Water → Silver behenate

HRID 1357452Notes

Reaction equation

HRID 1357452 reaction equation
[C:1]([OH:24])(=[O:23])[CH2:2][CH2:3][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][CH2:21][CH3:22].O.[OH-].[Na+].[N+]([O-])([O-])=O.[Ag+:32]>C(O)CCC>[C:1]([O-:24])(=[O:23])[CH2:2][CH2:3][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][CH2:21][CH3:22].[Ag+:32]

Participants

6

Reactant 4

HCID 962WaterHCID 8215Docosanoic AcidHCID 14798Sodium HydroxideHCID 24470Silver Nitrate

Product 1

HCID 164971Silver behenate

Reagents, catalysts & solvents 1

HCID 2631-ButanolSolvent

Procedure

While stirring 43.8 g of behenic acid (manufactured by Henkel Co., trade name: Edenor C22-85R), 730 ml of distilled water, and 60 ml of butanol at 79° C., 117 ml of 1 N NaOH aqueous solution was added thereto over 55 minutes and the mixture was allowed to reaction for 240 minutes. Then, 112.5 ml of an aqueous solution containing 19.2 g of silver nitrate was added thereto over 45 seconds and the solution was allowed to stand for 20 minutes, and then the temperature was lowered to 30° C. The solid content was then filtered by suction. The solid content was washed with water until the conductivity of the filtrate reached 30 mS/cm. The thus-obtained solid content was not dried and treated as a wet cake. Seven point four (7.4) grams of polyvinyl alcohol (trade name: PVA-205) and water were added to the wet cake of the amount corresponding to 100 g of dried solid content to make the entire amount 385 g, and then preliminarily dispersed in a homomixer. The preliminarily dispersed starting solution was treated three times using a disperser (trade name: Micro-fluidizer M-110S-EH equipped with G10Z interaction chamber, manufactured by Micro Fluidex International Corp.). Pressure of the disperser was adjusted to 1,750 kg/cm2. Thus, silver behenate dispersion B was obtained. Silver behenate grains contained in the thus-obtained silver behenate dispersion were acicular grains having an average short axis length of 0.04 μm, average long axis length of 0.8 μm, and variation coefficient of 30%. Grain size was measured by Master Sizer X (manufactured by Malvern Instruments Ltd.). Coiled heat exchangers were respectively installed before and after the interaction chamber. The desired temperature of dispersion was set by adjusting the temperature of the cooling medium.

Workup

  1. customthe mixture was allowed to reaction for 240 minutes
  2. additionwas added
  3. waitover 45 seconds
  4. waitto stand for 20 minutes
  5. customwas lowered to 30° C
  6. filtrationThe solid content was then filtered by suction
  7. washThe solid content was washed with water until the conductivity of the filtrate
  8. customThe thus-obtained solid content was not dried
  9. additiontreated as a wet cake
  10. additionSeven point four (7.4) grams of polyvinyl alcohol (trade name: PVA-205) and water were added to the wet cake of the amount corresponding to 100 g of dried solid content
  11. additionpreliminarily dispersed in a homomixer
  12. additionThe preliminarily dispersed
  13. additionwas treated three times
  14. customa disperser (trade name: Micro-fluidizer M-110S-EH equipped with G10Z interaction chamber, manufactured by Micro Fluidex International Corp.)

Sources & evidence

ORD record
ord-895e9dffc41e496694c7dc9bf50076f9
Source dataset
uspto-grants-2003_07
Patent number
US06593074B2

Reaction notes

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