Reaktionsgleichung
[CH:1]([O:3][CH3:4])=[CH2:2].C(OOC(CC)(CCCC)C([O-])=O)(C)(C)C.C(=O)C.[C:24]1(=[O:30])[O:29][C:27](=[O:28])[CH:26]=[CH:25]1>>[CH:1]([O:3][CH3:4])=[CH2:2].[C:27]1(=[O:28])[O:29][C:24](=[O:30])[CH:25]=[CH:26]1Komponenten
Reaktionsbedingungen
- Temperatur
- 75 °C
Versuchsvorschrift
A 1-liter Buchi pressure reactor was sparged with nitrogen and charged with 400 ml (300 g, 5.16 mol) of methyl vinyl ether (MVE), 0.55 g Trigonox® 21 (t-butylperoxy-2-ethylhexanoate, an initiator made by Akzo Nobel Chemicalls, Inc.), a concentration of 0.08% by weight based on copolymer obtained, and with 0.034 g of acetaldehyde, or 0.01% by weight based on total weight of the reaction system. The precharged reactor was heated to 75° C., with agitation, over 15 min. Then 41 g (0.418 mol) of molten maleic anhydride (MAN), was fed in over 1 hour, resulting in a MVE/MAN mole ratio of 12.3. The solids content of the resulting mixture was 16%. The temperature of 75° C. was maintained for 1.5 hours. Then excess MVE was stripped off, whereupon the pressure dropped to atmospheric. Upon opening the reactor, a fine, free-flowing copolymer powder was observed. The product was dried in a vacuum oven at 65° C. for 4 hours. A total of 64.8 g (99.37 % of theoretical yield) of product was obtained. 13C NMR analysis the product indicated a 1:1 MVE/MAN copolymer having a specific viscosity (SV) of 4.1 (1% w/v polymer solution in MEK at 25° C.). The product was odorless and tasteless (2.5% aqueous solution, pH 7).
Aufarbeitung
- customA 1-liter Buchi pressure reactor was sparged with nitrogen
- customobtained
- customwas fed in over 1 hour
Quellen und Nachweise
- ORD-Eintrag
- ord-a719cc642e6049b4a38a544537a0a2e6
- Quelldatensatz
- uspto-grants-2001_04
- Patentnummer
- US06214956B1
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