Welcome to LookChem.com Sign In | Join Free

Details

Home > Chemical Encyclopedia > Chemical Technology > Laboratory Chemical Technology >
 General procedures for the purification of Carboxylic acids
  • General procedures for the purification of Carboxylic acids
  • Liquid carboxylic acids are first freed from neutral and basic impurities by dissolving them in aqueous alkali and extracting with diethyl ether. (The pH of the solution should be at least three units above the pKa of the acid). The aqueous phase is then acidified to a pH at least three units below the PKa of the acid and again extracted with ether. The extract is dried with magnesium sulfate or sodium sulfate and the ether is distilled off, The acid is fractionally distilled through an efficient column. It can be further purified by conversion to its methyl or ethyl ester (vide supra) which is then fractionally distilled. Hydrolysis yields the original acid which is again purified as above.

    Acids that are solids can be purified in this way, except that distillation is replaced by repeated crystallisation (preferable from at least two different solvents such as , alcohol or aqueous alcohol, toluene, toluene/petroleum ether or acetic acid.) Water-insoluble acids can be partially purified by dissolution in N sodium hydroxide solution and precipitation with dilute mineral acid. If the acid is required to be free from sodium ions, then it is better to dissolve the acid in hot N ammonia, heat to ca 80°C, adding slightly more than an equal volume of N formic acid and allowing to cool slowly for crystallisation. Any ammonia, formic acid or ammonium formate that adhere to the acid are removed when the acid is dried in a vacuum - they are volatile. The separation and purification of naturally occurring fatty acids, based on distillation, salt solubility and low temperature crystallisation.

    Aromatic carboxylic acids can be purified by conversion to their sodium salts, recrystallisation from hot water, and reconversion to the free acids.


    Prev:No record
    Next:No record
  • Back】【Close 】【Print】【Add to favorite
Periodic Table
    Hot Products