Phosphoric Acid → Silver behenate

HRID 353685

Reaction equation

HRID 353685 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].[OH-].[Na+].P(=O)(O)(O)O.BrN1C(=O)CCC1=O.[N+]([O-])([O-])=O.[Ag+:44]>C(OCCCC)(=O)C.O>[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+:44]

Participants

8

Reactant 5

HCID 1004Phosphoric AcidHCID 8215Docosanoic AcidHCID 14798Sodium HydroxideHCID 24470Silver NitrateHCID 67184N-bromobutanimide

Product 1

HCID 164971Silver behenate

Reagents, catalysts & solvents 2

HCID 962WaterSolventHCID 31272Butyl AcetateSolvent

Procedure

10.6 g of behenic acid and 300 ml of distilled water were mixed at 90° C. for 15 minutes, 31.1 ml of a 1N aqueous solution of NaOH was added thereto over 15 minutes while vigorously stirring, the mixture was allowed to stand for 1 hour, and the temperature was then decreased to 30° C. 7 ml of a 1N aqueous solution of phosphoric acid was added, 0.13 g of N-bromosuccinimide (C-2) was added thereto while stirring more vigorously, and the previously prepared silver halide grains A were then added thereto so that the amount of silver halide became 2.5 moles. 25 ml of a 1N aqueous solution of silver nitrate was further added thereto continuously over 2 minutes, and the mixture was stirred as it was for 90 minutes. 37 g of a 1.2 wt % butyl acetate solution of polyvinyl acetate was added to the aqueous mixture above so as to form a floc dispersion, the water was then removed, the residue was washed with water twice and the water was removed, 20 g of a 2.5 wt % solution of polyvinyl butyral (Denki Kagaku Kogyo K.K., Denka Butyral #3000-K) in a mixture of butyl acetate and isopropyl alcohol at 1:2 was added while stirring, subsequently 7.8 g of polyvinyl butyral (Denki Kagaku Kogyo, Denka Butyral #4000-2) and 57 g of 2-butanone were added to the gel mixture of organic acid and silver halide so obtained and dispersed by a homogenizer to give a silver behenate emulsion (acicular particles having an average short diameter of 0.04 lam, an average long diameter of 1 μm and a variance coefficient of 30%).

Workup

  1. waitto stand for 1 hour
  2. customwas then decreased to 30° C
  3. stirringwhile stirring more vigorously
  4. waitcontinuously over 2 minutes
  5. stirringthe mixture was stirred as it
  6. waitwas for 90 minutes
  7. customto form a floc dispersion
  8. customthe water was then removed
  9. washthe residue was washed with water twice
  10. customthe water was removed
  11. addition20 g of a 2.5 wt % solution of polyvinyl butyral (Denki Kagaku Kogyo K.K., Denka Butyral #3000-K) in a mixture of butyl acetate and isopropyl alcohol at 1:2
  12. additionwas added
  13. stirringwhile stirring
  14. additionsubsequently 7.8 g of polyvinyl butyral (Denki Kagaku Kogyo, Denka Butyral #4000-2) and 57 g of 2-butanone were added to the gel mixture of organic acid and silver halide
  15. customso obtained
  16. additiondispersed by a homogenizer

Sources & evidence

ORD record
ord-702582276cac482cbbbb76d962be29a6
Source dataset
uspto-grants-2004_06
Patent number
US06756193B2

Linked notes

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