Pyromellitic Acid → 1,2,4,5-Cyclohexanetetracarboxylic Acid

HRID 1351049Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1351049
[C:1]([OH:18])(=[O:17])[C:2]1[C:3](=[CH:7][C:8](=[C:12]([CH:16]=1)[C:13]([OH:15])=[O:14])[C:9]([OH:11])=[O:10])[C:4]([OH:6])=[O:5].[H][H]>[Rh].O>[CH:8]1([C:9]([OH:11])=[O:10])[CH2:7][CH:3]([C:4]([OH:6])=[O:5])[CH:2]([C:1]([OH:18])=[O:17])[CH2:16][CH:12]1[C:13]([OH:15])=[O:14]

Komponenten

5

Reaktionsbedingungen

Temperatur
60 °C

Versuchsvorschrift

A 5-L Hastelloy (H22) autoclave was charged with 552 g of pyromellitic acid, 200 g of a catalyst, rhodium carried on activated carbon, available from N.E. Chemcat Corporation, and 1656 g of water. The inner atmosphere of the reactor was replaced with nitrogen gas under stirring. After replacing the inner atmosphere of the reactor with hydrogen gas, the hydrogen pressure was adjusted to 5.0 MPa and the temperature was raised to 60° C. While maintaining the hydrogen pressure at 5.0 MPa, the reaction was allowed to proceed for 2 h. Then, after replacing the hydrogen gas with nitrogen gas, the reaction product solution taken out of the autoclave was filtered while it was still hot to separate the catalyst. The filtrate was concentrated by evaporating water under reduced pressure using a rotary evaporator to precipitate crystals. The precipitated crystals were separated by solid-liquid separation and dried to obtain 481 g of 1,2,4,5-cyclohexanetetracarboxylic acid (yield: 85.0%).

Aufarbeitung

  1. filtrationwas filtered while it
  2. customto separate the catalyst
  3. concentrationThe filtrate was concentrated
  4. customby evaporating water under reduced pressure
  5. customa rotary evaporator
  6. customto precipitate crystals
  7. customThe precipitated crystals were separated by solid-liquid separation
  8. customdried

Quellen und Nachweise

ORD-Eintrag
ord-add9ba84556949f59ee32ff80c0ca223
Quelldatensatz
uspto-grants-2007_05
Patentnummer
US07217462B2

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