Tripotassium citrate → Citric acid, lanthanum(3+) salt(1:1)

HRID 2041797

Reaktionsgleichung

Reaktionsgleichung von HRID 2041797
C([O-])(=O)C.[La+3:5].C([O-])(=O)C.C([O-])(=O)C.[C:14]([O-:26])(=[O:25])[CH2:15][C:16]([CH2:21][C:22]([O-:24])=[O:23])([C:18]([O-:20])=[O:19])[OH:17].[K+].[K+].[K+]>O>[C:14]([O-:26])(=[O:25])[CH2:15][C:16]([CH2:21][C:22]([O-:24])=[O:23])([C:18]([O-:20])=[O:19])[OH:17].[La+3:5]

Komponenten

4

Edukt 2

HCID 13344Tripotassium citrateHCID 13511Lanthanum acetate2×

Produkt 1

HCID 18149Citric acid, lanthanum(3+) salt(1:1)Ausbeute 100 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel2×

Versuchsvorschrift

In one embodiment for the synthesis of (La,K,□)2Nb2(O,□)7 (OH)2; (□=vacancies) (1), lanthanum acetate (0.42 g, 1.35 mmol) is dissolved in 4 grams of DI water by stirring in a 23 ml Teflon cup for a Parr reactor, which is a closed-cell reactor suitable for use in hydrothermal synthesis. Other reaction vessels or reactors that are suitable for use for reactions conducted under pressure and at elevated temperatures may be used. Potassium citrate, tribasic (0.44 g, 1.35 mmol) is dissolved in 3 grams of DI water and added dropwise to the lanthanum acetate solution. A thick white precipitate of lanthanum citrate is formed immediately. The pH at this point is 8.4. Thirty drops of potassium hydroxide solution (4 molar) is added, and the precipitate redissolves after about 20 drops. K8[Nb6O19].16H2O (0.33 g, 1.35 mmol Nb) is dissolved in 2 grams of water and added to the solution in the Parr reactor. Alternatively, the K8[Nb6O19].16H2O can be dissolved directly in the lanthanum citrate solution. The final pH is recorded at 12.7. The reactor is closed in its steel casing and heated in a 225° C. box furnace for 3-4 days. A white crystalline powder is collected (approximately 0.8 grams; around 100% yield) by vacuum filtration and washing with DI water and then methanol. ˜2.5% weight loss by TGA analysis (calculated=3%) Compositional analysis for (La1.7K0.1□0.2)Nb2(O6.6□0.4)(OH)2 (FW=565.8). Calculated (from formula derived from X-ray data): 41.8% La, 32.9% Nb, 0.69% K. Experimental: 40.2% La, 30.0% Nb, 0.82% K.

Aufarbeitung

  1. customIn one embodiment for the synthesis of (La,K,□)2Nb2(O,□)7 (OH)2
  2. customin hydrothermal synthesis
  3. customOther reaction vessels or reactors that

Quellen und Nachweise

ORD-Eintrag
ord-8a38fc21afdd4438b14d86722bbb0e87
Quelldatensatz
uspto-grants-2013_11
Patentnummer
US08585928B1

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