Réaction #833539

ord-6f494feeca87416cb8d6422c87fb7f51

Équation de réaction

CCCCCCCCCCCCCCCCCCCCCC(=O)O
behenic acid
O
water
[Na+].[OH-]
NaOH
CCCCCCCCCCCCCCCCCCCCCC(=O)[O-].[Na+]
sodium behenate

Conditions de réaction

Conditions détaillées
See reaction.notes.procedure_details.

Traitement

  1. 1
    Autrereacted under agitation for 1 hour at 75° C.

Mode opératoire

88 kg of recrystallized behenic acid, 422 L of distilled water, 49.2 L of a 5 mol/L aqueous solution of NaOH, and 120 L of t-butyl alcohol were mixed and reacted under agitation for 1 hour at 75° C. to obtain a sodium behenate solution B. Separately, 206.2 L of an aqueous solution (pH 4.0) of 40.4 kg of silver nitrate was prepared and maintained at 10° C. A reaction vessel containing 635 L of distilled water and 30 L of t-butyl alcohol was maintained at 30° C., and the entire amount of the sodium behenate solution B and the entire amount of the silver nitrate solution were added under sufficient agitation with constant flow rates, over 93 minutes and 15 seconds and over 90 minutes, respectively. In this operation, during 11 minutes from the start of the addition of the silver nitrate solution, the silver nitrate solution alone was added, then the addition of the sodium behenate solution B was started, and, during 14 minutes and 15 seconds after the completion of addition of the silver nitrate solution, the sodium behenate solution B alone was added. In this operation, the temperature in the reaction vessel was maintained at 30° C., and the external temperature was so controlled as to maintain a constant liquid temperature. Also a piping for adding the sodium behenate solution B was temperature controlled by circulating warm water in an outer jacket of double tubes, thereby adjusting the liquid temperature at an exit end of the addition nozzle at 75° C. Also a piping for adding the silver nitrate solution was temperature controlled by circulating cold water in an outer jacket of double tubes. A position of addition of the sodium behenate solution B and a position of addition of the silver nitrate solution were symmetrically positioned with respect to an agitating shaft, and were adjusted at such a height not touching the reaction liquid.

Source

DOI: 10.6084/m9.figshare.5104873.v1Brevet: US07393626B2uspto-grants-2008_07