1997 TMS Annual Meeting: Monday Abstracts

INTERNATIONAL SYMPOSIUM ON RHENIUM AND RHENIUM ALLOYS: Session II: Extraction and Recycling of Rhenium

Session Chairpersons: I.D. Troshkina, D. Mendeleyev, University of Chemical Technology of Russia, Miusskaya Sq. 9, Moscow 125047, Russia; Tom A. Millensifer, Powmet, Inc., 2625 Sewell St., P.O. Box 5086, Rockford, IL 61125

EXTRACTION OF RHENIUM FROM MOLYBDENITE CONCENTRATES: Mahesh C. Jha, William A. May, Entech Molybdenum Inc., 5950 McIntyre Street, Golden, CO 80403-7499

By-product molybdenite concentrates from copper mines are the most important source of rhenium. The rhenium content is low, generally in the few hundred ppm range. Almost all of these concentrates are roasted to technical grade molybdic oxide, the most common molybdenum product sold commercially. Rhenium oxide is volatilized at high roasting temperatures and condensed downstream at lower temperatures, eventually reporting to the scrubber liquor as a dilute solution. This paper reviews several hydrometallurgical approaches that have been used commercially and for researched and recommended to recover the rhenium from such dilute solutions. The methods include ion exchange, solvent extraction, selective leaching/precipitation, and crystallization for concentration and purification steps. Ammonium perrhenate is typically the end product.

2:20 pm

A DATABASE APPROACH TO THE RECYCLING OF RHENIUM: Laird G.L. Ward, Noble and PGM Recycling Representation, 23 Longview Road, E. Fallowfield, Coatesville, PA 19320-4311; David P. Dillard, Research Librarian, Paley Library, Temple University, Philadelphia, PA

Since its discovery by the German investigators W. Noddack, Ida Tacke and 0. Berg in 1925 and, at about the same time, by the Czechs J. Heyrovsky and V. Dolejsek, and the British investigators J.G.F. Druce and F.H. Loring, rhenium, element of atomic number 75 has gradually established a niche for itself in the industrial world. With the technology of rhenium now well established, its further technical progress may be impeded for the lack of a ready means to recover it from scrapped sources. This conference, being the next to follow the Rhenium Conference in l963, affords an opportunity to review the approaches published for the recovery of the element rhenium from some of the diverse products in which it has played a unique and very special ro1e.

2:40 pm

PROCESSING OF SPENT PLATINUM-RHENIUM CATALYST FOR RHENIUM RECOVERY: Mahmoud I. ElGuindy, Gemini Industries Inc., 2311 South Pullman Street, Santa Ana, CA 92705

Annually, over 5 million lbs of spent Reformer Catalysts are treated for the recovery of contained Platinum and Rhenium. In this publication a summary of available technology and methods employed for the processing of spent Pt-Re Catalyst will be discussed. Special emphasis will be on Rhenium recovery, purification and production of Catalytic Grade Ammonium Perrhenate. Furthermore, the factors influencing the chemical processing, the residence time and the purity of products in addition to metal accountability will be discussed. Recommended actions to be taken by petroleum processors to assist and facilitate recovery operations will also be presented.

3:00 pm

RHENIUM RECOVERY FROM NON-TRADITIONAL RESOURCE: A.M. Chekmarev, I.D. Troshkina, D. Mendeleyev, University of Chemical Technology of Russia, Miusskaya Sq. 9, Moscow 125047, Russia

About 50% world resource of rhenium is found in non-traditional carbon-based resource. The search of rhenium occurrence and the study of rhenium distribution in high-viscous oil, native bitumen and oil shale processing are performed by the radiotracer and kinetic methods of analysis. The products-concentrate of rhenium are determined. Methods of rhenium recovery from the processing products including hydrometallurgical techniques are developed. Sorption methods are worked out for rhenium recovery from additional resource; waste water, intermediate products in processing of various types of source etc.

3:20 pm BREAK

3:40 pm

RHENIUM AND OSMIUM RECOVERY FROM SULFURIC ACID SCRUB SOLUTIONS: I.D. Troshkina, A.M. Chekmarev, A.B. Mayboroda, D. Mendeleyev University of Chemical Technology of Russia, Miusskaya Sq. 9, Moscow 125047, Russia

The presence of radiogenic osmium-187 formed by by-fussion of rhenium-187 is the specific characteristic of some rhenium -containing source. The technology for the recovery of rhenium and osmium from sulfuric acid scrub solutions formed by wet gas purifying in pyrometallurgical processing of sulfide polymetallic ores was developed. The technology is based on extraction and sorption techniques following preliminary conversion of the metals into the optimal chemical species. The technology ensures quantitative recovery, concentration and separation of rhenium and osmium, production of commercially viable concentration of the elements.

4:00 pm

RECYCLING OF RHENIUM: D.V. Drobot, V.I. Bukin, Moscow State Academy of Fine Chemical Technologies, Pr. Vernadskogo 86, 117571 Moscow, Russia

The aim of the investigation is the generalization of the published results according of rhenium extraction from secondary materials. Such materials can be classified as binary W-Re and Mo-Re alloys; several composition Ni-Re alloys; Al-Pt-Re catalysts and other Re-containing secondary products. The range of technological processes is very mice and depends on forms and Re concentration in secondary materials. For Re extraction from binary alloys can be used processes including interaction with KNO3 or oxidation. In the last case it may be obtained volatile Re207. Purification can be done by rectification Re2O7. The full extent of Re extraction from such materials is 92-94%. Combination of the chlorination process with solvent extraction allows to obtain Re metal with extent of extraction ~92%. Re can be obtained from Mo-Re, W-Re alloys by means of electrochemical process (alkali solutions) or H:SO. solutions (Ni-Re alloys). For the production of the pure Re products it's necessery to use combination with solvent extraction or sorbtion. Complex Re and Pt extraction metals from A1-Pt-Re containing catalyst is the most important problem. There are known two methods, which differ at the first step: annealing with Na2CO3 or annealing in oxidation atmosphere are possible. Extents of Re and Pt extraction are 90 and 92%.

4:20 pm

BEHAVIOR & RECOVERY OF RHENIUM DURING THE CONVERSION OF MOLYBDENUM CONCENTRATES AND MISCELANEOUS TYPES OF THE SECONDARY RAW MATERIALS: N.N. Rakova, L.V. Miakisheva, K.N. Yegorychev, V.S. Strizhko, The Moscow State Institute of Steel & Alloys, Moscow, Russia

The definite works to create scientific foundations and the technology for the recovery of rhenium from the primary and secondary raw materials were initiated in the 60's at the Chairs of the rare-earth metals & powder metallurgy led by the Distinguished Metallurgist of Russia, professor A. N. Zelikman. 1. The molybdenum concentrates- one of the prime sources to recover rhenium along with the sulfide copper and copper/moly raw materials. The researches have been tested to investigate a behavior of rhenium during roasting process of the molybdenum concentrates and during the attack by the nitrogen acid. 2. The researchers have been tested with form and mechanism of extraction of molybdenum and rhenium from sulfur acid and nitrogen/sulfur acid solutions of different compositions. During the elaborations of the extraction methods of distribution and the recovery it has been taken into account the differences in the forms of molybdenum and rhenium presence in the acid atmospheres and it has been suggested to utilize the neutral, anion- and cation exchange extragents. 3. The processes of the deep cleaning of the rhenium combination through trihydroxychloride, having the below melting and flashing temperature have been developed. The purity of the recovered ammonium perrhenate and metallic rhenium is exceeding their purity during the production and refinery by the other methods. 4. Some methods have been tested to regenerate rhenium, tungsten, molybdenum from the wastes of W-Re & Mo-Re alloys with further treatment of the mixtures of chlorides of tungsten and rhenium by the water with the presence of oxidant and oxidation of alloys by means of oxygene and sublimation of rhenium oxide.

4:40 pm

RHENIUM RECOVERY FROM SECONDARY RAW MATERIALS OF VARIOUS TYPES: A.V. Elutin, M.V. Istrashkina, Z.A. Peredereeva, State Research Centre-State Institute of Rare Metals-GIREDMET, 5 B. Tolmachevsky Per., Moscow 109017, Russia

This report submits data of high-efficiency methods for rhenium recovery from secondary raw materials of various types, such as exhausted platinum-rhenium catalysts and scrap of rhenium-containing molybdenum, tungsten and nickel based alloys. Developed methods are used on a commercial level at industrial enterprises of Russia and CIS. A process for selectively recovering rhenium from exhausted Pt-Re catalysts includes next steps: roasting, acid- or alkali-assisted leaching, ion-exchange recovery or rhenium from the solution and preparing high-purity ammonium perrhenate (99.99%). Results of developing commercially applicable methods are useful for rhenium recovery from scrap of rhenium-containing alloys.

5:00 pm

DETERMINATION OF RHENIUM BY RADIOTRACER METHODS OF ANALYSIS: I.D. Troshkina, A.M. Chekmarev, V.I. Shamaev, D. Mendeleyev, University of Chemical Technology of Russia, Miusskaya Sq. 9, Moscow 125047, Russia

Radiometric correction and interpolation methods have been worked out for rhenium determination with extraction of the tetraphenylphosphonium complex into dichlorethane. Radiotracer 188Re (16,9 h) is obtained in 188Re-generator which is a glass column filled with aluminium oxide with a parent isotope 188W (69, 4 d) adsorbed firmly. The isotope 188Re formed is eluted from the generator by 0,9% solution of sodium chloride. Liquid scintillation counting was used. The method allows to determine from 1 to 100 mg of rhenium (VII) in analyzed probe. The relative standard deviation is 0.05-0,09 over the whole concentration range.

5:20 pm

AN OUTLINE OF THE PROCESS OF ACCESSORY RHENIUM EXTRACTION FROM MOLYBDENITE CONCENTRATES IN FLUID-BED ROASTERS: R.A. Apriamov, E.D. Doronkin, and F.V. Baroev, OAO "TVERDOSPLAV", 56 Warshavkoye Shosse, Moscow, Russia