FIELD: chemistry.
SUBSTANCE: invention can be used in field of chemistry. Method for obtaining potassium dodecahydro-closo-dodecaborate includes carrying out process of pyrolysis of initial mixture, containing sodium tetrahydroborate NaBH4 and potassium tetrafluoroborate KBF4, in inert atmosphere in the interval of temperatures 280-475°C. Molar ratio of sodium tetrahydroborate NaBH4 to potassium tetrafluoroborate KBF4 in initial mixture equals (2.53-1.90) to 1. After that, leaching of obtained cake with water is carried out, formed solution is acidified with hydrofluoric acid HF to pH 3-4 to decompose residues of sodium tetrahydroborate, that did not react, and formed in the process of pyrolysis lower polyhedral borohydride compounds, then solution, containing K2B12H12, formed as a result of pyrolysis, is separated from non-soluble residue, representing mixture of excessive KBF4 and NaF, formed as a result of pyrolysis, after which portion of HF is added to said solution, and obtained mixture is poured with mixing to freshly precipitated chitosan C6O4H9NH2 to precipitate chitosan dodecahydro-closo-dodecaborate (C6O4H9NH3)2B12H12, which is separated from solution, washed with water and processed with potassium hydroxide KOH solution, which results in formation of K2B12H12 solution and freshly precipitated chitosan C6O4H9NH2, which is separated from K2B12H12 solution and washed with water, with washing waters being combined with obtained K2B12H12 solution, and target product K2B12H12 is separated.
EFFECT: invention makes it possible to increase output of target product - potassium dodecahydro-closo-dodecaborate and reduce temperature mode in the process of mixture hydrolysis.
9 cl, 2 ex
Authors
Dates
2016-01-27—Published
2013-05-07—Filed