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THE ELECTROLYTIC PRODUCTION of PEROXYDISULFURIC ACID It USING PERIODICALLY REVERSED DIRECT CURRENT and ALTERNATING CURRENT SUPERIMPOSED on DIRECT CURRENT

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THE ELECTROLYTIC PRODUCTION of PEROXYDISULFURIC ACID It USING PERIODICALLY REVERSED DIRECT CURRENT and ALTERNATING CURRENT SUPERIMPOSED on DIRECT CURRENT THE ELECTROLYTIC PRODUCTION OF PEROXYDISULFURIC ACID It USING PERIODICALLY REVERSED DIRECT CURRENT AND ALTERNATING CURRENT SUPERIMPOSED ON DIRECT CURRENT by Sin-Chou Fan Thesis submitted to the Graduate Faculty of the Virginia Polytechnic Institute in candidacy for the degree of MASTER OF SCIENCE in CHEMICAL ENGINEERING APPROVED: APPROVED: ~rector of Graduate Studies Head of Department ~ean of'"Engineering Major· Professor v July, 1956 Blacksburg, Virginia -ii- TABLE OF CONTENTS Page I. INTRODUCTION • • • . • • • • . • • • 1 II. LITERATURE REVIEW . 3 Properties and Uses of Peroxydisulfuric Acid . 3 Methods of Preparing Peroxydisulfuric Acid • . 5 Chemical Methods of Preparing Peroxy- disulfuric Acid . 5 Electrolytic Methods of Preparing Peroxy- disulfuri c Acid • • • • • • • 6 Electrolysis with Periodically- Reversed Direct Current • • • • . 11 Definitions • • • • • • 11 Periodic Reverse Wave Forms • • 13 Use of Complex Wave Forms . 16 Periodic Reverse Electro- chemical Reaction • • • . 16 Limitations of Periodic Reverse Electrolysis • . 18 Current Reversal Equipment • 19 Electrolysis with Alteniating Current Superimposed on Direct Current • • • • • • • . 20 Electric Double Layer . 20 -iii- Page Polarizable Electrode • • • • • 21 Types of Superimposed Alternating Current • • • • • 23 Depolarization by Alter- nat~ng Current • • • • • • • • 26 Experimental Work on Alternating Current Depolarization • • • . 34 Electrolysis of Sulfuric Acid with Alternating Current Superimposed on Direct Current • • • • • • 40 Applications • • • • • • 43 Electrolytic Production of Lead Chromate Using Alternating Current Superimposed on Direct Current • • • • • • 44 Other Applications • • • • . 46 Advantages of Alternating Current Superimposed on Direct Current • • • • • . 47 Comparison of Superimposed Alternating Current Plating with Periodic Reverse Current Plating . Electric Circuits for Superimposing Alternating Current • • • • • • • • . 50 III. EXPERIMENTAL • • • • . • • • . 57 Purpose of Investigation • • • • • • 57 -iv- Page Plan of Investigation • • . 57 Literature Search . 57 General Procedure . 58 Evaluation of Results . 59 Materials • • • • . 60 Apparatus • • . • • • • • . 62 Method of Procedure • • • • . 67 Operating Procedure for Direct Current Electrolyses • • • • • . 67 Operating Procedure for Periodically-Reversed Direct Current Tests • . 71 Operating Procedure for Electrolyses Performed with Alternating Current Superimposed on Direct Current • • • • • • • • • • • 73 Relationship Between Root- Mean-Square and Peak Values of High Frequency Alternating Current ••• . 76 Operating Procedure for Measuring Anode Potential- Current in Sulfuric Acid • . 76 Operating Procedure for Measuring the Anode Potential-Current in Sulfuric Acid with Super- imposed Alternating Current • • • • • • • • • • • 78 Analytical Procedure • . 78 -v- Page Data and Results . 80 Calibration Data for the Periodic Reverser • • . 80 Periodic Reverser Calibra- tion Curves • • • • • • • • • 80 Operating Conditions, Data and Results for the Elec- trolytic Production of Peroxydisulfuric Acid Using Direct Current • • • . 80 Operating Conditions, Data and Results for the Elec- trolytic Production of Peroxydisulfuric Acid Using Periodically Reversed, Direct Current • • • • • • • • 80 Operating Conditions, Data and Results for Electro- lytic Production of Peroxy- disulfuric Acid Using Alternating Current, 60 Cycles per Second, Super- imposed on Direct Current • • 84 Operating Conditions, Data and Results for the Elec- trolytic Production of Peroxydisulfuric Acid Using Alternating Current, 240 and 500 Cycles per Second, Superimposed on Direct Current • • • • • • • • • • • 84 Data from the Measurements of Current-Anode Potential Curve in Sulfuric Acid with Stirring • • • • • • • • • • • 84 -vi- Page Data from the Measurements of Current-Anode Poten- tial Curve in Sulfuric Acid without Stirring • • • • 89 Data from the Measurements of Current-Anode Poten- tial Curve in Sulfuric Acid by Using 60 Cycles per Second, Superimposed Alternating Current • • • • • 89 Sample Calculations ••• . 92 Volume of Anolyte . 92 Anode Current Density • • • 94 Peroxydisulfuric Acid Produced • • • • . 95 Actual Current • • • • . 96 Current Efficiency • . 97 Direct to Reverse Current Ratio from Coulometers • • • • 98 Ratio of Peak Alternating Current to Direct Current . 100 IV. DISCUSSION • . 101 General Discussion . 101 Previous Work . 101 Selection of Anolyte Concentration • • . • • 102 Influence of Temperature on the Formation of Peroxy- disulfuric Acid • • • • • 103 -vii- Page Treatment of Platinum Anode • • • • • • . 104 Influence of Current Density • • • • • • • • • • • 105 Formation and Decomposition of Peroxydisulfuric Acid • • • 106 Decomposition Potential of Sulfuric Acid of Specific Gravity 1.4 •• . 107 Discussion of Results from Direct Current Electrolyses • • 113 Hydrogen and Oxygen Bubbles • • 113 Effect of Current Density • • • 113 Relationship Between the Time of Electrolysis and Current Efficiency . 118 Discussion of Results for Periodically-Reversed, Direct Current Electrolysis • • • • 121 Production of Peroxydisul- furic Acid Using Period- ically-Reversed, Direct Current • • • • • • • • • • • 121 Depolarization Action of Periodically-Reversed, Direct Current • • • • . • • 123 Ammeter Fluctuations During Current Reversal • • • ~ • • • 125 Time and Current Ratio • . 128 Comparison of Current Efficiencies • • • • • • • • • 129 -viii- Page Discussion of Results from Alternating Current Super- imposed on Direct Current Electrolyses • • • • • • • • • • • 131 Formation of Peroxydisul- fµric Acid with 60-Cycle, Alternating Current Super- imposed on Direct Current • • 131 Formation of Peroxydisul- furic Acid with 500-Cycle, Superimposed Alternating Current • • • • • • • • • • • 135 Formation of Pero:x:ydisul- furic Acid with 240-Cycle Alternating Current Super- imposed on Direct Current • • 136 Summary of Effect of Frequency • • • • • • • • • • 136 Behavior of Platinum Electrode • • • • • . Current Efficiency • • • • • . Comparison of Current Efficiencies • • • • . • • • 139 Recommendations • • • • • • . 142 Limitations • • • • • • . 145 v. CONCLUSIONS - • • • • • • • • • • . 148 VI. SUMMARY • • • • • • • • • • • • • • • • • 151 VII. BIBLIOGRAPHY • • • . • • • • • . 155 VIII. ACKNOWIEDGMENTS . 162 IX. VITA • • • • • • . • • 163 -ix- LIST OF TABLES Page TABLE I. Calibration Data for Plater's Research Corporation ' Periodic Reverser . • . • • 81 TABLE II. Operating Conditions, Data and Results Obtained from the Electrolytic Production of Peroxydisulfuric Acid . • • . • • 83 TABLE III. Operating Conditions, Data and Results Obtained from the Electrolytic Production of Peroxydisulfuric Acid Using Periodically-Reversed, Direct Current . • • • • . • 85 TABLE IV. Operating Conditions, Data and Results Obtained from the Electrolytic Production of Peroxydisulfuric Acid Using Alternating Current, 60 Cycles, Superimposed on Direct Current . • . • • • . • 86 TABLE v. Operating Conditions, Data and Results Obtained from the Electrolytic Production of Peroxydisulfuric Acid Using High Frequency of Alternating Current Superimposed on Direct Current . • • • • . • . 87 TABLE VI. Data from the Measurements of Current-Anode Potential Curve in Sulfuric Acid with Stirring • • . • • • • . • • 88 TABLE VII. Data from the Measurements of Current-Anode Potential Curve in Sulfuric Acid without Stirring • • • • • • . • 90 -x- Page TABLE VIII. Data from the Measurements of Current-Anode Potential Curve in Sulfuric Acid Using Superimposed alternating Current • • • • • • • • • • • • • 91 -xi- LIST OF FIGURES Page Figure 1. Time-Current Curves for Various Wave Forms . • • • . • 17 Figure 2. Representation of the Poten- tial-Distance Relation for the Electrode-Solution Interface . • • • . • • • • . • 22 Figure 3. Time-Current Relations for Alternating Current Superimposed on Direct Current • • . • . • • • • . 24 Figure 4. Experimental Hook-Up Used to Study the Effect of Super- imposed Alternating Current on Direct Current on the Electrodeposition of Aluminum . • • . • . • • • • . • . 52 Figure 5. Experimental Hook-Up Used to Study the Effect of Super- imposed Alternating Current on Direct Current on the Anodic Behavior of A-A Type Nickel . • . • . • 53 Figure 6. Experimental Hook-Up Used to Study the Effect of Super- imposed Alternating Current on Direct Current on the Anodic Behavior of Nickel . • • 55 Figure 7. Experimental Hook-Up Used to Study the Effect of Super- imposed Alternating Current on Direct Current on the Electrodeposition of Copper- Lead Alloys from Fluoborate Solutions • • • . • • . • 56 -xii- Page Figure 8. Wiring Diagram of Equipment Used to Study the Electro- lytic Production of Peroxy- disulfuric Acid Using Direct Current • • • • • • • . 69 Figure 9. Wiring Diagram of Equipment Used to Study the Electro- lytic Production of Peroxy- disulfuric Acid Using Periodically Reversed Direct Current • • • • • • . 72 Figure 10. Experimental Circuit Used to Study the Effect of Super- imposed Alternating Current on the Production of Peroxy- disulfuri c Acid • • • • • • • • • 74 Figure 11. Experimental Circuit Used for Measuring Current-Anode Potential Curve • • • • • • . 77 Figure 12. Graph Showing the Relationship Between the Ratio of Direct to Reverse Time and the Dial Settings for the Periodic Reverser • • • • • • • • • • . 82 Figure 13. Relationship Between Current and Anode Potential in Sulfuric Acid with Stirring . 108 Figure 14. Relationship Between Current and Anode Potential in Sulfuric Acid without
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