Lead diacetate trihydrate → Lead oleate

HRID 1095206

Reaktionsgleichung

Reaktionsgleichung von HRID 1095206
O.O.O.C([O-])(=O)C.[Pb+2:8].C([O-])(=O)C.[C:13]([OH:32])(=[O:31])[CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20]/[CH:21]=[CH:22]\[CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH3:30].[C:33]([O-:52])(=[O:51])[CH2:34][CH2:35][CH2:36][CH2:37][CH2:38][CH2:39][CH2:40]/[CH:41]=[CH:42]\[CH2:43][CH2:44][CH2:45][CH2:46][CH2:47][CH2:48][CH2:49][CH3:50].[Se](=O)=O>>[C:13]([O-:32])(=[O:31])[CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20]/[CH:21]=[CH:22]\[CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH3:30].[Pb+2:8].[C:33]([O-:52])(=[O:51])[CH2:34][CH2:35][CH2:36][CH2:37][CH2:38][CH2:39][CH2:40]/[CH:41]=[CH:42]\[CH2:43][CH2:44][CH2:45][CH2:46][CH2:47][CH2:48][CH2:49][CH3:50]

Komponenten

5

Edukt 4

HCID 22456Lead diacetate trihydrateHCID 24007Selenium DioxideHCID 445639Oleic AcidHCID 5460221Oleic acid, ion(1-)

Produkt 1

HCID 6435829Lead oleate

Reaktionsbedingungen

Temperatur
85 °C

Versuchsvorschrift

Lead oleate was prepared as follows: lead acetate trihydrate (1 mmol) was mixed with ODE (4 mL) and oleic acid (1.3 mL) in a 50-mL three-neck flask. The mixture was degassed under vacuum (˜50 mTorr) at RT for 10 minutes and then gradually heated to 85° C. and kept for 1 hour to further remove the water and acetic acid. After the mixture turned colorless, the vacuum was removed and the lead-oleate solution was cooled to room temperature. The lead-oleate solution was mixed with TOP (8 mL) and SeO2 (1 mmol). Under argon flow and with stirring, the resulting mixture was heated to 180° C. After 5 min at the temperature, the reaction was terminated by cooling the reaction solution to room temperature. The resulting PbSe nanocrystals were precipitated from the reaction solution using acetone and redispersed in toluene.

Aufarbeitung

  1. customThe mixture was degassed under vacuum (˜50 mTorr) at RT for 10 minutes
  2. customto further remove the water and acetic acid
  3. customthe vacuum was removed
  4. temperaturethe lead-oleate solution was cooled to room temperature
  5. temperaturethe resulting mixture was heated to 180° C
  6. waitAfter 5 min at the temperature
  7. customthe reaction was terminated
  8. temperatureby cooling the reaction solution to room temperature
  9. customThe resulting PbSe nanocrystals were precipitated from the reaction solution
  10. additionredispersed in toluene

Quellen und Nachweise

ORD-Eintrag
ord-2a81f0c567724a2a87bde01722404282
Quelldatensatz
uspto-grants-2012_03
Patentnummer
US08137457B2

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