Abstract: The invention relates to a process for the preparation, by nitriding, of a refractory powder containing more than 40% of silicon nitride from spent contact masses issuing from chlorosilane synthesis. The process involves mixing with the copper-free spent mass, silicon or a silicon-rich alloy and optionally a refractory compound to adjust the non-oxidised silicon content to a predetermined value >30%, heating the mixture in a nitrogen atmosphere to trigger the exothermic nitriding reaction, then reducing the product obtained to powder. The refractory powder thus obtained can be mixed with an organic binder to produce taphole blocking masses for blast furnaces or electric furnaces for pyrometallurgy.