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May 8, 1973 D May 8, 1973 D. BROWN ETAL 3,732,094 PROCESS FOR PREPARING ELEMENTAL MERCURY Filed June 29, 1970 8 Sheets-Sheet 1 BY ???? ATTORNEYS May 8, 1973 D. BROWN ETA 3,732,094 PROCESS FOR PREPARING ELEMENTAL MERCURY Filled June 29, 1970 8 Sheets-Sheet 4 9NIHOVET–139w1s INVENTORS ALTON R. CARLSON DUANE BROWN BY ATTORNEYS May 8, 1973 D. BROWN ET AL 3,732,094 PROCESS FOR PREPARING ELEMENTAL MERCURY Filed June 29, 1970 8 Sheets-Sheet : NOI.Ld8OSOV/ ? 9NITLLES NOIIVOIHIHnd–z39WLS 8º INVENTORS ALTON R. CARLSON DUANE BROWN BY ATTORNEYS May 8, 1973 D. BROWN ETAL 3,732,094 PROCESS FOR PREPARING ELEMENTAL MERCURY Filed June 29, 1970 09.2° AMJBAOOBHTVLEWSTOIOB}}dTVNOI.LdO 239\/]LS-JOdB.LS DUANE BROWN li?BY A TORNEYS May 8, 1973 D. EROVVN ET AL 3,732,094 PROCESS FOR PREPARING ELEMENTAL MERCURY Filed June 29, 1970 8 Sheets-Sheet , 31.ooosx9NINIVILNO? QOHLEWGEMJH3-||38d:NO|100038-239WLS -OL1STATOV; ATTORNEYS May 8, 1973 D. BROWN ET AL 3,732,094 PROCESS FOR PREPARING ELEMENTAL MERCURY Filed June 29, l970 8 Sheets-Sheet 7 OBVOS#C) BLATOHLOBT3LNBdS AHEAOOBHLN30V3HNOILOnQ38-v39\/1S E9NOCHSuS OILNO|LOTAGE}} E9NOdSUS INVENTORS A TON R. CARLSON DUANE BROWN ATTORNEYS May 8, 1973 D. BROWN ET AL 3,732,094 PROCESS FOR PREPARING ELEMENTAL MERCURY Filed June 29, 1970 ?? 8 Sheets-Sheet 3 98 dELSNOILOTIC]38 NOllwg3N3938LN39v38NOILOnQ38–G39WLS INVENTORS ATON. R. CARLSON DUANE BROWN BY ATTORNEYS 3,732,094 United States Patent Office Patented May 8, 1973 2 Similarly, according to still another aspect of the inven 3,732,094 tion, if precious metals such as gold compounds are pres PROCESS FOR PREPARNG ELEMENTAL ent, they are selectively separated from the pregnant mer MERCURY Duane Brown, 104 E. Huntington Drive, Tempe, Ariz. cury leach liquor prior to the reduction steps for the same 85281, and Alton R. Carlson, 720 E. Dobbins Road, CaSO Phoenix, Ariz. 85040 In still another and more particular respect, the inven Filed June 29, 1970, Ser. No. 50,838 tion relates to a method for reducing the mercury con nt. C. C22b 3/00, 11/00, 43/00 tent of mercury-containing solutions to elemental mercury U.S. C. 75-101 R 1. Claims involving a preferred two-step reduction which includes 0 the formation of an intermediate, partially reduced, in soluble mercury compound which is physically separated ABSTRACT OF THE DISCLOSURE from the mother liquor before the second stage reduc This application discloses a process for recovering mer tion which completes the process of forming elemental cury from various mercury-containing materials such as mercury. ores, ore concentrates, alloys, amalgams and compounds. 5 Finally, the invention contemplates an overall inte According to one feature of the process, the mercury is ex grated process especially adapted for the production of ele tracted in the form of a soluble mercury complex by leach mental mercury from cinnabar ore or from cinnabar ore ing the mercury source with a novel leach liquid. The concentrates, the integrated process providing for the re novel leach liquid contains components which react during covery of virtually all of the reagents employed in the the leaching step to generate a hypohalite leach reagent in 20 reduction step, and the regeneration of the reducing agent situ. The hypohalite, in turn, oxidizes the mercury or mer for re-use. cury compound which is then solubilized in the leach liquid to form a strong pregnant liquor. DESCRIPTION OF THE PRIOR ART According to another feature of the process, arsenic, selenium and tellurium impurities are separated from the In the past, several methods have been employed to pregnant liquor by means of a novel technique involving 25 produce elemental mercury from its naturally occurring the formation of an insoluble metal hydroxide Suspen ore or by extracting it from its amalgams with other metals sion in the pregnant liquor, which suspension selectively and its compounds with other elements. Virtually all of adsorbs the soluble impurity metal compounds which are the virgin mercury is produced by winning the metal from in turn separated from the pregnant liquor. If gold com 30 its common mineral, cinnabar (HgS). The most common pounds are present in the purified pregnant liquor, they prior technique of producing elemental mercury from cin are selectively removed prior to the reduction step by con nabar involves roasting the naturally occurring ore under tacting the pregnant liquor with a combined reductant and highly oxidizing conditions and at elevated temperatures adsorbent for the gold. in the range of 500-1000° C. This process involves the According to another feature of the invention, preg 35 oxidation of the sulfur content of the cinnabar, forming nant leach liquors containing soluble mercury complexes, Sulfur dioxide gas and mercury vapor. The mercury vapor either prepared as described above or by any other suit is condensed by cooling with either air or water to approxi able process, are treated to reduce the mercury complex mately 40 C. or lower to form the liquid elemental to form elemental mercury in a single homogeneous liquid mercury. phase. The liquid phase reduction is preferably carried out 40 During the roasting step of the prior art method de in two stages, i.e., a first stage in which the mercury con scribed above, approximately 70-90% of the mercury tent of the leach liquor is only partially reduced to form content of the ore is separated and a substantial portion an insoluble mercury compound which is separated from of the separated mercury vapor is lost along with the the mother liquor. After separation of the partially re SOa byproduct. Aside from the very obvious air pollu duced insoluble mercury compound, it is treated with an 45 tion problems associated with the prior art roasting additional quantity of the reducing agent to complete the process, there are other important disadvantages such as reduction of the insoluble mercury compound to elemental the corrosion problems caused by the SO, and the fact mercury. that the mercury product contains substantial quantities of contaminants such as antimony oxides, arsenic oxides, 50 and the like. Furthermore, roasting is economically This invention relates to a process for preparing ele feasible only when very high-grade ore deposits are avail mental mercury. ble, e.g., containing above 5 lbs. Hg/ton. If such ores More particularly, the invention concerns a process are not available, then the ore must be concentrated by for winning mercury from various mercury-containing gravity, flotation or other beneficiation procedures. sources such as its naturally occurring ores (e.g., cinna 55 According to the Thornhill process developed in ap bar), ore concentrates, amalgams of mercury with other proximately 1917, cinnabar ore was leached with a dilute metals such as copper, silver, gold, the alkaline metals, solution of sodium hydroxide and sodium sulfide. This selenium, tellurium, arsenic, etc., and compounds of mer reaction could be conducted at ambient temperature but cury with other elements such as the halogens, OXygen, at elevated pH, i.e., at least above 9, to produce a very sulfur, etc. 60 dilute pregnant liquor containing sodium thiomercurate, In a further and still more particular aspect, the inven e.g., approximately 20 grams Hg/liter or less. It was tion concerns a method for separating mercury from such highly critical to maintain the pH at least above 9 in mercury-containing sources by means of leaching with a order to prevent reversal of the leach reaction, i.e., novel leach liquid, the components of the leach liquid re decomposition of the sodium thiomercurate into mer acting during the progress of the leaching step to form a 65 curic sulfide and sodium sulfite. The sodium thiomercu hypohalite leach reagent in situ. rate solution was then reacted with aluminum and an According to another aspect of the invention, impurities excess of sodium hydroxide in solution to produce ele such as soluble compounds of arsenic, selenium, and tel mental mercury and other reaction byproducts. Mercury lurium, if present, are separated from the pregnant mer thus produced was ordinarily contaminated with other cury leach liquor in order to improve the purity of the 70 ore-derived impurities such as arsenic, antimony, unre final mercury product as such compounds would other acted HgS, etc. Because of the contaminated mercury, wise be reduced in the following mercury reduction steps. the product of the Thornhill process required triple dis 3,732,094 3 4. tillation in order to render it sufficiently pure for com method of recovering the elemental mercury product mercial sale and use. The economics of the Thornhill from the purified pregnant liquor produced in Stage 2; process were also unfavorable because of the extremely FIG. 6 illustrates an alternate method for carrying out high aluminum consumption, i.e., approximately 0.30 the reduction step of Stage 3 for reduction and recovering 0.35 pound of aluminum per pound of mercury produced. the mercury product from the purified pregnant liquor According to still another proposed prior art tech from Stage 2; nique, the cinnabar ore was leached with a sodium thio FIG. 7 illustrates (Stage 4) the recovery of the reduc sulfate solution to produce a soluble mercury-thiosulfate tion reagent used to reduce the mercury complex in the complex. This complex was then contacted with copper preferred embodiment illustrated in FIG. 5; and powder and the ensuing reaction produced a mercury FIG. 8 illustrates (Stage 5) the regeneration of the copper amalgam. The amalgam was then briquetted and O reduction reagent recovered according to the process of the briquets were distilled, driving off mercury vapor, FIG. 7, for re-use in Stage 3. the remaining copper being recycled for use in the step of reducing the mercury-thiosulfate complex.
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