Ammonium Hydroxide → Antimony oxalate

HRID 1987531Notes

Reaction equation

[C:1]([O-:4])(=[O:3])[CH3:2].[Sb+3:5].[C:6]([O-:9])(=[O:8])[CH3:7].[C:10]([O-:13])(=[O:12])[CH3:11].[OH-:14].[NH4+].[Sb]>O.C(O)(=O)C(O)=O>[C:1]([O-:4])(=[O:3])[C:2]([O-:8])=[O:14].[Sb+3:5].[C:6]([O-:9])(=[O:8])[C:7]([O-:12])=[O:14].[C:10]([O-:13])(=[O:12])[C:11]([O-:3])=[O:14].[Sb+3:5]

Participants

Conditions

Temperature: 60 °C

Procedure

Antimony oxalate solution was prepared by mixing antimony (III) acetate as obtained from Aldrich with a 1 M solution of oxalic acid in deionized water and heating the mixture to 60° C. A concentrated solution of ammonium hydroxide in deionized water was added dropwise to the antimony containing mixture until the solution became homogeneous. At this point, the solution was diluted as-required with oxalic acid solution or deionized water to desired metal concentration. The prepared antimony oxalate solution (3.3% antimony, 290.9 μL) was mixed with deionized water (1149.1 μL) and the resultant diluted solution (120 μL) was added to the supported rhodium-indium product of the first impregnation step and agitated by vibration for 30 minutes at room temperature. The obtained trimetallic material was dried at 120° C. for 2 hours and then calcined in air at 450° C. for 4 hours.

Workup

concentrationto desired metal concentration
additionThe prepared antimony oxalate solution (3.3% antimony, 290.9 μL) was mixed with deionized water (1149.1 μL)
additionthe resultant diluted solution (120 μL) was added to the supported rhodium-indium product of the first impregnation step
customThe obtained trimetallic material was dried at 120° C. for 2 hours
waitcalcined in air at 450° C. for 4 hours

Sources & evidence

ORD record: ord-60750c09de864974ba4571e2fc4f3a33
Source dataset: uspto-grants-2009_06
DOI: 10.6084/m9.figshare.5104873.v1
Patent number: US07550637B2

Reaction notes

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