FIELD: chemistry.
SUBSTANCE: invention relates to the production of borohydrides of titanium, zirconium and hafnium used in the production of composite materials. Method comprises reaction of tetrachlorides of titanium, or zirconium, or hafnium with sodium borohydride in an organic solvent medium in a planetary mill while stirring with a nozzle. Process is carried out in the presence of a catalyst, which is anhydrous lithium chloride, taken in an amount of 1-10 mol% of the sodium borohydride added. Solvent used is high-boiling absolute and aromatic hydrocarbons C7-C10 with Tb. 90-190°C. Mixture is stirred at a temperature of 20-90°C three times for 20 minutes with two 30-minute breaks. Mixture is filtered from the nozzle and sludge in an atmosphere of dry inert gas - argon or nitrogen in a funnel with a porous glass plate - Schott funnel at a vacuum of 10-100 mm hg.st. Obtained filtrates with dissolved borohydrides of titanium, zirconium and hafnium after analysis for the content of the final products, are stored in a closed vessel in an atmosphere of dry inert gas at a temperature not higher than -18°C.
EFFECT: invention makes improves the fire and explosion safety of producing borohydrides of titanium, zirconium and hafnium, and increases the yield of the desired products.
1 cl, 2 dwg, 9 ex
Authors
Dates
2018-04-18—Published
2017-02-09—Filed