1 kg sugar dissolved in 700ml acid from old battery(25%). Mixture poured into glass canned jar 3l volume. Silicone tube inserted into the lid outside
leaves to the window. Jar placed at boiling water bath at 2 days with break at night. Pan with jar covered with a rag to reduce heat loss
After 2 days mixture contains many gumins. It was filtred from textile and solid was washed with 500 ml water.
Obtained 2 liters of liquid was electrolysed in 2 liter jar with 2 lead plate. 6 Volts and 5 amperes. Anode MUST BE LESS CATHODE AREA IN 5-10 TIMES
Every 5 hours cathode and anode must to replace at 5-10 minutes to recovery cathode activity.
Across several hour electrolyte have unpleasant odor. Across day dark liquid pops up at the top
After 2 days of electrolysis, the current began to fall. At the cathode, hydrogen bubbles began to be released. Liquid began to clean . This is an
electrolysis end signs
Upper layer was separated and liquid was extracted with toluene 2 times 200 ml(xylene also may be used)
Upper layer and toluene extract was combined and extracted with 100 gr KOH dissolved in 300 ml water. After toluene separation hydrochloric acid was
added in mixture. About 50 ml of liquid with an unpleasant smell obtained
Yield about 10%(fructose)
NOTES
25% sulfuric acid is much. 5-10% enough. Many gumins
High concentration sugar. 1 kg sugar needs 5 liters solution
Glucose give levulinic acid in 10 times slowly than fructose
Reaction rate proportional acid concentration and temperature
Electolysis needs anode diaphragm to better yield(fiberglass as example)
After extraction valeric acid electrolyte can be used again
After extraction toluene can be used again
Vareric acid need to distillation for cleaning from impurities
[Edited on 12-11-2021 by Hexabromobenzene]
[Edited on 13-11-2021 by Hexabromobenzene]DraconicAcid - 12-11-2021 at 19:35
Valeric acid is not merely "unpleasant". It's orders of magnitude worse than butyric.Fery - 13-11-2021 at 00:48
Hexabromobenzene - well done !!! So levulinic acid (4-oxovaleric) is produced from sugars and then it is electrolytically reduced to valeric acid.
As Draconic acid wrote - valeric acid is the worst stink from all aliphatic monocarboxylic acids. But its esters are pleasant.Boffis - 13-11-2021 at 01:45
Very interesting Hexabromobenzene! Is this your own procedure or is it from a published source? If the latter please could you provide us with a
reference or a link?
Is it possible to isolate the intermediate levulinic acid as this would be a very useful intermediate.Hexabromobenzene - 13-11-2021 at 03:15
Valeric acid is not merely "unpleasant". It's orders of magnitude worse than butyric.
From my experience it seems to be about the same as butyric acid, but I could be wrong. The last time I smelled butyric acid was in middle school, and
I remember it being horrible. When I made valeric and isovaleric acid the smell was unpleasant but not too bad, there are definitely much worse smells
in my opinion.
