Azobisisobutyronitrile → 9-Oxo-2,4,5,7-decatetraenoic acid
Reaktionsgleichung
[CH3:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7]CC(C)C.[C:12]([O:17]C)(=[O:16])[C:13]([CH3:15])=C.C(OC)(=[O:22])C=C.C(OCCN(C)C)(=O)C(C)=C.N(C(C(C)C)C#N)=NC(C(C)C)C#N.CC(N=NC(C#N)(C)C)(C#N)C>>[CH3:1][C:2](/[CH:3]=[CH:4]/[CH:5]=[C:6]=[CH:7]/[CH:15]=[CH:13]/[C:12]([OH:17])=[O:16])=[O:22]Komponenten
Reaktionsbedingungen
- Temperatur
- 70 °C
Versuchsvorschrift
A mixed solution of 10 g of Resin for Dispersion Stabilization (P-1) shown below and 280 g of Isopar G was heated to temperature of 70° C. with stirring under a nitrogen gas stream. To the solution was dropwise added a mixture of 30 g of methyl methacrylate, 61 g of methyl acrylate, 9 g of 2-(N,N-dimethylamino)ethyl methacrylate and 1.5 g of 2,2′-azobis(isovaleronitrile) (abbreviated as AIVN) over a period of one hour, followed by stirring for 2 hours. Then, 1.0 g of AIVN was added to the reaction mixture and the mixture was heated to temperature of 75° C., followed by stirring for 3 hours. Then, 0.8 g of 2,2′-azc)bis(isobutyronitrile) (abbreviated as AIBN) was added to the mixture and the mixture was heated to temperature of 80° C., followed by stirring for 3 hours. The temperature of the reaction mixture was raised to 100° C., followed by stirring under a reduced pressure of 200 mmHg for 2 hours, thereby distilling off the unreacted monomers. After cooling the reaction mixture, it was passed through a nylon cloth of 200 mesh. The resulting white dispersion was a latex having a polymerization rate of 99% and an average particle size of 0.35 μm. The particle size was measured by CAPA-500 manufactured by Horiba Ltd. (hereinafter the same).
Aufarbeitung
- additionTo the solution was dropwise added
- stirringby stirring for 2 hours
- temperaturethe mixture was heated to temperature of 75° C.
- stirringby stirring for 3 hours
- temperaturethe mixture was heated to temperature of 80° C.
- stirringby stirring for 3 hours
- temperatureThe temperature of the reaction mixture was raised to 100° C.
- stirringby stirring under a reduced pressure of 200 mmHg for 2 hours
- distillationdistilling off the unreacted monomers
- temperatureAfter cooling the reaction mixture, it
Quellen und Nachweise
- ORD-Eintrag
- ord-b69be9f814fd424f84270f41a341ff6a
- Quelldatensatz
- uspto-grants-2001_10
- Patentnummer
- US06302537B1
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