. for 60 minutes. An aqueous solution of calcium chloride (300 g/L) (408 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 90 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 in a mortar to give calcium stearyl phosphate (1011 g). Yield, 97%. M.P., 110° to 118° C. Apparent specific volume, 3.5 ml/g. Elementary analysis: calcd., P=5.4%, Ca=4.2%; found, P=5.3%, Ca=4.1%.
WORKUP
后处理
- additionWhen the addition
- additionAfter the addition
- stirringthe mixture was stirred at 60° C. for 90 minutes
- customThe product was collected
- washwashed with water
- filtrationfiltered
- customdried at 75° C. for 72 hours