Ethylene → ethylphosphonous acid aluminum(III) salt

HRID 338047

Reaktionsgleichung

Reaktionsgleichung von HRID 338047
O.[PH2]([O-])=O.[Na+].C=C.Cl.N(C(C(=N)N)(C)C)=NC(C(=N)N)(C)C.O.O.O.O.O.O.[Cl-].[Al+3:30].[Cl-].[Cl-].[Al+3].[CH2:34]([P:36](CC)(=[O:38])[O-:37])[CH3:35].[CH2:41]([P:43](CC)(=[O:45])[O-:44])[CH3:42].[CH2:48]([P:50](CC)(=[O:52])[O-:51])[CH3:49]>O>[Al+3:30].[CH2:34]([P:36]([O-:38])[O-:37])[CH3:35].[CH2:41]([P:43]([O-:45])[O-:44])[CH3:42].[CH2:48]([P:50]([O-:52])[O-:51])[CH3:49].[Al+3:30]

Komponenten

7

Edukt 5

HCID 6325Ethylene3×HCID 84924Propanimidamide, 2,2'-(1,2-diazenediyl)bis[2-methyl-, hydrochloride (1:?)2×HCID 9794789AlCl3.6H2OHCID 21863131Phosphinic acid, P,P-diethyl-, aluminum salt (3:1)HCID 178418950HCID 178418950, Verbindung

Produkt 1

HCID 131732054ethylphosphonous acid aluminum(III) saltAusbeute 95,9 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel3×

Reaktionsbedingungen

Temperatur
100 °C

Versuchsvorschrift

1500 g (14 mol) of sodium hypophosphite monohydrate are dissolved in 7.5 kg of water and initially charged in a 16 l steel-enamel jacketed pressure reactor. After heating the reaction mixture to 100° C., a reducing valve set to 6 bar is used to introduce ethylene into the reactor up to saturation. While stirring constantly at an ethylene pressure of 6 bar and a temperature of 100-110° C., a solution of 19 g (0.5 mol %) of 2,2′-azobis(2-amidinopropane) hydrochloride in 300 g of water is metered in homogeneously. At a conversion of ethylene of 87.3%, the metered addition of 2,2′-azobis(2-amidinopropane) hydrochloride is stopped and the reactor is decompressed. After cooling to about 90° C., 650 g (4.67 mol of aluminum) of aluminum chloride hexahydrate in 2350 g of water were added within 60 minutes. Subsequently, the resulting solid is filtered off, washed with 2 l of hot water and dried at 130° C. under reduced pressure. The resulting mixture comprises diethylphosphinic acid aluminum(III) salt and ethylphosphonous acid aluminum(III) salt in a ratio of 83.3% by weight of diethylphosphinic acid aluminum(III) salt and 16.7% by weight of ethylphosphonous acid aluminum(III) salt (95.9% yield).

Aufarbeitung

  1. customa reducing valve set to 6 bar
  2. customa temperature of 100-110° C.
  3. temperatureAfter cooling to about 90° C.
  4. filtrationSubsequently, the resulting solid is filtered off
  5. washwashed with 2 l of hot water
  6. customdried at 130° C. under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-62181522f1414160b080f68bc8e751a6
Quelldatensatz
uspto-grants-2014_11
Patentnummer
US08889772B2

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