反应 #75331

ord-c54d522ea3d64a909f8f52bdf6327b68

反应方程式

CO
methanol
O=C(O)[C@H](O)[C@@H](O)[C@H](O)[C@H](O)CO
gluconic acid
ClOCl.[Hf]
hafnium oxychloride
→
O=C(O)[C@H](O)[C@@H](O)[C@H](O)[C@H](O)CO
gluconic acid
[Hf]
hafnium

反应物

CO
methanol
O=C(O)[C@H](O)[C@@H](O)[C@H](O)[C@H](O)CO
gluconic acid
ClOCl.[Hf]
hafnium oxychloride

试剂

无

溶剂

—
aqueous solution

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他to precipitate the hafnium-gluconate
  2. 2
    温度the suspension was heated to 60°
  3. 3
    workup.ADDITIONThe pH of the preparation was then adjusted to 6.5 by addition of concentrated NH4OH
  4. 4
    过滤The hot solution was filtered
  5. 5
    其他to remove NH4Cl and ammonium gluconate
  6. 6
    其他The precipitate was dried at 90° for 1 hour
  7. 7
    其他resuspended in anhydrous methanol at 60°
  8. 8
    workup.STIRRINGwith stirring for 60 minutes
  9. 9
    过滤then filtered
  10. 10
    其他to remove additional excess of NH4Cl and ammonium-gluconate
  11. 11
    萃取The precipitate was further extracted
  12. 12
    其他to remove additional NH4Cl and ammonium-gluconate employing anhydrous methanol
  13. 13
    萃取in a Soxhlet apparatus, extraction
  14. 14
    其他The precipitate was then dried at 90° for approximately 2 hours

实验过程

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.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US04176173uspto-grants-1979_11