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The Extraction of Iron, Cobalt, and Nickel Sulfates

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The Extraction of Iron, Cobalt, and Nickel Sulfates THE EXTRACTION OF IRON, COBALT, AND NICKEL SULFATES Dissertation Presented in Partial Fulfillment of the Requirements for the Degree Doctor of Philosophy in the Graduate School of The Ohio State University By CARL SOLOMON SCHLEA, B.Ch.E., M.Sc. The Ohio State University 1955-- Approved by • \ C , Dr. C. J. Geankoplis, Adviser Chemical Engineering Department i Acknowledgement The author would like to express his appreciation to his adviser, Dr. C. J. Geankoplis, for his very generous assistance and helpful advice. Grateful acknowledgement is made to the Battelle Memorial Institute for their financial assistance by means of a fellowship for the years 1952-1955. TABLE OP CONTENTS Page ABSTRACT................ 1 INTRODUCTION ....................................... 4 LITERATURE R E V I E W .................................. 10 1. The Extraction of Metal Halides .......... 10 2. The Extraction of Metal Nitrates ........ 18 3. The Extraction of Thiocyanates............... 24- 4-. The Extraction of Metal Sulfates ......... 26 5. The Extraction of Cobalt and Nickel Acetates and. 28 the Separation of Chromium and Vanadium 6. The Extraction of Chelate Compounds ........ 28. STATEMENT OF THE PROBLEM............................. 30 THEORY...................... 32 ANALYTICAL METHODS.................................. 36 1. Aqueous-Phase Analyses .......... ....... 36 2. Organic-Phase A n a lyses................. 4& EXPERIMENTAL PROCEDURE .............................. 62 1. Equipment.................. 62 2. Extraction Procedure.................. 65 3. Phase Diagram Determination ................ 71 4-. Materials Used................... 72 EXPERIMENTAL D A T A ............. 77 1. Solvent and Additive Search D a t a ......... 77 2. Extractions With Normal Butyl Alcohol..... 94. 3. Solubility Determinations With Normal Butyl Alcohol 94. TREATMENT AND DISCUSSION OF D A T A .................... 106 1. Calculations ................... 106 2. Discussion of Solvent Search and Additive Search. 108 Data iii TABLE OF CONTENTS (Continued) Page a. Solvent Search ................ 10S b. Additive S e a r c h ............. 113 c. Selection of the Solvent......... 114 3. Correlation and Discussion of Distribution Data . 115 a. Effect of Sulfuric A c i d ............... 116 b. Effect of Metal and Metal Composition .... 120 c. Effect of Temperature................. 126 d. The Distribution of Sulfuric Acid............ 129 e. Distribution in Mixtures................... 132 f. Density Correlations ............. I36 4» Solubility Determinations....................... 136 CONCLUSIONS. .................................... 144 SUGGESTIONS FOR FURTHER INVESTIGATIONS .................. 147 NOMENCLATURE.......... ............... ............149 autobiography:........................................ 151 iv LIST OF TABLES Page TABLE 1. ERRORS IN COLORIMETRIC ANALYSES.............. 51 TABLE 2. MATERIALS U S E D .......... .......... 74 TABLE 3. SOLVENT SEARCH DATA AT 25.0°C................ 78 TABLE A. DISTRIBUTION IN SYSTEMS: METAL SULFATE - . 90 WATER - SOLVENT - ADDITIVE AT 25.0°C. TABLE 5. DISTRIBUTION IN SYSTEMS: NICKEL SULFATE - . , ; 95 SULFURIC ACID - WATER - NORMAL BUTYL ALCOHOL - AT 25.0°C. TABLE 6. DISTRIBUTION IN THE SYSTEM: COBALT SULFATE - i . 96 SULFURIC ACID - WATER - NORMAL BUTYL ALCOHOL AT 25.0°C. TABLE 7. DISTRIBUTION IN THE SYSTEM: FERRIC SULFATE - . ♦ 97 SULFURIC ACID - WATER - NORMAL BUTYL ALCOHOL AT 25.0°C. TABLE 8. DISTRIBUTION IN THE SYSTEM: SULFURIC ACID - . 98 . WATER - NORMAL BUTYL ALCOHOL AT 25.0°C. TABLE 9. DISTRIBUTION IN THE SYSTEM: NICKEL SULFATE - . 99 SULFURIC ACID - WATER - NORMAL BUTYL ALCOHOL AT VARIOUS TEMPERATURES TABLE 1C . DISTRIBUTION IN THE SYSTEM: COBALT SULFATE - . 100 SULFURIC ACID - WATER - NORMAL BUTYL ALCOHOL AT VARIOUS TEMPERATURES TABLE 13 . DISTRIBUTION IN THE SYSTEM: FERRIC SULFATE - . ”101 SULFURIC ACID - WATER - NORMAL BUTYL ALCOHOL AT VARIOUS TEMPERATURES TABLE 12.. DISTRIBUTION IN THE SYSTEM: NICKEL SULFATE - . 102 COBALT SULFATE - FERRIC SULFATE - SULFURIC ACID - WATER - NORMAL BUTYL ALCOHOL AT 25.0°C. TABLE 13. SOLUBILITY ENVELOPE FOR THE SYSTEM: SULFURIC . 103 ACID - WATER - NORMAL BUTYL ALCOHOL AT 25.0°C. V LIST OP TABLES (Continued) Page TABLE 14. THE EFFECT OF METAL SULFATES ON T H E .............104 SOLUBILITY OF NORMAL BUTYL ALCOHOL IN AQUEOUS SULFURIC ACID SOLUTIONS AT 25.0°C. TABLE 15. THE EFFECT OF NICKEL SULFATE ON T H E .............105 SOLUBILITY OF WATER IN SULFURIC ACID SOLUTIONS OF NORMAL BUTYL ALCOHOL AT 25.0°C. TABLE 16. SEPARATION FACTORS AT 25.0°C....................121 TABLE 17. EXTRACTION IN MIXTURES COMPARED TO T H A T ...... 134 WHEN SALTS EQUILIBRATED SEPARATELY AT 25.0°C. TABLE IS. TIE LINE DATA FOR THE SYSTEM: SULFURIC..... 140 ACID - WATER - NORMAL BUTYL ALCOHOL AT 25.0°C. vi LIST OF FIGURES Page FIGURE 10. THE DISTRIBUTION OF CHROMIC SULFATE AND .... 27 SULFATE BETWEEN NORMAL BUTYL ALCOHOL AND AQUEOUS SULFURIC ACID FIGURE 2„ THE EFFECT OF METAL SULFATES AND NORMAL BUTYL . 1(3 ALCOHOL ON SULFURIC ACID NEUTRALIZATION * ’ ' FIGURE 3o ERRORS IN COLORIMETRIC ANALYTICAL PROCEDURES . h9 FIGURE lw THE DISTRIBUTION OF NICKEL SULFATE BETWEEN. 0H 7 NORMAL BUTYL ALCOHOL AND AQUEOUS SULFURIC ACID FIGURE 5. THE DISTRIBUTION OF COBALT SULFATE BETWEEN. • .118 NOMAL BUTYL ALCOHOL AND AQUEOUS SULFURIC ACID FIGURE 6*. THE DISTRIBUTION OF FERRIC SULFATE BETWEEN. .119 NORMAL BUTYL ALCOHOL AND AQUEOUS SULFURIC ACID FIGURE 7* THE EFFECT OF SULFURIC ACID ON THE. ..... .122 SEPARATION FACTOR BETWEEN IRON AND NICKEL AT 25.0°C. FIGURE 8 ,. THE EFFECT OF SULFURIC ACID ON THE. ..... ,123 SEPARATION FACTOR BETWEEN IRON AND COBALT AT 25.0°C. FIGURE 9o THE EFFECT OF SULFURIC ACID ON THE........ .121* SEPARATION FACTOR BETWEEN COBALT AND NICKEL AT 25.0°C* FIGURE 10* THE EFFECT OF METAL CONCENTRATION ON. .125 DISTRIBUTION AT CONSTANT ACID CONCENTRATIONS FIGURE 11*. THE EFFECT OF TEMPERATURE ON DISTRIBUTION . 0127 FIGURE 12 o. THE EFFECT OF TEMPERATURE ON DISTRIBUTION , . ,128 vii LI SI’ OF FIGURES (Continued) FIGURE 13. THE DISTRIBUTION OF SULFURIC ACID BETWEEN . , * 130 • WATER AND NOMAL BUTIL ALCOHOL AT 25.0°C., FERRIC SULFATE PRESENT FIGURE lUo THE DISTRIBUTION OF SULFURIC ACID BETWEEN o . o 131 WATER AND NORMAL BUTYL ALCOHOL AT 25a0°Co, COBALT SULFATE AND NICKEL SULFATE PRESENT FIGURE 1$. DISTRIBUTION IN MIXTURES AT 2$.0°C, 133 FIGURE 160 EXTRACTION IN MIXTURES COMPARED TO THAT WHEN. ,13$ EACH SALT EQUILIBRATED SEPARATELY FIGURE 17* DENSITY OF THE WATER PHASE IN THE SYSTEM. 0 • » 137 HgSOj^ - NiSO^ - HgO - nC^HpOH AT 2S.0°C» FIGURE 18*. DENSITY OF THE WATER PHASE IN THE SYSTEM* , . 0 138 HgSO^ - NiSO^ - HgO - n C ^ O H AT 20.0°C* FIGURE 19+ DENSITY OF THE N-BUTYL ALCOHOL PHASE IN THE „ * 139 SYSTEM* H2SO^ - NiSO^ - HgO - n C ^ O H AT 20 .0 °C*. FIGURE 20* PHASE DIAGRAM FOR THE SfSTEM:' SULFURIC ACID lUl WATER - NORMAL BUTYL ALCOHOL AT 25,0°C„ FIGURE 21, THE EFFECT OF METAL SULFATES ON THE , , . „ 1^2 SOLUBILITY OF NORMAL BUTYL ALCOHOL IN WATER AT 25bO°C. 1 ABSTRACT The separation of iron, cobalt, and nickel has long been of commercial and academic importance. In recent years, interest has been shown in the use of liquid-liquid extraction to separate compon­ ents of mixtures of inorganic compounds. Some cobalt and nickel recovery processes involve the use of sulfuric acid solutions of the metals* This investigation was carried out to thoroughly study the use of liquid-liquid extraction as a method of separating iron, cobalt, and nickel sulfates from aqueous solutions. The first series of tests were made to determine distri­ bution data for the pure metal sulfates between water and a large number of organic solvents at 2£.Q°C. when each metal was equilibrated separately. The effects of sulfuric acid, sodium sulfate, and ammoni­ um sulfate on the distribution characteristics were determined for each metal. Distribution runs were then carried out with the best solvent* The alkyl acid phosphates were found to be the best series of compounds for extraction purposes* Supplementary experimental work showed that a chemical reaction took place and the sulfate ion was not extracted. These compounds were thus eliminated as possible extraction media. Most non-acidic organic compounds did not extract iron, cobalt, and nickel sulfates to any measurable degree. Of these non-acidic organic solvents, the lower alcohols were found to be the best series of compounds to extract the metal sulfates. Sulfuric acid increased distribution coefficients markedly, while sodium sulfate and ammonium sulfate had detrimental effects on extraction. 2 Electrostatic considerations of ions in solution could not explain the extraction,* Solvents with high dielectric constants ex­ tracted less than some with considerably lower dielectric constants# Also, extraction could not be correlated with the degree of water solubility in the organic phase# Although no quantitative information of the strength of hydrogen bonds is available, the relative order of magnitude of distribution coefficients changed in much the same manner as relative strengths of hydrogen bonding characteristics of the organic solvents# Normal butyl alcohol was chosen in conjunction with sulfuric acid to determine extraction characteristics with iron, cobalt, and mickel sulfates# Distribution coefficients, when each metal was equilibrated separately, were on the order of magnitude of 0.0001 at 25#0°C# By adding up to 250 grams sulfuric acid per liter of the water phase, these distribution coefficients increased over 100 times, values over 0.01 being obtained* Separation factors were
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