Methanol → Gluconic Acid

Hydrated hafnium-ammonium-gluconate was prepared as follows: 125 grams of hafnium oxychloride.8H2O was dissolved in 600 ml of 50% aqueous solution gluconic acid. Four litters of anhydrous methanol were added to precipitate the hafnium-gluconate and the suspension was heated to 60° with stirring for 30 minutes. The pH of the preparation was then adjusted to 6.5 by addition of concentrated NH4OH. The hot solution was filtered to remove NH4Cl and ammonium gluconate. The precipitate was dried at 90° for 1 hour, resuspended in anhydrous methanol at 60° with stirring for 60 minutes then filtered to remove additional excess of NH4Cl and ammonium-gluconate. The precipitate was further extracted to remove additional NH4Cl and ammonium-gluconate employing anhydrous methanol in a Soxhlet apparatus, extraction was continued until the methanol surrounding the precipitate was clear. The precipitate was then dried at 90° for approximately 2 hours and ground to a fine powder. Elemental analysis was consistent with a formula of (HfO)2 (NH 4)2 gluconate3 (H2O)x. It was found that the same final product was obtained when the molar ratio of gluconic acid to hafnium was varied from 1:1 to 100:1. Moreover, the same product was obtained utilizing hafnium-tetrachloride instead of hafnium-oxychloride.

1. customto precipitate the hafnium-gluconate
2. temperaturethe suspension was heated to 60°
3. additionThe pH of the preparation was then adjusted to 6.5 by addition of concentrated NH4OH
4. filtrationThe hot solution was filtered
5. customto remove NH4Cl and ammonium gluconate
6. customThe precipitate was dried at 90° for 1 hour
7. customresuspended in anhydrous methanol at 60°
8. stirringwith stirring for 60 minutes
9. filtrationthen filtered
10. customto remove additional excess of NH4Cl and ammonium-gluconate
11. extractionThe precipitate was further extracted
12. customto remove additional NH4Cl and ammonium-gluconate employing anhydrous methanol
13. extractionin a Soxhlet apparatus, extraction
14. customThe precipitate was then dried at 90° for approximately 2 hours

ORD 기록

ord-c54d522ea3d64a909f8f52bdf6327b68

출처 데이터셋

uspto-grants-1979_11

DOI

10.6084/m9.figshare.5104873.v1

특허 번호

US04176173