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Removal of Cyanide and Metals from Mineral Processing Waste Waters

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Removal of Cyanide and Metals from Mineral Processing Waste Waters ~ IRII8836 U.S. Bureau of M' S I mas ~ Bureau of Mines Report of Investigations/1983 PO fane Research Cente f. 315 MOl1tgomer A r Spokane WA .. Y ve. 9207 \-\ LlBRAR/ ~ I, Removal of Cyanide and Metals From Mineral Processing Waste Waters By Joseph E. Schiller UNITED STATES DEPARTMENT OF THE INTERIOR Report of Investigations 8836 Removal of Cyanide and Metals From Mineral Processing Waste Waters By Joseph E. Schiller UNITED STATES DEPARTMENT OF THE INTERIOR William P. Clark, Secretary BUREAU OF MINES Robert C. Horton, Director Library of Congress Cataloging in Publication Data: Schiller, Joseph E Removal of eyanide and metals from mineral proeessing waste waters. (Report of investigations; 8836) Bibliography: p. 8. Supt. of Docs. no.: I 28.23:8836. 1. Sewage-Purificadon-Cyanide removal. 2. Sewage-Purifica­ don-Heavy metals l'emoval. 3. Mineral industries-Waste disposal. I. Title. II. Series: Report of investigations (United States. Bureau of Mines) ; 8836. TN23.U43 [TD758.5.C93] 622s [669] 83·600305 CONTENTS Abs t r ac t. • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • .. • • • • • • • 1 ExperimentalIntroduction. work..............................................................• • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • .. • • • • 32 Results and discussion •••••••••••••••••••••••••••••• o.......................... 4 Cyanide and metals removal................................................... 4 Theory of operation.......................................................... 4 Effect of pH on free-cyanide reaction rate................................... 5 Reaction of Fe2+ with cyanide................................................ 5 Mechanism of metals and ferrocyanide removal.................................. 6 Use of Fe3+ salts for Cu 2+ removal........................................... 6 Activated carbon and prussian blue........................................... 7 Canclus ions ••••••••••••••••••••••••••••••• III • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • 7 References. • • ••••• •• •• ...... •• •• •••••• • • •• ••••• ... •• ••• .... •••• ......... • ••• •••• • • • 8 TABLES 1. Analysis of cyanide-containing solutions before treatment •••••••••••••••••• 3 2. Pseudo first-order rate constant for the disappearance of free cyanide (initially at 10 mg/L) in a solution initially containing 6 x 10- 3 M hydrogen peroxide and 10-2 M sodium thiosulfate ••••••••••••••••••••••••••• 5 3. Effect of pH on residual ~ree cyanide when 0.5 mmol/L Fe 2+ ts added to a lO-mg/L cyanide solution •••••••••••••••••••••••••••••••••••••••••••••••••• 6 4. Residual cyanide after addition of Fe 2+ to a solution of free cyanide at pH 8.5 .............................................................................. (0 • C' • • • • 6 5. Copper remaining in a solution treated with Fe2(S04)3 in the pH range of 5 to 8 ................................................................. $ ••••• 7 UNIT OF MEASURE ABBREVIATIONS USED IN THIS REPORT °C degree Celsius min minute h hour mmol/L millimole per liter ;J I, M molar (mole per liter) mol mole l' mg/L milligram per liter ppm part per million REMOVAL OF CYANIDE AND METALS FROM MINERAL PROCESSING WASTE WATERS By Joseph E. Schiller 1 ABSTRACT The Bureau of Mines is investigating methods to treat waste water that contains cyanide. This report describes a new method that removes heavy metals and all forms of cyanide. In the first step, hydrogen peroxide and sodium thiosulfate are added at pH 7 to 9 in a 1:2 molar ratio to convert free and weakly complexed cyanide to nontoxic thiocyanate. Then steryldimethylbenzylammonium chloride is added to precipitate ferro­ cyanide, and finally, fe·rric sulfate is added as a sweep floc and sequestrant for heavy metals. After the suspended solids settle, the water is polished by filtering. The water initially contained 1 to 5 mg/L Fe, 1 to 5 mg/L Cu, and 10 to 30 mg/L total cyanide; the level of each of these constituents was reduced to less than 0.02 mg/L. lsupervisory physical scientist, Twin cities Research Center, Bureau of Mine;, Min­ neapolis, MN. 2 INTRODUCTION ~~e Bureau of Mines is conducting re­ are small and located in remote areas. search to improve methods for treating Therefore, a treatment process is needed mining and mineral processing waste that is reliable, is capable of being waters. Water is needed in virtually automated, and does not use difficult- every mineral operation, and new technol­ to-handle chemicals. ogy is needed to purify the aqueous wastes so that the resultant clean water This report describes a new approach can be recycled or discharged safely. for removing heavy metals and strongly Process waters may contain a variety of complexed cyanides from water and con­ contaminants, including suspended par­ verting free and weakly complexed cyanide ticles, undesirable dissolved metals or to nontoxic thiocyanate and cyanate. The nonmetal ions, and chemicals used in min­ method utilizes three steps that accom­ ing and beneficiation processes. One plish the following: (1) conversion of current need is for better methods to free and weakly complexed cyanides to handle mineral processing wastes that nontoxic forms, (2) precipitation of contain cyanide. strongly complexed cyanides and metals, and (3) sedimentation and filtration to Cyanide is used widely in leaching pre­ remove solids. In the first step, hydro­ cious metal ores, and it is sometimes gen peroxide reacts with the thiosulfate employed in flotation of sulfide miner­ ion to form an intermediate (1)2 that, in als. For over 50 years, cyanide leaching turn, reacts with most of the free and has been the method of choice for dis­ weakly complexed cyanide to form solving finely disseminated gold and thiocyanate. silver from their ores. In typical com­ mercial operations, a 0.1- to 0.3-pct The method described in this report was caustic cyanide solution is percolated evaluated in laboratory-scale experi­ through crushed or ground ore to dissolve ments. It was developed mainly for the precious metals. The gold and silver treating waste waters from precious metal are won from the "pregnant" leach solu­ ore leaching, but it could be used for tion, usually by cementation with zinc other wastes containing similar metals dust. This leaves a waste solution that and forms of cyanide. Depending on site­ contains some of the original free cya­ specific agreements, Federal and State nide along with complexed cyanides, base regulations generally require that the metals (such as copper and iron), and total cyanide content of water discharged thiocyanate. These ions were formed by to the environment be less than 0.02 mg/L reaction of cyanide with various gangue (2). Since mining and mineral process­ minerals in the ore. The dilute solu- ing operations seldom release water tions, diverse forms of cyanide and met­ into municipal treatment systems, treat­ als, and high toxicity make effective ment methods used by these operations treatment of precious metal leaching must enable their discharged water to wastes a definite necessity and a signif- meet these requirements. icant challenge. Technical or economic problems make None of the present cyanide treatment existing treatment methods undesirable to methods are very effective with precious the mining industry. Either the cost is metal leach solution. Therefore, the considered excessive, or the cyanide con­ Bureau is conducting studies to devise a tent is not reduced to sufficiently low method for handling the constituents com­ levels. Common industrial processes to monly found in mining wastes. Due to the present high price for gold and silver, 2underlined numbers in parentheses re­ many new cyanide leaching operations are fer to items in the list of references at being started. A large fraction of these the end of this report. 3 treat cyanide wastes include oxidation, chemical industry prior to secondary ion exchange, complexation, volatiliza­ treatment. This method is unsuitable as tion with or without cyanide recovery, the sole treatment, because the cyanide and other lesser used methods (3-4). remains soluble and appears in the total Although mining companies h'ave evaluated cyanide analysis. By acidifying a waste these methods on a small scale, none have to liberate gaseous hydrogen cyanide, gained universal acceptance. Most com­ most of the free cyanide in a waste can monly, mines in North America treat be removed. This form of cyanide can be cyanide wastes by oxidation or by dis­ recovered by absorption in a base or charging waste water after dilution and vented if quantities are small. detention in a tailings pond. The most widely used oxidation system is alkaline Two very new methods specifically chlorination, where reactions are quite designed for mining wastes use sulfur rapid and most metals are removed. How­ dioxide or sulfite salts (5-6). In the ever, ferrocyanide is not destroyed in International Nickel CO. (INCO)3 process, this method, and chlorine consumption can 2 to 5 pct 802 in air is bubbled through be very high, since thiocyanate and other a waste containing at least 50 mg/L dis­ sulfur species react with chlorine. solved Cu. Cyanide levels are reduced from several hundred milligrams per liter Alternatively, ozone and hydrogen per­ to 1 mg/L in 10 to 30 min. This method oxide have been investigated as oxidants. would best be applied to very concen­ Both are usually
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