Methacrylic Acid → Vinylphosphonic Acid Methacrylic Acid

HRID 75080

Reaktionsgleichung

Reaktionsgleichung von HRID 75080
[CH:1]([P:3](=[O:6])([OH:5])[OH:4])=[CH2:2].[C:7]([OH:12])(=[O:11])[C:8]([CH3:10])=[CH2:9].CC(N=NC(C#N)(C)C)(C#N)C>C(OCC)(=O)C>[CH:1]([P:3](=[O:4])([OH:6])[OH:5])=[CH2:2].[C:7]([OH:12])(=[O:11])[C:8]([CH3:10])=[CH2:9]

Komponenten

5

Edukt 3

HCID 4093Methacrylic AcidHCID 6547AzobisisobutyronitrileHCID 168725Poly(vinylphosphonic acid)

Produkt 1

HCID 86663293Vinylphosphonic Acid Methacrylic Acid

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8857Ethyl AcetateLösungsmittel2×

Reaktionsbedingungen

Temperatur
70 °C

Versuchsvorschrift

In a 10 liter flask equipped with a stirrer, a capacitor and a dropping device, 3,500 g of ethyl acetate was charged and heated to 70° C. Then, 390 g (3.61 mol) of a vinylphosphonic acid monomer, 1,243 g (14.44 mol) of methacrylic acid and 52 g of AIBN were dissolved in 1,000 g of ethyl acetate and the obtained solution was added dropwise in a reactor over 4 hours. During the dropwise addition of a monomer solution, a white precipitate was produced. After heating and stirring for 2 hours while maintaining at 70° C., heating was stopped and the reaction solution was cooled to room temperature. The precipitate thus produced was collected by filtration under reduced pressure and then washed with 1,000 g of ethyl acetate. The precipitate was vacuum-dried at 40° C. for 24 hours to obtain a white fine crystal. Yield: 1,550 g

Aufarbeitung

  1. customIn a 10 liter flask equipped with a stirrer
  2. additionthe obtained solution was added dropwise in a reactor over 4 hours
  3. additionDuring the dropwise addition of a monomer solution
  4. customa white precipitate was produced
  5. temperatureAfter heating
  6. temperaturewhile maintaining at 70° C.
  7. temperatureheating
  8. temperaturethe reaction solution was cooled to room temperature
  9. customThe precipitate thus produced
  10. filtrationwas collected by filtration under reduced pressure
  11. washwashed with 1,000 g of ethyl acetate
  12. customThe precipitate was vacuum-dried at 40° C. for 24 hours
  13. customto obtain a white fine crystal

Quellen und Nachweise

ORD-Eintrag
ord-d412556cfedc4d898fb1b9e3ac99e0ab
Quelldatensatz
uspto-grants-2014_09
Patentnummer
US08835099B2

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