Vanadium recovery from spent catalyst in multistage process

• Main Author: A. M. KUNAEV, V. A. KOZLOV, L. K. BATRAKOVA, B. B. BEISEMBAEV, A. M. ALESHIN, J. V. AZHIKINA, L. G. BEREZKINA, S. T. TAKEZHANOV, K. Z. KUANYSHEVA, G. L. PASHKOV, D. V. ILIINKOV, A. P. VOLOSHKIN, P. I. VOLPIN, V. M. MOROAOV, V. N. BALAK, V. A. GUSARENKO, N. M. CHECHULIN, J. I. OGORODNIKOV, B. M. MASLENNIKOV (DECEDE), A. M. BIKINEEV, A. I. MANOKHIN, T. S. SHI
• Format: Patent
• Language: English; French
• Published: 06.02.1987
• Edition: 4
• Subjects: AMMONIA; CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOIDCHEMISTRY; CHEMISTRY; COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSESC01D OR C01F; COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM,CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THERARE-EARTH METALS; COMPOUNDS THEREOF; CYANOGEN; FERROUS OR NON-FERROUS ALLOYS; INORGANIC CHEMISTRY; METALLURGY; PERFORMING OPERATIONS; PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL; PRETREATMENT OF RAW MATERIALS; PRODUCTION AND REFINING OF METALS; THEIR RELEVANT APPARATUS; TRANSPORTING; TREATMENT OF ALLOYS OR NON-FERROUS METALS

Spent catalysts (I) contg. V are processed by: (a) lixiviation in the presence of a reducing agent (II) to give a slurry, with conversion of V(V) to V(IV); (b) sepn. of the slurry into a soln. contg. V(IV) and a solid support; (c) oxidn. of V(IV) in the soln. to V(V); (d) extn. of V(V) from this soln. with aliphatic amines (III) in a water-immiscible organic solvent (IV), to give an extract and raffinate (V); (e) re-extn. of V(V) from this extract by bringing into contact with NH3 soln., giving ammonium vanadate (VI); and (f) treating (VI) with a H2SO4 soln.. Novel features are that: (g) in (a), V(II) soln. is used as (II) and a constant wt. ratio of V(II) ions in (II) to V(V) ions in (I) of (0.6-0.7):1.0 is maintained; (h) the solid obtd. in (b) is treated with 4-5% H2SO4 by direct steam digestion for 1-2 h to give a slurry contg. hydrochemically activated support; (i) the slurry from (h) is sepd. into a H2SO4 soln., which is recycled to (a), and a hydrochemically activated support, which is used in V catalyst prodn.; (k) pt. of the soln. from (b) is subjected to electrochemical treatment at a cathode current density of 100-300 A/m2 and 15-50 deg.C to give a V(II) soln., which is recycled to (a); (l) in (d), (IV) is pretreated with H2SO4 in (35-40):1 vol. ratio; (m) in (e), re-extn. is carried out in the presence of (NH4)2S2O8 in a constant wt. ratio of V(IV) ions of (0.5-3):1 to form an organic phase and an aq. phase contg. solid (VI); (n) the organic phases obtd. in (e) and (d) and the aq. phase contg. (VI) are filtered; (o) (VI) is filtered to a residual moisture content of 50-60% and H2SO4 is passed through the (VI) filter cake in a H2SO4:V ratio of 1:2-3 to give V2O5 and (NH4)2SO4 soln.; (p) after extn. of V, (V) is conc. by evapn. and crystallised to give K alum; (r) the soln. from (o) is conc. by evapn. and crystallised to give (NH4)2SO4. LE PROCEDE COMPREND LA LIXIVIATION EN 1 DU CATALYSEUR USE EN PRESENCE D'IONS VANADIUM DIVALENT; LA SEPARATION 2 DE LA PULPE EN UN SUPPORT SOLIDE QUE L'ON ENVOIE APRES TRAITEMENT 3 A L'OBTENTION DE CATALYSEUR AU VANADIUM 5 ET EN UNE SOLUTION DONT UNE PARTIE EST ENVOYEE A UN TRAITEMENT ELECTROCHIMIQUE 6 AVEC OBTENTION D'UNE SOLUTION DE VANADIUM DIVALENT ET RETOUR DE CETTE SOLUTION A LA LIXIVIATION 1; L'OXYDATION 7 DU VANADIUM IV EN VANADIUM V; L'EXTRACTION 8 DU VANADIUM V PAR DES AMINES ALIPHATIQUES TRAITEES PAR L'ACIDE SULFURIQUE; LA REEXTRACTION 9 DU VANADIUM V EN PRESENCE DE PERSULFATE DE POTASSIUM; LE PASSAGE 11 D'ACIDE SULFURIQUE A TRAVERS UN LIT DE VANADATE D'AMMONIUM SOLIDE OBTENU, AVEC OBTENTION DE PENTOXYDE DE VANADIUM. LE PRODUIT RAFFINE APRES EXTRACTION EST SOUMIS A UNE EVAPORATION PARTIELLE ET UNE CRISTALLISATION AVEC OBTENTION D'UN ALUN DE POTASSIUM. APRES SEPARATION DU VANADATE D'AMMONIUM DE LA SOLUTION, ON EVAPORE PARTIELLEMENT CETTE DERNIERE ET ON LA CRISTALLISE AVEC OBTENTION DE SULFATE D'AMMONIUM.