Acrylic Acid → Acrylic Acid Sodium Vinyl Sulfonate

HRID 1198861

Reaktionsgleichung

Reaktionsgleichung von HRID 1198861
[CH:1]([S:3]([O-:6])(=[O:5])=[O:4])=[CH2:2].[Na+:7].S(OOS([O-])(=O)=O)([O-])(=O)=O.[Na+].[Na+].[C:20]([OH:24])(=[O:23])[CH:21]=[CH2:22]>O>[C:20]([OH:24])(=[O:23])[CH:21]=[CH2:22].[CH:1]([S:3]([O-:6])(=[O:5])=[O:4])=[CH2:2].[Na+:7]

Komponenten

5

Edukt 3

HCID 6581Acrylic AcidHCID 62655Sodium PersulfateHCID 3270262Sodium vinylsulfonate

Produkt 1

HCID 23688942Acrylic Acid Sodium Vinyl Sulfonate

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Reaktionsbedingungen

Temperatur
95 °C

Versuchsvorschrift

A 1 liter round bottom flask equipped with a thermometer, agitator, condenser, nitrogen inlet tube, and slow addition funnels was charged with a solution of 10 g. water, 20.0 g. sodium vinyl sulfonate (as a 25% solution), 0.8 g. sodium persulfate, and 0.20 g. acrylic acid (Charge A). The contents were purged subsurface with nitrogen for 1 hour while heating to 95° C. The following charges were slowly and separately added over 4 hours: 94.8 g. acrylic acid and 60.0 g. isopropanol (99%) (Charge B) and 18 g. water and 3.0 g. sodium persulfate (Charge C). Reflux developed during the additions and was maintained for 1 hour thereafter. The flask was equipped with a Dean-Stark trap, stripping off of the alcohol was begun, and during the stripping 100.0 g. of 50% sodium hydroxide (Charge D) was slowly added over 2.5 hours. The solution was stripped to about 95° C. and 100 parts of alcohol were removed.

Aufarbeitung

  1. customA 1 liter round bottom flask equipped with a thermometer, agitator, condenser, nitrogen inlet tube, and slow addition funnels
  2. additionwas charged with a solution of 10 g
  3. customThe contents were purged subsurface with nitrogen for 1 hour
  4. additionseparately added over 4 hours
  5. temperatureReflux
  6. temperaturewas maintained for 1 hour
  7. customThe flask was equipped with a Dean-Stark trap
  8. additionof 50% sodium hydroxide (Charge D) was slowly added over 2.5 hours
  9. customwas stripped to about 95° C.
  10. custom100 parts of alcohol were removed

Quellen und Nachweise

ORD-Eintrag
ord-79a342860a994eddb88931acb0af030e
Quelldatensatz
uspto-grants-1990_02
Patentnummer
US04898677

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