Development of Acetic Acid Removal Technology for the UREX+Process Page: 53 of 147
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FS-13 solvent is used during the PEG/CCD step. It was decided that the most probable place to
extract the excess acetic acid was after the UREX step and before the PEG/CCD step (Figure 3-
1). At this point, the acetohydroxamic acid is hydrolyzed into acetic acid and hydroxylamine
nitrate (HAN). Since FS-13 was not readily available early in this study, dichloroethane was used
initially as an analogue for FS-13 solvent [13]. Dichloroethane is not a suitable solvent for the
UREX+ process.A limited quantify of FS-13 became available during the experimental trials and
was also tested. These solvents were also used in the experiment with tributyl phosphate (TBP)
at a 2.5M concentration.
2. EXPERIMENT
The distribution coefficients for a number of solvents and conditions were measured to
determine the amount of acid transferred into the organic phase from solutions similar to those
found in the UREX+ process. Solutions of various acidic concentrations were prepared ranging
from O.O1M to 1M of both nitric and acetic acids to serve as the reference aqueous solutions for
this study. Organic solvents (diluents) dichloroethane, dodecane, and FS-13 were the first
solvents tested. Dodecane 99% was obtained from ACROS Chemicals, ACS grade
dichloroethane was obtained from Fisher Scientific, and FS-13 was obtained from Marshallton
Reasearch Laboratories. Using a 250 mL separatory funnel, 10 mL of aqueous and 10 mL of
organic solvent were added. The funnel was hand-shaken for approximately one minute and
settling was allowed for full separation of the layers. The aqueous layer was drawn off into a
small beaker and analyzed using a Mettler-Toledo SevenEasy pH meter and a Brinkmann 765
Dosimat set on dose mode containing 1M caustic solution. Using the amount of caustic required40
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Counce, Robert M. & Watson, Jack S. Development of Acetic Acid Removal Technology for the UREX+Process, report, June 30, 2009; United States. (https://digital.library.unt.edu/ark:/67531/metadc927996/m1/53/: accessed April 25, 2024), University of North Texas Libraries, UNT Digital Library, https://digital.library.unt.edu; crediting UNT Libraries Government Documents Department.