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Views on Coal Liquefaction, Used As a Basis for This Survey Are: M L~OLVENT REFINED COAL AND COAL-OIL MIXTURES/ A Thesis presented to The Faculty of the College of Engineering and Technology Ohio University In Partial Fulfillment of the Requirements for the Degree Master of Science by Avant! E-mbalia; June 13, 1981 ACKNOWLEDGEMENTS The author wishes to thank his advisor, Professor Robert L. Savage, for his advice and guidance in bringing this work to a successful com­ pletion. The author wishes to thank the Pittsburgh Midway Coal Mining Company of Dupont, Washington for supplying SRCI and SRCII samples. Finally, the author also wishes to thank Louella Rich and Diana Miller at the Word Processing Center of The Standard Oil Co, Cleveland, Ohio, for the typing of this thesis. TABLE OF CONTENTS PAGE INTRODUCTION 1 COAL-OIL MIXTURES 6 Coal-Oil Mixture Technology 6 Stability of Coal-Oil Mixture 7 Testing Procedures Used for Stability Study 8 Density of Coal-Oil Mixture 11 COAL LIQUEFACTION 12 Relations of Coal and Solvent for Extraction 13 Variables Important for Extraction 17 SRC Technology 19 OBJECTIVES 23 EQUIPMENT AND EXPERIMENTAL PROCEDURE 25 Stability Study 25 Viscosity -and Density Measurements of Coal-Oil Mixtures 38 Coal-Oil Mixture Sample Preparation 41 Preparation of Low-Ash Coal 43 Apparatus 47 RESULTS AND DISCUSSION 50 Stability Studies 50 TABLE OF CONTENTS (Cont'd) PAGE Coal Concentration with Height 72 Tuned Circuit Detector 90 Viscosity of Coal-Oil Mixtures 104 Density of Coal-Oil Mixtures 117 Low-Ash Coal 121 CONCLUSIONS 130 RECOMMENDATIONS 132 REFERENCES 134 Appendix A- Derivation of the formula used for the A1-A4 pendulum Appendix B- Procedure used for the percent solids BI-B2 determinations in coal-oil mixtures Appendix C- Proximate, ultimate, sulfur and ash analysis CI-C2 for the coal used Appendix D- Settling data DI-D9 Appendix E- Data for a metal detector EI-EIO Appendix F- Viscosity data for COM F1-F8 Appendix G- Viscosity data for SOM GI-G5 Thesis Abstract LIST OF FIGURES FIGURE PAGE 1 Pendulum Apparatus used in Determining Settling in Coal-Oil Mixtures 26 lA Sketch of Pendulum Apparatus 27 2 The Arrangement used for Fixing Settling Tube inside the Carriage 28 3 Settling Tube with Block inserted at the Carriage Bottom and Timer Contacts 28 4 Sketch of Coal-Oil Mixture Column 33 5 A Metal Detector used for Stability Study 36 6 Circuit for a Metal Detector 37 7 Dissolver for Preparation of Low-Ash Coal 44 8 Size Distribution for No. 8 Coal 53 9 Size Distribution for Solvent Refined Coal 55 10 Stability of Suspensions: Curves showing the Relationship between C.G. drop and Time 60 11 Pendulum Error Analysis: Thread Number vs. Time Period 68 12 Pendulum Error Analysis: Thread Number vs. Deviation in Time Period 68 LIST OF FIGURES (Cont'd) FIGURE PAGE 13 Pendulum Error Analysis: Thread Number vs.~T/~T 71 14 Coal Concentration versus Height 76 15 Coal Particles at Top of Tube, 1 day after the Mixture Preparation 78 16 Coal Particles at Bottom of Tube, 1 day after the Mixture Preparation 78 17 Coal Particles at Top of Tube, 24 days after the Mixture Preparation 79 18 Coal Particles at Bottom of Tube, 24 days after the Mixture Preparation 79 19 Relationship between C.G. drop and Coal Content 81 20 Coal Particles at Top of Tube, 12 days after the Mixture Preparation 86 21 Coal Particles at Bottom of Tube, 12 days after the Mixture Preparation 86 22 Coal Particles at Top of Tube 32 days after the Mixture Preparation 89 23 Coal Particles at Bottom of Tube, 32 days after the Mixture Preparation 89 LIST OF FIGURES (Cont'd) FIGURE PAGE 24 Curves for an Original Circuit 91 25 Curve for NO. 6 oil at 25°C. 93 26 Curve for 40% COM, after 1 hour 94 27 Curve for 40% COM, after 8 hours 95 28 Curve for 40% COM, after 2 days 96 29 Curve for Glycerine, liquid level I" above the top coil 99 30 Curve for Glycerine, liquid level 4" above the top coil 100 31 Curve for a Viscosity Standard 102 32 Viscosity versus Percentage Coal 112 33 Log-log plot of Apparent Viscosity versus Spindle Speed 113 34 Thixtropy: Dial readings versus Spindle Speed for Coal-Oil Mixtures 116 35 Variations in Density of Coal-Oil Mixtures 120 LIST OF TABLES TABLE PAGE 1. Extraction of Bituminous Coal by Aromatic Compounds 15 2. Dry Sieve Analysis for No. 8 Coal 51 3. Dry Sieve Analysis for solid Solvent Refined Coal 52 4. Coal-Oil Mixture Compositions used for Stability Studies 56 5. Settling Data for COM 57 6. Settling Data for SOM and Low-ash coal-oil mixtures 58 7. Pendulum Reproducibility Data (Standard tube) 64 8. Pendulum Reproducibility Data (Tube with No. 6 Oil) 65 9. Error Analysis for the Pendulum (data) 67 10. Error Analysis for the Pendulum 70 11. Variation in Coal Concentration with Height 74 12. Variation in Coal Concentration with Height 85 13. Variation in Coal-Oil Mixtures Viscosity with the Coal Content 111 14. Thixotropic Behavior of Coal-Oil Mixtures 115 15. Density of Coal, Oil and Coal-Oil Mixtures 118 16. Preparation of Low-ash Coal (using phenanthrene) 122 17. Preparation of Low-ash Coal 127 INTRODUCTION World demand for energy is increasing at a dramatic rate, and this trend is unlikely to change in the foreseeable future. Because a combination of economic, technological and ecological pressures are preventing atomic energy from meeting any significant portion of the demand, the major energy sources continue to be oil, coal and natural gas. Projected limitations on supplies of domestic oil and natural gas, and the need to reverse the country's increasing reliance on foreign petroleum sources, are stimulating consideration of America's vast coal deposits as a way of satisfying more of the nation's energy requirements. Several technologies to convert coal to various synthetic fuels are being developed in the United States, some with support from the U.S. Department of Energy. Commercial coal-gasification and demon­ stration coal-liquefaction plants are proposed(l). Many existing gas and oil fired electric power plants are designated candidates for coal-boiler conversion in accordance with power plant and Industrial Fuel Act of 1978. Substantial economic incentives exist to convert coal to liquid and gaseous fuels, since most energy using devices require such fuels. Coal Liquefaction The term "liquefaction of coal" refers to any method (other than carbonization of coal for coke) by which all or part of the coal is 2 converted to liquid form. The advantage of coal liquefaction, over other coal conversion processes is that the entire range of liquid products, including fuel oil, gasoline, jet fuel and diesel oil, can be produced from coal by varying types of catalyst and operating conditions. Furthermore, coal-derived liquid fuels have potential for use as a chemical feed stocks (2). The u.s. Department of Energy program for the conversion of coal to liquid fuels was started by its predecessor agencies: Energy Research and Development Administration (ERDA), Office of Coal Research (OCR) in 1962, and Bureau of Mines, U.S. Department of the Interior, in the 1930's (2). Techniques for converting coal to synthetic liquid fuel, originally developed in Germany in the early 1930' s , are being improved to increase the supply of non-polluting liquid fuel to produce a more easily transportable and usuable fuel. Current emphasis is on the development of fuels suitable for firing industrial and electric utility boilers and gas turbines. Some of the coal liquid production processes are: Consolidation Coal Company CSF process, PAMeO Solvent-Refined Coal, H-Coal process, Char-Oil Energy Development (COED) process, Seacoke process by Atlantic Richfield Company and Bureau of Mines Synthoil process. These processes are currently in different stages of development. Solvent Refined Coal The PAMCO solvent refined coal process was developed by the Pittsburgh and Midway Coal Mining company (formerly Spencer Chemical 3 Company). The primary objective of the process is to produce a low-ash low-sulfur fuel which can be fed to a boiler in either solid or liquid form. Solvent Refined Coal (SRC) meets any existing and proposed EPA regulations and it can be considered as an attractive potential fuel. Two major government funded projects are in progress for the development of Solvent Refined Coal. At present SRC is produced by two different methods known as SRC I and SRC II (4,5). In short, SRC I involves solution of most of the coal in a donor solvent derived from the process, separating the undissolved solids by filtration, distilling of the original process solvent and recovering the dissolved coal as a solid material known as SRC I. SRC II is an advanced coal-liquefaction process, in which coal is mixed with the portion of the product slurry and hydrocracked to liquid and gaseous products. The dissolved coal unconverted to distillate fuel and lighter product is sent to a gasifier, together wi th the undissolved mineral residue, to produce hydrogen for the process. Thus, a solid liquid separation step is not required and the primary product from SRC II process is distillate fuel oil. The present work includes a laboratory investigation of some alternate method--other than conventional SRC process, for the preparation of a low-ash coal. Motivation for the problem came from (1) the project "A Study of the Potential Use of Solvent Refined Coal in Ohio" at Ohio University, sponsored by Ohio Air Quality Development Authority and (2) a Bituminous Coal Research, Inc. report on the 4 preparation of low-ash coal by solvent extraction based on research conducted for North American Coal Corporation in 1959.
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