Sodium Hydroxide → Calcium stearyl phosphate

HRID 972045

Reaction equation

[P:1]([O-:23])([O-:22])([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][CH2:19][CH2:20][CH3:21])=[O:2].[OH-].[Na+].[Cl-].[Ca+2:27].[Cl-]>O>[P:1]([O-:22])([O-:23])([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][CH2:19][CH2:20][CH3:21])=[O:2].[Ca+2:27]

Participants

Conditions

Temperature: 85 °C

Procedure

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

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

Sources & evidence

ORD record: ord-1d238dafe27a4b1d82a3df708221910d
Source dataset: uspto-grants-1979_07
DOI: 10.6084/m9.figshare.5104873.v1
Patent number: US04163018

Linked notes

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