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A Study of Leonardite-Water Gel Systems Philip H University of North Dakota UND Scholarly Commons Theses and Dissertations Theses, Dissertations, and Senior Projects 1-1-1968 A Study of Leonardite-Water Gel Systems Philip H. Tufte Follow this and additional works at: https://commons.und.edu/theses Recommended Citation Tufte, Philip H., "A Study of Leonardite-Water Gel Systems" (1968). Theses and Dissertations. 662. https://commons.und.edu/theses/662 This Thesis is brought to you for free and open access by the Theses, Dissertations, and Senior Projects at UND Scholarly Commons. It has been accepted for inclusion in Theses and Dissertations by an authorized administrator of UND Scholarly Commons. For more information, please contact [email protected]. A STUDY OF LEONARDITE-WATER GEL SYSTEMS by Philip H. Tufte B.S. in Chemical Engineering, University of North Dakota 1961 A Thesis Submitted to the Faculty of the University of North Dakota in partial fulfillment of the requirements for the Degree of Master of Science Grand Forks, North Dakota January 1968 V This thesis submitted by Philip H. Tufte in partial fulfillment of the requirements for the Degree of Master of Science from the Univer­ sity of North Dakota is hereby approved by the Faculty Advisory Committee under whom the work has been done. ii 272406 Permission Title A STUDY OF LEONARDITE-WATER GEL SYSTEMS Department Chemical Engineering Degree Master of Science In presenting this thesis in partial fulfillment of the requirements for a graduate degree from the University of North Dakota, I agree that the Library of this University shall make it freely available for inspection. I further agree that permission for extensive copying of this thesis for scholarly purposes may be granted by the professor who supervised my thesis work or, in his absence, by the Chair­ man of the Department or the Dean of the College in which my thesis work was done. It is understood that any copying or publication or other use of this thesis or part thereof for financial gain shall not be allowed without my written per­ mission. It is also understood that due recognition shall be given to me and to the University of North Dakota in any scholarly use which may be made of any material in my thesis. Signature Date 7 / iii ACKNOWLEDGMENTS The writer expresses great appreciation to Professor D. E. Severson for his aid in directing and editing this thesis. Appreciation is also extended to Professors W. R. Kube and A. M. Cooley for their constructive criticisms and advice and to Professor G. A. Kemper for serving as an adviser. Very special thanks is given to Professor D. R. Skidmore who guided this research until he left the University for further academic pursuits. The writer is also indebted to Mr. D. J. Winge for his drawing and to Mrs. Eugene Rose for her fine typing. Especially, I thank my wife, Linda, for her patience and encouragement. iv TABLE OF CONTENTS Page ACKNOWLEDGMENTS .............................................. iv LIST OF T A B L E S .............................................. vi LIST OF FIGURES.............................................. vii A B S T R A C T .................................................... viii Chapter I. INTRODUCTION........................... 1 II. PREVIOUS W O R K ....................................... 4 III. MATERIALS........................................... 10 IV. TERMINOLOGY, EQUIPMENT AND EXPERIMENTAL PROCEDURES . 13 V. LEONARDITE-WATER SLURRIES ........................... 18 VI. LEONARDITE-SODIUM HYDROXIDE-WATER GEL SYSTEMS (SODIUM GEL SYSTEMS) .............................. 21 VII. LEONARDITE-SODIUM HYDROXIDE-CALCIUM HYDROXIDE- WATER GEL SYSTEMS (CALCIUM GEL SYSTEMS)............ 39 VIII. SUMMARY.............................................. 45 APPENDICES A. MOISTURE TESTING .................................... 46 B. BROOKFIELD CALIBRATION .............................. 48 C. SUGGESTIONS FOR FUTURE EXPERIMENTATION .............. 52 REFERENCES ................... 55 V LIST OF TABLES Table Page 1. Proximate and Ultimate Analysis of Leonardite ........... 11 2. Chemical Analysis of Leonardite................ 11 3. Analysis of Leonardite A s h ............................ 12 4. Example of a Calcium Gel Sample Ru n ..................... 17 5. Viscosity of Leonardite-Water Slurries ................ 18 6 . Reproducibility of Gel V i s c o s i t y ...................... 26 7. Effect of Temperature on Sodium Gel Viscosity ........... 28 8. Preliminary Study of Effect of Leonardite:Water Ratio on Viscosity ................................... 30 9. Sodium Gel Viscosities................................ 31 10. Calcium Gel Viscosities................................. 40 LIST OF FIGURES Figure Page 1. Viscosity of Leonardite-Water Slurries ................ 19 2. Effect of Viscometer Spindle and Speed on Indicated Viscosity ................................ 24 3. Effect of Temperature on Sodium Gel Viscosity ........ 27 4. Viscosity of Sodium G e l s .............................. 34 5. Viscosity of Calcium G e l s ............................ 41 vii ABSTRACT Leonardite has been considered as a substitute for bentonite as an iron ore pellet binder since it would impart less undesirable impu­ rities to the iron ore. In the case of leonardite, pellet binding strength is believed to be derived from the formation of leonardite- water gel systems. In this respect, the gels formed by addition of sodium hydroxide ("sodium gels") or sodium hydroxide and calcium hy­ droxide ("calcium gels") to leonardite-water slurries are of interest. Procedures were developed giving reproducible results in the preparation and study of these gel systems. The effects of variable composition, temperature, time and order of reagent addition on gel viscosity was determined. Viscosities, as measured by a Brookfield Viscometer ranged from 10 to greater than 8,000,000 cp. for both systems studied. Maximum sodium gel viscosities were achieved at sodium hydroxide:leonardite ratios between 0.08 and 0.12. Increased leonardite:water ratios resulted in increased viscosities. Calcium gels had high viscosities over a broader range of compositions and at lower leonardite:water ratios. Both gel systems studied were non-Newtonian, thixotropic and became more viscous at lowered temperatures. The gelling phenomena in both systems were attributed to the formation of a lattice network of humic acid molecules linked by divalent calcium ions. viii CHAPTER I INTRODUCTION Leonardite is a naturally oxidized lignite occurring in virtually all lignite outcrops in North Dakota. It was named after Professor A. G. Leonard, former head of the Geology Department at the University of North Dakota, who did much of the early study on this mineral (1). Humic acid is the principal organic constituent and imparts gelling properties to leonardite. Due to its abundance, low cost and gelling properties, leonardite has been studied as an iron ore pellet binder since 1955. The binder used commercially is bentonite clay, consisting mainly of alumina and silica which are undesirable impurities in the iron ore. Since the cost of the two materials is comparable, the essentially organic leonardite would be preferable to bentonite if equal pellet strength could be attained and a suitable process developed. It has been estimated that by 1975 approximately 7,000,000 tons of leonardite per year would be required if leonardite replaced bentonite as a binder (2). Experimentation has shown that satisfactory pellets can be manufactured using leonardite (3, £). However, in most testing, there has been an indication that leonardite bound pellets are inferior in green or wet strength (3, 4, 5). Green or newly formed pellets must be strong to avoid deformation during handling and transportation. 1 2 Work by Professor A. M. Cooley at the University of North Dakota indi­ cated that there is a correlation between the viscosity of a binder and the green pellet strength (4). This focused attention on the study of leonardite gel systems. Preliminary work by Adams (6) showed that the composition of a leonardite gel can greatly affect its properties. This work involved the addition of leonardite to calcium oxide and sodium hydroxide in water. The most successful leonardite pelletizing experiments involved a gel system of leonardite and sodium hydroxide to which calcium hydrox­ ide and water were added. The research reported here was undertaken to expand the knowledge of this gel system in a fourfold manner. First, an experimental procedure giving a high degree of reproducibility in the preparation and testing of leonardite gels was established. Second, the rheological properties of the underlying leonardite, sodium hydrox­ ide and water gel system were defined. Third, the effect of adding calcium hydroxide to the sodium gel system was determined. Finally, the observed phenomena was explained in terms of chemical reactions. The main experimental results show the effects of variable composition, order of reagent addition, time, temperature and visco­ meter parameters on gel viscosities. Further results show the degree of reproducibility attainable in the gel formation and testing using a carefully controlled procedure. The range of material variation studied per 100 ml. water was 5 to 50 grams of leonardite, 0 to 20 grams NaOH and 0 to 28 grams CaCOH^. Temperatures ranged from 25°C. to 45°C. The time of interest in this experimentation was the time from mixing to cal­ cination of a green pellet in a commercial process, approximately 15 minutes. 3 However, some experimentation on gel behavior
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