反応式
[P:1]([O-:21])([O-:20])([O:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH3:19])=[O:2].[OH-].[Na+].[Cl-].[Ba+2:25].[Cl-]>O>[P:1]([O-:20])([O-:21])([O:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH3:19])=[O:2].[Ba+2:25]参加物
反応条件
- 温度
- 70 °C
実験手順
Water (20 L) was added to cetyl phosphate (molar ratio of diester/monoester=1/1; acid value, 194 mg KOH/g) (1 kg) while heating at 70° C., whereby the cetyl phosphate was dispersed uniformly. An aqueous solution of sodium hydroxide (500 g/L) (278 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 barium chloride (200 g/L) (1825 ml) was gradually added thereto at a temperature of 70 to 80° C. After the addition was finished, the mixture was stirred at about 70° C. for 30 minutes. On confirming that the remaining barium ion became constant, the reaction was finished. The product was collected, washed with water, filtered, dried at 70° C. for 76 hours and pulverized in a mortar to give barium cetyl phosphate (1154 g). Yield, 93.5%. M.P., 174 to 183° C. Apparent specific volume, 3.6 ml/g. Elementary analysis: calcd., P=5.8%, Ba=19.2%; found, P=5.9%, Ba=18.0%.
後処理
- additionWhen the addition
- customat a temperature of 70 to 80° C
- additionAfter the addition
- stirringthe mixture was stirred at about 70° C. for 30 minutes
- customThe product was collected
- washwashed with water
- filtrationfiltered
- customdried at 70° C. for 76 hours
出典と根拠
- ORDレコード
- ord-eacb43f7d08c4ce9a4082be818c02361
- 出典データセット
- uspto-grants-1979_07
- 特許番号
- US04163018
関連ノート
読み込み中…