2,3-Dihydroxybutanedioic Acid → Lead oxide sulfate (Pb4O3(SO4))

Participants

Reaction Steps

Water was added to the starting lead monoxide powder containing 0.89% or 0.07% of PbOn to form a slurry having a PbO concentration of 93 g/l and a pH value of 9.8. A 2-liter capacity beaker was charged with 985 ml of the so prepared lead monoxide slurry, and 0.7 ml of acetic acid having a concentration of 2.2 moles/l was added to the slurry on a water bath under agitation by a glass vane. The mixture was agitated for 10 minutes, and 0.8 ml of hydroxylamine sulfate having a concentration of 0.84 mole/l and 0.03 g of powdery tartaric acid were added to the mixture. The mixture was sufficiently agitated to reduce lead peroxide present in the lead monoxide slurry (pH=9.7), and then, the mixture was heated. When the slurry temperature was elevated to 65° to 70° C., 26.61 ml of sulfuric acid having a concentration of 3.861 moles/l was gradually added dropwise to the slurry over a period of 30 minutes (the pH value was 6.3 or 6.4 at the initial stage of addition) and the mixture was agitated at 65° to 70° C. for 40 minutes to effect aging. Thus, there were obtained two kinds of tribasic lead sulfate base slurries having pH values of 8.4 and 8.5, respectively.

Provenance & Evidence