Water → Sodium Behenate

Participants

Reaction Conditions

Reaction Steps

87.6 g of behenic acid (Edenor C22-85R, product name, produced by Henckel), 423 ml of distilled water, 49.2 ml of an aqueous 5N-NaOH solution and 120 ml of tert-butanol were mixed and reacted by stirring at 75° C. for 1 hour to obtain a sodium behenate solution. Separately, 206.2 ml (pH: 4.0) of an aqueous solution containing 40.4 g of silver nitrate was prepared and kept at 10° C. To a reaction vessel containing 635 ml of distilled water and 30 ml of tert-butanol and kept at 30° C., the entire amount of the sodium behenate solution prepared above and the entire amount of the aqueous silver nitrate solution prepared above were added while stirring at a constant flow rate over 62 minutes and 10 seconds, and 60 minutes, respectively. At this time, for 7 minutes and 20 seconds after the initiation of addition of the aqueous silver nitrate solution, only the aqueous silver nitrate solution was added, then the addition of the sodium behenate solution was started, and for 9 minutes and 30 seconds after the completion of addition of the aqueous silver nitrate solution, only the sodium behenate solution was added. The temperature in the reaction vessel was 30° C. and the ambient temperature was controlled to prevent the liquid temperature from rising. The pipeline for the addition system of the sodium behenate solution was kept warm by the steam tracing where the steam opening was controlled to set the liquid temperature at the tip of addition nozzle to 75° C. The pipeline for the addition system of the aqueous silver nitrate solution was kept cold by circulating chilled water outside the duplex tube. The site where the sodium behenate solution was added and the site where the aqueous silver nitrate solution was added were symmetrized with respect to the stirring axis as the center. The heights were adjusted to prevent the solutions from contacting with the reaction solution.

Provenance & Evidence