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The Electrochemical Production of Ferrate THE ELECTROCHEMICAL PRODUCTION OF FERRATE IONS FROM IRON ANODES IN ALKALINE SOLUTIONS By NIGEL EDWIN TUFFREY B.Sc.(Eng.), A.R.S.M. Imperial College of Science and Technology (University of London), 1981 A THESIS SUBMITTED IN PARTIAL FULFILLMENT OF THE REQUIREMENTS FOR THE DEGREE OF MASTER OF APPLIED SCIENCE in THE FACULTY OF GRADUATE STUDIES Department of Metallurgical Engineering We accept this thesis as conforming to the required standard THE UNIVERSITY OF BRITISH COLUMBIA November 1983 (c) Nigel.Edwin Tuffrey, 1983 In presenting this thesis in partial fulfilment of the requirements for an advanced degree at the University of British Columbia, I agree that the Library shall make it freely available for reference and study. I further agree that permission for extensive copying of this thesis for scholarly purposes may be granted by the head of my department or by his or her representatives. It is understood that copying or publication of this thesis for financial gain shall not be allowed without my written permission. Department of fY\tlTflLLU RfilCfl U B^GXUBE9JLN& The University of British Columbia 2075 Wesbrook Place Vancouver, Canada V6T 1W5 Date DE-6 (2/79) i i ABSTRACT An investigation into the electrochemical production of ferrate ions by anodic dissolution of iron anodes in strong alkaline electrolytes has been carried out. The stability of ferrate ions in alkaline solutions and the dependence of the decomposition reaction on temperature, hydroxyl ion concentration and ferrate ion concentration were determined. The stability of ferrate ions is favoured by low temperatures and ferrate ion concentrations, and high hydroxyl ion concentrations. Particulate ferric hydroxide is catalytic to the ferrate decomposition.reaction. An electrochemical cell was designed to measure the rate of ferrate production. Using this cell and other techniques the efficiency of ferrate production as a function of the quantity of charge passed, the superficial current density and the hydroxyl ion concentration wane determined. The efficiency of ferrate formation is low and declines gradually to zero as increasing quantities of charge are passed. The efficiency of ferrate formation is independent of the super• ficial current density but declines rapidly as the hydroxyl ion concentration is reduced. A limited quantity of ferrate can be produced from an anode. There are indications that periodic current reversal can prevent the steady decline i i i in the ferrate production rate. The oxide or hydroxide layer which formed on the anode during electrolysis could not be positively identified. This layer was x-r.ay amorphous, thickened slowly and an outer layer dissolved or spalled as the layer grew. The anode behaviour was examined using potentiodynamic, potentiostatic and constant current techniques. Transient anode behaviour was observed during the period of ferrate formation. It is proposed that the rate of ferrate production and the decline in the efficiency of ferrate formation with in• creasing quantities of charge passed can be explained, by: 1) the involvement of the oxide or hydroxide layer on the anode in the ferrate formation mechanism, and 2) changes which occur in the chemical or physical properties of the anode layer during electrolysis. i v Table of Contents Pa^e Abstract ii Table of Contents iv List of Tables ... "ix List of FlCJUK'GS ••••••• •••••••••>•»••••••••.•••••''••-••'•••'•••••••'••'••'»•*••'•••••'.••• "»••'•-'•"•••••'•'•••'••• Acknowl edgement xv Chapter 1 INTRODUCTION 1 1.1 General 1 1.2 The Use of Ferrate Ions as an Oxidant 4 1.3 The General Properties of Ferrates 5 1.4 The Chemical Properties of Ferrate Solutions 7 1.4.1 The Chemical Kinetics of Ferrate Decomposition 1° 1.5 The Production of Ferrate Ions 13 1.5.1 Literature Review I3 1.5.1.1 Chemical Methods of Producing Ferrates 13 1.5.1.2 The Electrochemical Production of Ferrate Solutions 14 1.5.1.2.1 Low Current Density Studies I7 1.5.1.2.2 High Current Density Studies 18 1.5.1.2.3 General 20 1.5.2 The Methods of Production - Conclusion 20 1.6 The Electrochemical Generation of Ferrate Ions - An Overall View of the Reactions Involved 21 1.7 The Thermodynamic Properties of Strong Alkali Solutions.. 24 1.8 The Anodic Behaviour of Iron in Strong Alkaline Solutions 2^ 1.9 The Electrochemical Evolution of Oxygen 33 1.10 The Purpose of the Present Investigation 34 2 THE STABILITY OF FERRATE SOLUTIONS 36 2.1 Introduction 36 Chapter Page 2.2 Experimental 36 2.2.1 Reagents 36 2.2.2 Procedure 37 2.2.3 Errors 38 2.3 Results and Discussion 39 2.3.1 The Effects of the Ferrate Ion Concentrations 39 2.3.2 The Effects of Temperature 45 2.3.3 The Effects of Sodium Hydroxide Concentration 50 2.3.4 The Effects of Particulate Ferric Hydroxide 55 2.4 Summary and Comparison with Previous Work 55 2.5 The Additive Effects of the Individual Variables Affecting the Rate of Ferrate Decomposition 56 3 THE ELECTROCHEMICAL PRODUCTION OF FERRATE IONS •... 58 CO 3.1 Experimental Objectives 3.2 Experimental Problems 58 60 3.3 Experimental Methods 60 3.3.1 Beaker Experiments 61 3.3.2 Continuous Flow Anolyte Experiments 61 3.4 Experimental 61 3.4.1 Electrolyte Preparation 62 3.4.2 Electrode Materials and Preparation 3.4.3 Power Sources and Auxiliary Equipment 63 3.4.4 Materials of Construction 63 3.4.5 Electrochemical Cells 64 3.4.5.1 Beaker Experiments 64 3.4.5.2 Continuous Flow Anolyte Electrochemical 65 Cell 69 3.5 Analysis 69 3.6 Experimental Variables Examined 70 3.6.1 Beaker Experiments - Type 1 70 3.6.2 Beaker Experiments - Type 2 .... 70 3.6.3 Continuous Flow Anolyte Experiments v i Chapter Page 3.7 Experimental Errors — 71 3.7.1 Beaker Experiments 71 3.7.2 Continuous Flow Anolyte Experiments 72 3.8 Results and Observations 73 3.8.1 The Effects of Current Density on the Efficiency of Ferrate Formation 73 3.8.1.1 Continuous Flow Anolyte Experiments 73 3.8.1.2 Beaker experiments - Type 1 79 3.8.1.3 Beaker Experiments - Type 2 79 3.8.1.4 Summary of the Results of the Experiments Investigating the Effects of Superficial Current Density on the Efficiency of Fer• rate Information 83 3.8.2 The Effect of Alkali Type and Concentration 85 3.8.3 The Effects of Sodium Chloride Additions 90 3.8.4 The Effects of Current Reversal 90 3.8.5 Magnetite Anodes ... 93 3.9 Scale Morphologies 93 3.9.1 Iron Anodes 93 3.9.2 Magnetite Anodes 104 3.10 Summary of the Experimental Results of Chapter 3 106 4 THE ELECTROCHEMICAL BEHAVIOR OF IRON IN CONCENTRATED SODIUM HYDROXIDE SOLUTIONS 108 4.1 Techniques Used 108 4.2 The Measurement of the Electrochemical Potential 108 4.3 The Magnitude of the Measured Components of Anodic i Potential 110 4.3.1 The Potential Drop Due to Electrolyte Resistance .. 4.3.2 Potential Drop Across an Anode Surface Layer ...... 113 4.3.3 Anode Potential Component Due to the Electro- 1 chemical Reactions ^4 VI 1 Chapter Page 4.4 Experimental — ^5 4.4.1 Experimental Apparatus 115 4.4.2 Luggin Capillary Tube Probe ... 115 4.4.3 Reference Electrode 116 118 4.5 Experiments Conducted 4.5.1 Iron Electrodes 118 4.5.2 Magnetite Electrodes 119 1 ?fl 4.6 Results and Analysis 120 4.6.1 Potentiodynamic Studies of Iron 4.6.1.1 Summary of the Potentiodynamic Studies of j 126 Iron 127 4.6.2 Constant Current Studies of Iron 12g 4.6.2.1 Backside Luggin Capillary Results 4.6.2.2 Comparison of the Backside and Frontside 130 Luggin Capillary Probe Results 131 4.6.3 Potentiostatic Studies of Iron 131 4.6.4 Magnetite Anodes 131 4.6.4.1 Potentiodynamic Studies of Magnetite 4.6.4.2 Potentiostatic and Cathodization Studies of 134 Magnetite 5 DISCUSSION 137 1 37 5.1 Review of Results 141 5.2 The Mechanism of Ferrate Formation 5.2.1 The Role of the Anode Layer in the Ferrate Formation Mechanism ^ 5.3 The Decline of the Efficiency of Ferrate Formation 153 with Increased Quantity of Charge Passed 5.4 General Conclusions on the Ferrate Formation Reaction ... 161650 67 CONCLUSIONRECOMMENDATIONS S FOR FUTURE STUDY 162 v i i i Pagj. REFERENCES 166 APPENDICES A Reactions and Equilibria Pertaining to the Potential -pH Diagram for the Iron Water System at 25°C 170 A.l ; Substances.Considered 171 A.2.1. Two Dissolved Species 172 A.2.2 Two solid Substances 174 A. 2;3 One solid Substance and One Dissolved Substance ... 175 B The Analysis of Ferrate Containing Solutions 178 B. l Methods Available ......... "179 B.2 Chemical Analysis ......... 179 B.2.1 The Chromium (Iii) - Ferrous Method for the Analysis of Solid Ferrate 180 B.2.1.1 Analytical Procedure 181 B.3 Spectrophotometric Analysis 181 B.3.1 Calibration 182 B.4 The Electrochemical Analysis of Ferrate Ion Solutions 183 B.5 Total Iron Analysis 184 C Tables of Results 185 i x LIST OF TABLES Table Page 1.1 Previous studies of the electrochemical formation of ferrate ions . .... 15 1.2 Activity of water for sodium hydroxide solutions as a function of temperature 25 1.3 Mean molal activity coefficients for sodium hydroxide as a function of temperature and. concentration 26 2.1 The effect of temperature on the graphically determined ferrate decomposition rate constant [NaOH] =• 14.3 g.mol/1 48 2.2 The effect of hydroxy! ion concentration on the graphically determined ferrate decomposition rate constant @ 323 K 50 3.1 Comparison of the total iron content of continuous flow anolyte experimental samples with, that measured as ferrate ions 77 C.l to The effects of ferrate concentration on the ferrate C.4 decomposition rate 186 C.5 to The effects of temperature on the ferrate decomposition C.9 rate 187 CIO to The effects of sodium hydroxide concentration on the rate C.12 of ferrate decomposition ^89 C.13 to Continuous flow anolyte experiments (Armco Iron Anodes) C.l8 C.13 Ferrate formation at 10 KA/m2 190 C.14 Ferrate formation at TO KA/m2 190 C.15 Ferrate formation at i9 KA/m2 191 C.
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