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United States Patent (19) (11) 4,079,116 Ronzio Et Al

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United States Patent (19) (11) 4,079,116 Ronzio Et Al United States Patent (19) (11) 4,079,116 Ronzio et al. (45) Mar. 14, 1978 54 PROCESS FOR PRODUCING AMMONIUM Primary Examiner-Herbert T. Carter HEPTAMOLYBDATE AND/OR Attorney, Agent, or Firm-Harness, Dickey & Pierce AMMONUM DIMOLYBDATE (57 ABSTRACT (75) Inventors: Richard A. Ronzio, Golden; Phillip A process for producing a high purity ammonium hep K. Davis, Arvada; Robert C. Ziegler, tamolybdate and/or ammonium dimolybdate product Lakewood, all of Colo. by which a particulated molybdenum oxide concentrate 73) Assignee: AMAX Inc., New York, N.Y. is purified to remove contaminating metal cations, whereafter it is leached with an ammoniacal leach solu (21) Appl. No.: 754,593 tion to extract the molybdenum trioxide constituent 22 Filed: Dec. 27, 1976 therein as soluble ammonium molybdate compounds. The resultant ammoniacal leach solution is thereafter 51) Int. Cl. .............................................. C01G 39/00 concentrated at an elevated temperature, whereafter at 52 U.S. C. ........................................ 423/56; 423/54; least a portion thereof is adjusted to provide an am 423/58; 42.3/593; 23/297; 23/302 A monia-to-molybdenum trioxide mol ratio ranging from 58) Field of Search ....................... 423/53, 56, 58,54, about 0.86:1 to about 1.25:1, and the adjusted solution 423/61, 593; 23/296,297, 302 A, 299, 305 R thereafter is cooled to effect a precipitation of ammo 56 References Cited nium heptamolybdate crystals which are separated and recovered, and the balance of the cooled solution is U.S. PATENT DOCUMENTS recirculated for admixture with additional ammoniacal 1,838,767 12/1931 Iredell .................................... 423/56 leach solution. A portion of the concentrated ammonia 3,357,821 12/1967 Henrickson ... ... 423/58 cal leach solution can be further concentrated by evapo 3,829,550 8/1974 Ronzio et al. ... ... 42.3/55 ration to effect crystallization of ammonium dimolyb 3,848,049 11/1974 Ronzio et al. ... ..., 423/56 3,932,580 1/1976 Vertes et al. ... 423/56 date which is separated and recovered. 3,957,946 5/1976 Ronzio et al. ... 423/54 3,963,823 6/1976 Kulkarni................................ 423/56 9 Claims, 2 Drawing Figures Moasey ap as a 4 Afe - ?ears ea a -12ars a 427-eare 12 ea dozeera. Ma --- a 17 aeae /2 A/A Me/Aac ava 52.7/?opy 42/2/7 a azzera 4: 1777azaga Cafe axaazzeAsy aea ea /777ervae-zz M/// are Aeaea wa, a 7 l A2//zape 27.727 a %.4.4, a 7227 serif Axe?aves/sier aafe 2 w a 2 /777rezzzzzy rysa/rez a-Ma. 47%s 2.77%rer /27a- 1777272/7 M, 242 fe dez7%- saa/27 4,079,116 1 2 and is heated to effect an evaporation of the water con PROCESS FOR PRODUCING AMMONUM stituent therein to a point approaching the saturation of HEPTAMOLYBDATE AND/ORAMMONUM the dissolved ammonium molybdate compounds DMOLYBDATE therein. In accordance with one embodiment of the process, at least a portion of the concentrated solution is BACKGROUND OF THE INVENTION withdrawn and the molar ratio of ammonia to molybde Ammonium heptamolybdate (NH)6Mo.O4.4H2O) num trioxide is adjusted by acidification or ion ex sometimes also referred to as ammonium paramolyb change to a range within about 0.86:1 to about 1.25:1 at date, comprises a valuable source of molybdate ions and an elevated temperature whereafter the adjusted solu is in extensive use as an analytical reagent, is employed 10 tion is cooled to a temperature of about 20° C or lower for synthesizing molybdenum-containing pigments and to effect a precipitation of ammonium heptamolybate catalysts for various liquid and gas phase hydrogenation crystals. The AHM crystals are separated from the and desulfurization reactions in petroleum refining op residual solution, such as by filtration or centrifugation, erations and coal technology, as well as for the produc and the residual solution is recycled for admixture with tion of a relatively pure grade of molybdenum metal. 15 additional ammoniacal leach solution which is recon A relatively high purity ammonium heptamolybdate centrated in the concentrator and again subjected to or AHM product has heretofore been produced on a adjustments followed by a cooling precipitation cycle. commercial scale by dissolving a high purity molybde By employing an evaporative crystallizer as a concen num trioxide in ammonium hydroxide to produce a trator, a controlled portion of the dissolved ammonium saturated solution having a pH of about 6 to about 6.6, 20 molybdate compounds can be recovered in the form of which thereafter is cooled from its saturation tempera ammonium dimolybdate. ture of about 55' C to temperatures as low as about 20 In accordance with an alternative embodiment of the C or lower. During the cooling cycle, a precipitation of process, a vacuum evaporator can be employed as the AHM crystals occurs which are removed such as by concentrator whereby a controlled adjustment in the centrifugation. The balance of the solution is employed 25 molar ratio of ammonia and molybdenum trioxide is for forming a fresh solution by the addition of further effected obviating the need for pH adjustment by acidi molybdenum trioxide and ammonia to provide the fication. proper pH at 55C, whereafter the cooling step is again The process can be operated as a closed system to repeated. While the foregoing prior art process is emi which an impure molybdenum trioxide concentrate is nently satisfactory for producing an ammonium hep 30 fed in addition to make up ammonia and from which a tamolybdate product of the requisite purity, certain high purity ammonium heptamolybdate product, to economic disadvantages are inherent due to the neces gether with ammonium dimolybdate product, is recov sity of employing high purity starting materials, such as ered along with waste side streams comprising the ex molybdenum trioxide derived from sublimation or from tracted contaminating metal cations and the insoluble the calcination of ammonium dimolybdate (ADM) de 35 residue remaining at the completion of the ammoniacal rived from the evaporative crystallization of ammonia leaching step. In accordance with a preferred embodi cal solutions containing molybdate ions. ment of the present invention, carbon dioxide is em The present invention overcomes many of the disad ployed for effecting a pH adjustment of the solution vantages associated with prior art techniques for form prior to cooling crystallization to provide the requisite ing high purity ammonium heptamolybdate as well as mol ratio of ammonia to molybdenum trioxide which ammonium dimolybdate by directly utilizing impure subsequently is removed during reheating of the resid molybdenum oxide concentrates as a starting material, ual solution in the concentrator. achieving substantial cost savings over techniques here Additional advantages and benefits of the present tofore known. invention will become apparent upon a reading of the 45 description of the preferred embodiments taken in con SUMMARY OF THE INVENTION junction with the accompanying drawing. The benefits and advantages of the present invention are achieved by a process in which an impure particu BRIEF DESCRIPTION OF THE DRAWINGS lated molybdenum oxide concentrate, such as derived FIG. 1 comprises a schematic flow diagram of one from an air roasting of the molybdenite concentrate, is 50 embodiment of the process for producing a high purity first treated with a hot aqueous leach solution in order ammonium heptamolybdate or ammonium dimolybdate to solubilize and extract a substantial portion of the product; and contaminating metal cations present therein. The aque FIG. 2 of the drawings comprises a schematic flow ous leach solution is separated from the leached concen diagram of an alternative embodiment of the process in trate, such as by filtration, and preferably is further 55 which a high purity ammonium heptamolybdate prod processed to recover the solubilized molybdate ions uct is produced from an impure roasted molybdenum therein which are recirculated for further processing. oxide concentrate feed material. The aqueous leached concentrate thereafter is con tacted with an ammoniacal leach solution to form a DESCRIPTION OF THE PREFERRED slurry of a concentration ranging from about 20 to EMBODIMENTS about 50% solids containing an excess of ammonia. The The feed material to the process in accordance with ammoniacal leaching step is continued until substan the flow diagrams shown in FIGS. 1 and 2 of the draw tially all of the molybdenum trioxide constituent therein ings comprises a particulated impure or technical grade is converted to soluble ammonium molybdate com concentrate consisting predominantly of molybdenum pounds. 65 oxide and further containing various contaminating The ammoniacal leach solution thereafter is separated metal constituents and compounds thereof in percent from the remaining insoluble residue which is discarded ages varying in accordance with the particular charac and the leach solution is transferred to a concentrator teristics of the original ore body and the manner by 4,079,116 3 4. which the concentrate was produced. Most commonly, No. 535,671, filed Dec. 23, 1974, for "Molybdenum technical grade molybdenum oxide concentrates are Oxide. Purification Process', now U.S. Pat. No. produced from an air roasting of molybdenite (MoS) 3,957,946, the substance of which is incorporated herein concentrates produced such as by an oil flotation ex by reference. The further oxidation of contaminating traction beneficiation process, whereby the gangue metal compounds, such as compounds of potassium, constituents are reduced to a level less than about 40% copper, calcium, magnesium, iron, aluminum, lead, and preferably less than about 10% by weight. The oil zinc, bismuth, or the like, renders them more susceptible flotation beneficiation process is normally carried out in to extraction by water leaching, providing for increased a series of successive cycles, each including a grinding processing efficiency and providing a product of in step followed by a flotation step, in which the particle 10 creased purity.
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