tags
sodiumiodineHClphosphinesodium hypophosphatechloridehypophosphite

video tutorial Hypophosphorus acid preparation

  • Subject: sodium hypophosphate (sodium salt of hypophosphorus acid) and its use with iodine to reduce alcohols to alkanes; aim to prepare the acid from the salt.
  • Method and yield: reacted 100 g of sodium hypophosphate dihydrate with two portions of concentrated HCl to form sodium chloride and hypophosphorus acid; isolated about 40 g of NaCl (expected ~47 g).
  • Filtrate contained hypophosphite/hydrogen ions; concentrated filtration and partial distillation produced a strong hypophosphorus acid solution; observed pale yellow filtrate density ~1.35 g/mL (theory ~1.49).
  • Test of reducing power: added iodine; reduction occurred, described as working well (perhaps too well).
  • Thermal test: heating the acid caused condensation, slight boiling, and a tiny explosion, indicating hazardous decomposition to phosphine; cautioned about reflux safety.
  • Final steps: evaporated liquid to dryness; noted reactive hazards—upon heating (~150°C) large clouds of phosphorus pentoxide form as phosphine gas ignites in air; plan to test reduction of an alcohol in a future video.
  • Overall note: demonstration emphasizes the reactivity and safety concerns of hypophosphorus acid/phosphine formation; stay tuned for further results.

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