Réaction #2275681

Équation de réaction

polyoxyethylene

polyoxyethylene (6) oleyl ether

sodium hydroxide

N2

dimethylacrylamide

2-acrylamido-2-methylpropanesulfonic acid

methylenebisacrylamide

ammonium persulfate

N2

→

N,N-Dimethylacrylamide 2-Acrylamido-2-Methylpropane Sulfonic Acid Sodium Salt

Solvants

n-hexane

acetone

water

Conditions de réaction

Traitement

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

Mode opératoire

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.

Source