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Amélioration De La Maîtrise Des Ressources Françaises En Tungstène Improvement in Control of French Tungsten Resources BRGM

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Amélioration De La Maîtrise Des Ressources Françaises En Tungstène Improvement in Control of French Tungsten Resources BRGM ^ **' Amélioration de la maîtrise des ressources françaises en tungstène Improvement in control of french tungsten resources BRGM Rapport final M. SAVE M. PASTOR R 30346 Diffusion : MIN DAM 90 DG 1 ex page de garde, résumé, table mat., conclusions January 1990 LOG/D 1 ex non relié SGN/DIG 2 ex DS (M. Sustrac) 1 ex DAM/0P4 (M. Dumas) 1 ex DAM/MP (M. Snoep) 1 ex DAM/MIN : MM. Save 1 ex Morizot 1 ex Hau/Ollivier 1 ex chrono A.F.M.E. (M. Marcé) 6 ex CERMeP (M. Pastor) 1 ex IRCHA (Mme Presvot) 1 ex BUREAU DE RECHERCHES GÉOLOGIQUES ET MINIÈRES DIRECTION DES Activités minières Département Minéralurgie B.P. 6009 - 45060 ORLÉANS CEDEX 2 - France -Tél. : (33) 38.64.34.34 AMELIORATION DE LA MAITRISE DES RESSOURCES FRANÇAISES EN TUNGSTENE Responsable Scientifique : G. MORIZOT N* de contrat A.F.M.E. : 7.02.0035 Objet : Amélioration de la maîtrise de ressources françaises en tungstène Date de notification : 30/12/1987 Durée du contrat : 32 mois Montant du contrat : 1 600 000 F.F. H.T. Responsable A.F.M.E. : M. BEUTIN Service Industrie - Matières Premières RAPPORT CONFIDENTIEL BUREAU DE RECHERCHES GÉOLOGIQUES ET MINIÈRES DIRECTION DES ACTIVITÉS MINIERES Département Minêmlurqie B.P. G003 • 4E0H0 OKLEANS ŒDEX 2 - n.inc.* - îi'l.: (13) 23 ru IMJ.I R E S U M E Un programme général visant à améliorer la maîtrise des ressources françaises en tungstène a été entrepris par le B.R.G.M. et la Société EUROTUNGSTENE POUDRES (E.T.P.). Les études ont débuté le 1er octobre 1985 dans le cadre d'une première convention A.F.M.E. nô 5.02.1061 concernant : - la déphosphoration des concentrés de scheelite de SALAU (Ariège - Société Minière d'Anglade), - l'amélioration des performances du procédé d'attaque acide des concentrés de scheelite de E.T.P., - le traitement métallurgique des déchets de tungstène, - la définition d'un procédé d'enrichissement du minerai de wolframite de LEUCAMP. Les résultats obtenus ont été présentés dans le rapport de fin d'études n' 87 DAM 035 MIN. La seconde étape du programme fait l'objet de la présente conven­ tion. Elle concerne : - l'étude du recyclage des déchets de tungstène, à différents niveaux : . bibliographie sur les méthodes de traitement, . enquête sur les circuits de production et de récupération des déchets, . caractérisation physico-chimique de certains déchets, . fin des essais pilotes de certaines voies de traitement métallurgique, . essais de purification des solutions produites ci-dessus par extraction par solvant - l'étude de la valorisation des gisements français de wolframite : . bibliographie des voies de traitement métallurgique (y compris par voie solvant) . définition des voies de production de concentrés pauvres et de concentrés riches à partir du minerai de LEUCAMP. La réalisation des travaux se traduit par les résultats suivants : - la recherche bibliographique des procédés de recyclage des déchets tungstiques a recensé 325 références réparties sur les années 1935 à 1988. Une synthèse partielle a été réalisée. - l'enquête sur les circuits de recyclage, en dépit des blocages actuels du marché, a permis de cerner les différents opérateurs en fonction des types de déchets. L'aboutissement final des déchets (pour retransfor­ mation) est essentiellement limité à COLDSTREAM S.A. (Belgique) et SANDVIK pour les pièces métalliques triées, à STARCK (Allemagne) pour les déchets non triés tels que les boues d'usinage, - la caractérisation des boues d'usinage a été réalisée sur deux types de déchets (E.T.P. et SAFETY). Seules les boues relativement grenues d'E.T.P. peuvent être épurées par lavage, séparations granulometriques et magnétiques, - les essais pilotes et industriels de traitement de déchets de métal lourd et/ou de carbures cémentés ont permis de remettre en évidence les avantages et inconvénients de procédés présélectionnés dans la première phase de programme. Le procédé de fusion oxydante avec oxydation simul­ tanée de tous types de déchets a été retenu pour évaluation complémen­ taire technique (précision de certains points) et économique dans la suite du programme, - les essais d'extraction par solvant ont été réalisés au stade labora­ toire en utilisant des produits purs. L'étape d'extraction est bien maîtrisée mais une précipitation incontrôlée d'APT se produit au moment de la désextraction. Des éléments de solution ont été mis en évidence - la recherche bibliographique du traitement chimique des concentrés de wolframite a été totalement réalisée, - ainsi que les voies de production de concentrés pauvres à forte récupération métal (25 % W03 - 90,1 % métal ou 46 % WO-, - 83,7 % métal) et de concentrés riches à moindre récupération métal (65-67 % W03 - 70 % de métal). Ces derniers sont directement commercialisables et utilisa­ bles par les procédés conventionnels, les premiers demandent une filière intégrée avec application de traitements métallurgiques spécifiques. JU J. J. J. J. TABLE des MATIERES Pages RESUME INTRODUCTION 1 I. OBJECTIFS DE L'ETUDE 4 1.1. Bibliographie du traitement des déchets 5 1.2. Enquête sur les circuits déchets 5 1.3. Caractérisation des boues d'usinage 5 1.4. Essais pilotes et industriels des voies de traitement chimique des déchets 5 1.5. Essais de purification des solutions obtenues par les tements ci-dessus, en voie extraction liquide-liquide 6 1.6. Etude bibliographique du traitement chimique des con­ centrés de wolframite y compris par voie solvant ... 6 1.7. Etude de la concentration du minerai de LEUCAMP .... 6 II. REALISATION DES TRAVAUX 7 11.1. Bibliographie du traitement des déchets 8 Annexe 1 9 Etude bibliographie sur la récupération du tungstène à partir de divers déchets Annexe 2 39 Bibliographie 11.2. Enquête sur les circuits des déchets 70 11.2.1. Les différents types de déchets 70 11.2.2. Les différents opérateurs 71 11.2.3. Le contexte européen 73 11.2.4. Le contexte français 73 11.3. Caractérisation des boues d'usinage 78 11.3.1. Préparation des échantillons 78 11.3.2. Traitement de l'échantillon E.T.P 78 11.3.3. Traitement de l'échantillon SAFETY 79 11.3.4. Conclusions sur la caractérisation des boues 79 11.4. Essais pilotes ou industriels de traitement des déchets 86 Annexe 1 136 The recovery of Tungsten from a flotation concen- trate containing scheelite, wolframite, apatite and fluorspar Annexe 2 148 Report of an investigation into the recovery of tungsten and other metals from scrap supplied by Ugicarb Morgon, Grenoble - France Annexe 3 172 An investigation into the recovery of tungsten from tungsten-nickel-Iron swarf using hydrogen peroxide and a minerai acid for Ugicarb Morgon, France 11.5. Evaluation de la qualité des produits recyclés .... 184 11.6. Essais de purification des solutions obtenues par extraction liquide-liquide 195 11.6.1. Introduction 195 11.6.2. Extraction du tungstène 196 11.6.3. Réextraction par l'ammoniaque 198 11.6.4. Conclusions 200 11.7. Etude bibliographique du traitement chimique des concentrés de wolframite (y compris par voie solvant) 207 11.7.1. Introduction 207 11.7.2. Prétraitement des concentrés 207 11.7.3. Attaque des concentrés 208 11.7.4. Purification des solutions de tungstate de sodium 214 11.7.5. Extraction du tungstène des solutions de tungstate de sodium 217 11.8. Essais de concentration du minerai de LEUCAMP .... 256 11.8.1. Rappel des résultats antérieurs 256 11.8.2. Essais d'amélioration de la récupération W03 dans le concentré riche 260 11.8.3. Conclusions sur l'enrichissement du minerai à wolframite de LEUCAMP 269 Annexe 1 272 Séparation des sulfures par flottation 277 CONFIDENTIEL 1 INTRODUCTION La présente étude entre dans le cadre d'un programme visant à améliorer la maîtrise des ressources françaises en tungstène. Cette maîtrise peut être améliorée à trois niveaux : - l'industrie minière existante qui produit les minerais concentrés commercialisables, - l'industrie des produits tungstiques existante, qui utilise les concentrés ci-dessus et les déchets industriels. Les produits tungstiques sont les formes d'utilisation du tungstène - la valorisation future des gisements de wolframite français. Dans chaque secteur, un programme de travaux particuliers a été défini en commun accord entre les principaux partenaires du projet : - Bureau de Recherches Géologiques et Minières (Département Minéralurgie) - Société Eurotungstène Poudres (laboratoire de Recherche et Déve­ loppement) - Société Minière d'Anglade (Mine de Scheelite de Salau - Ariège). L'ensemble du programme devait être réalisé en plusieurs étapes. Il est présenté de manière synthétique sur le tableau n" I. Ainsi, la première étape des travaux a été réalisée en 1986-1987 dans le cadre de la convention A.F.M.E. n" 5.02.1061. Elle comprenait les travaux suivants : - industrie minière actuelle : . étude de la déphosphoration des concentrés de flottation par lixiviation - industrie des produits tungstiques : . amélioration des performances de la chaîne acide E.T.P. début des essais pilotes des quatre voies de traitement des déchets sélectionnés après les tests en laboratoire - valorisation des gisements français de wolframite : . début des essais de concentration du minerai de Leucamp. Cette étape s'est achevée le 30 mars 1987 et a fait l'objet d'un rapport de fin d'études 87 DAM 035 MIN. La seconde étape des travaux correspond à la présente étude placée dans le cadre de la convention A.F.M.E. n° 7.02.0035. Elle comprend les travaux suivants : 2 - industrie des produits tungstiques (recyclage des déchets de tungstène) : . bibliographie sur le traitement des déchets . enquête sur les circuits, flux, qualité de la production et la récupération des déchets . caractérisation de différentes boues de récupération . fin des essais pilotes ou industriels des voies de traitement des déchets . essais de purification des solutions obtenues par extraction liquide-liquide - valorisation des gisements français de wolframite : .
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