Reacción #2275681

ord-aa1b19d1538645b3bddf7cf3837b6d6d

Ecuación de reacción

C(C[*:2])O[*:1]
polyoxyethylene
CCCCCCCC/C=C\CCCCCCCCOCCO
polyoxyethylene (6) oleyl ether
[Na+].[OH-]
sodium hydroxide
N#N
N2
CC(C)=CC(N)=O
dimethylacrylamide
C=CC(=O)NC(C)(C)CS(=O)(=O)O
2-acrylamido-2-methylpropanesulfonic acid
NC(=O)C=CCC=CC(N)=O
methylenebisacrylamide
O=S(=O)([O-])OOS(=O)(=O)[O-].[NH4+].[NH4+]
ammonium persulfate
N#N
N2
C=CC(=O)N(C)C.C=CC(=O)NC(C)(C)CS(=O)(=O)[O-].[Na+]
N,N-Dimethylacrylamide 2-Acrylamido-2-Methylpropane Sulfonic Acid Sodium Salt

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    Otroprovided with a reflux device
  2. 2
    workup.ADDITIONwere mixed together
  3. 3
    workup.DISSOLUTIONwere thus subjected to dissolution
  4. 4
    OtroThe aqueous monomer solution having been prepared in the manner
  5. 5
    workup.ADDITIONabove was then introduced into the three-neck flask
  6. 6
    TemperaturaThe resulting mixture was heated to a temperature of 65° C. to 70° C. in an oil bath, while the mixture
  7. 7
    Otrothe temperature of 65° C. to 70° C., it
  8. 8
    workup.ADDITIONwas then added to the polymerization system
  9. 9
    OtroPolymerization
  10. 10
    Otrowas kept at the temperature of 65° C. to 70° C.
  11. 11
    Otroa microgel was thus formed
  12. 12
    Otrothe microgel was thus precipitated
  13. 13
    LavadoSubsequently, washing with acetone
  14. 14
    Otrothe residual monomers and the surfactants were thus removed
  15. 15
    FiltraciónThe obtained precipitate was collected by filtration
  16. 16
    Otrodried under reduced pressure
  17. 17
    Otroa white powder-like microgel dry product was thereby obtained

Procedimiento

Firstly, 35 g of dimethylacrylamide (manufactured by Kojin Co., Ltd.), 17.5 g of 2-acrylamido-2-methylpropanesulfonic acid (manufactured by Sigma), and 7 mg of methylenebisacrylamide were dissolved in ion-exchanged water, and the pH value of the resulting solution was adjusted at 7.0 by the addition of sodium hydroxide. Thereafter, 260 g of n-hexane, 8.7 g of polyoxyethylene (3) oleyl ether (EMULEX 503, manufactured by Nihon Emulsion Co., Ltd.), and 17.6 g of polyoxyethylene (6) oleyl ether (EMULEX 506, manufactured by Nihon Emulsion Co., Ltd.) were introduced into a 1,000 ml three-neck flask provided with a reflux device, were mixed together, and were thus subjected to dissolution. The inside atmosphere of the three-neck flask was then replaced by an N2 gas. The aqueous monomer solution having been prepared in the manner described above was then introduced into the three-neck flask. The resulting mixture was heated to a temperature of 65° C. to 70° C. in an oil bath, while the mixture was being stirred under the N2 gas atmosphere. At the stage at which the system had reached the temperature of 65° C. to 70° C., it was confirmed that the system had come into a semitransparent microemulsion state, and 2 g of ammonium persulfate was then added to the polymerization system. Polymerization was thus begun. The polymerization system was kept at the temperature of 65° C. to 70° C. with stirring, and a microgel was thus formed. After the polymerization had finished, acetone was added to the microgel suspension, and the microgel was thus precipitated. Subsequently, washing with acetone was performed three times, and the residual monomers and the surfactants were thus removed. The obtained precipitate was collected by filtration and dried under reduced pressure, and a white powder-like microgel dry product was thereby obtained.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US08323629B2uspto-grants-2012_12