Reaktion #171119

ord-a8203ea07a78435ba41ac0091019f882

Reaktionsgleichung

O=S(=O)([O-])OOS(=O)(=O)[O-].[Na+].[Na+]
Na2S2O8
C=CC(=O)O
acrylic acid
O=C([O-])CN(CCN(CC(=O)[O-])CC(=O)[O-])CCN(CC(=O)[O-])CC(=O)[O-].[Na+].[Na+].[Na+].[Na+].[Na+]
Versenex 80
C=CC(=O)O.C=CC(=O)O.C=CC(=O)O.CCC(CO)(CO)CO
trimethylolpropane triacrylate
C=CC(=O)O
acrylic acid
→
C=CC(=O)O.C=CC(=O)O.C=CC(=O)O.C=CC(=O)O.CCC(CO)(CO)CO
Acrylic Acid Trimethylolpropane Triacrylate

Edukte

O=S(=O)([O-])OOS(=O)(=O)[O-].[Na+].[Na+]
Na2S2O8
C=CC(=O)O
acrylic acid
O=C([O-])CN(CCN(CC(=O)[O-])CC(=O)[O-])CCN(CC(=O)[O-])CC(=O)[O-].[Na+].[Na+].[Na+].[Na+].[Na+]
Versenex 80
C=CC(=O)O.C=CC(=O)O.C=CC(=O)O.CCC(CO)(CO)CO
trimethylolpropane triacrylate
C=CC(=O)O
acrylic acid
—
solution

Reagenzien

Keine

Lösungsmittel

O
water

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeTo a three neck round bottom glass flask, equipped with a mechanical stirrer
  2. 2
    workup.ADDITIONadded to the reaction flask
  3. 3
    SonstigeA gel formed
  4. 4
    Temperaturwas heated for another hour at 70° C.
  5. 5
    SonstigeThen the aqueous gel was removed
  6. 6
    TemperaturOne portion was heated in a vacuum oven for 2 hours at 170° C.
  7. 7
    Temperatura second portion was heated for several hours at 220° C
  8. 8
    Filtrationsieved with 30 mesh (595 μm) and 50 mesh (297 μm)

Vorschrift

To a three neck round bottom glass flask, equipped with a mechanical stirrer and a thermocouple with a nitrogen inlet at the side of the inlet-tube was added 70.38 g of 20% caustic (0.353 mol) and 15.63 g water. Next, 26 g of acrylic acid (0.36 mol) were added slowly via a dropping funnel. After the mixture was cooled to room temperature, 0.28 g of a 40 wt. % active solution of Versenex 80 (diethylene glycol triamine pentaacetate from Aldrich) were added. Then 0.8 g trimethylolpropane triacrylate (TMPTA) were dissolved in 13.75 g acrylic acid (0.19 mol) and added to the reaction flask. The dropping funnel was taken off and the opening was covered by a septum. An amount of 0.2 ml of a 0.1% solution of FeSO4x7H2O was added by a syringe through the septum, followed by 0.635 ml of a 10% Na2S2O8 solution. The reaction started immediately. A gel formed. After the temperature peaked the flask was heated for another hour at 70° C. using a heating mantle. Then the aqueous gel was removed and was minced in a lab grinder. One portion was heated in a vacuum oven for 2 hours at 170° C. and a second portion was heated for several hours at 220° C. The products were ground and sieved with 30 mesh (595 μm) and 50 mesh (297 μm) sieves.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08846817B2uspto-grants-2014_09