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Characterization of Coal Solvent Extraction Processes Using Petrographic, Chemical, and Physical Methods FINAL REPORT Reporting

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Characterization of Coal Solvent Extraction Processes Using Petrographic, Chemical, and Physical Methods FINAL REPORT Reporting 648 Characterization of Coal Solvent Extraction Processes Using Petrographic, Chemical, and Physical Methods FINAL REPORT Reporting Period March 1, 2003 to February 29, 2004 Report Prepared by Peter G. Stansberry Department of Chemical Engineering College of Engineering and Mineral Resources P. O. Box 6102 West Virginia University Morgantown, WV 26506-6102 Report Issued April 15, 2004 DOE Award Number DE-FC26-98FT40350 Other Contributors Kevin DeVanney & Ralph J. Gray Coal Tech Petrographic Associates 3100 Braun Avenue Murrysville, PA 15668 649 DISCLAIMER This report was prepared as an account of work sponsored by an agency of the United States Government. Neither the United States Government nor any agency thereof, nor any of their employees, makes any warranty, expressed or implied, or assumes any legal liability or responsibility for the accuracy, completeness, or usefulness of any information, apparatus, product, or process disclosed, or represents that its use would not infringe privately owned rights. Reference herein to any specific commercial product process, or service by trade name, trademark, manufacturer, or otherwise does not necessarily constitute or imply its endorsement, recommendation, or favoring by the United States Government or any agency thereof. The views and opinions of authors expressed herein do not necessarily state or reflect those of the United States Government or any agency thereof. ii 650 ASTRACT Nine bituminous coals were selected based on petrographic composition for solvent extraction in N-methyl pyrrolidone (NMP). The lowest rank coal had a vitrinite reflectance of 0.53 and the highest rank coal 1.53. All of the coals underwent laboratory extraction to determine which petrographic features were most amenable to solvent processing. In addition to detailed petrographic analyses of the feed coals, the NMP- insoluble residues and NMP-soluble extracts were also examined by a wide range of chemical and physical characterization methods. It was found that the liptinite and inertinite macerals and mineral matter were not significantly affected nor solubilized by the solvent. Vitrinite had the largest influence on yield and quality of the extract. Solvent etching of polished coal surfaces with NMP proved informative on describing the nature by which NMP attacks the organic coal portion. A combination of conventional test methods can be used to identify candidate coals. Coals most suitable to NMP extraction should be comprised predominantly of vitrinite with a mean maximum reflectance of about 1.1, should exhibit extensive Gieseler plasticity and Audibert-Arnu dilatometry, and should produce high free-swelling index buttons. Not only did the analysis show that rank parameters were important in establishing yields but also were influential in determining the optical microtexture of the cokes following simulated carbonization in the free-swelling index test: low rank bituminous coal extracts produced more isotropic cokes than extracts from high rank bituminous coals. Based on selection criteria developed in this project, a bituminous coal was chosen and successfully processed through the WVU coal extraction pilot plant. iii 651 TABLE OF CONTENTS Page DISCLAIMER ……………………………………………… ii ABSTRACT ……………………………………………………… iii TABLE OF CONTENTS ……………………………………… iv LIST OF FIGURES ……………………………………………… v LIST OF TABLES ……………………………………………… vi 1 EXECUTIVE SUMMARY ……………………………… 1 2 INTRODUCTION ……………………………………………… 3 3 BACKGROUND ……………………………………………… 4 3.1 Coal Formation Primer ……………………………… 4 3.2 Action of Solvents on Coal ……………………… 8 3.3 Role of Extracts on Thermoplastic Properties ……… 10 3.4 Optical Microscopy as Applied to Coal, Coal Products, and Coke/Carbon Forms ……………………… 12 4 EXPERIMENTAL ……………………………………………… 18 4.1 Feed Coal Characterization and Solvent Processing …. 18 4.1.1 Coal Selection, Preparation, and Characterization ……………………………… 18 4.1.2 Coal Extraction in NMP (n-methyl pyrrolidone) ……………………… 21 4.1.3 Determination of Plastic Properties and Proximate Analysis ………………………. 21 4.2 Analyses of Feed Coals, Residues, and Extracts ………. 23 4.2.1 Physical and Chemical Characterization of Feed Coals, Residues, and Extracts ………. 23 4.2.3 Physical and Chemical Characterization of Feed Coals, Residues, and Extracts ………. 23 5 RESULTS AND DISCUSSION ………………………………. 24 5.1 Results of NMP Extraction ………………………. 24 5.2 Correlation of Coal Characteristics with Solvent Extraction Performance ………………………. 27 5.3 Optical Microscopy of Coal and Solvent Extracted Products: Observations and Comments ………………. 34 iv 652 TABLE OF CONTENTS (Continued) Page 5.3.1 Petrographic Analysis of Feed Coals and Insoluble Residues ………………………. 37 5.3.2 Coal Types and Non-Maceral Microstructures ….. 41 5.3.3 Coal Etching in NMP ………………………….. 41 5.3.4 Microscopic Properties of NMP-Soluble Extracts …………………………………………. 47 5.3.5 Microstructures in NMP-Insoluble Residues …... 47 5.3.6 Reflectance Characteristics of Coal, Extract, Residue, FSI Coke …………………………………. 49 5.3.7 Petrographic Analysis of FSI Coke from Coal, Extract, Residue …………………………………. 52 5.4 Results of WVU Coal Extraction Pilot Plant Runs …. 56 6 CONCLUSIONS …………………………………………………. 58 7 REFERENCES …………………………………………………. 58 APPENDIX 1 Feed Coals Basic Analyses ………………….. 62 APPENDIX 2 Surface and Bulk Properties Feed Coals and Residues ………………………………….. 63 APPENDIX 3 Feed Coals Thermoplastic Properties ………….. 64 APPENDIX 4 Thermoplastic Properties Feed Coals, Extract, and Residue ………………………….. 65 APPENDIX 5 FTIR Feed Coal, Residue, and Extract ………… 66 APPENDIX 6 Maceral Analysis Feed Coal ………………….. 67 APPENDIX 7 Maceral Analysis Insoluble Residue ………….. 68 APPENDIX 8 Vitrinoid Types Feed Coal ………………….. 69 APPENDIX 9 Vitrinoid Types Soluble Extract ………….. 70 APPENDIX 10 Vitrinoid Types Residue ………………….. 71 APPENDIX 11 Non-Maceral Microstructures Feed Coal ….. 72 APPENDIX 12 Coke Petrography Feed Coal ………………….. 73 APPENDIX 13 Coke Petrography Soluble Extract ………….. 74 APPENDIX 14 Maceral Analysis Weight% Feed Coal ….. 75 APPENDIX 15 Maceral Analysis Weight% Residue ….. 76 APPENDIX 16 Elemental Analysis Feed Coal, Extracts, And Residue ………………………………….. 77 v 653 LIST OF FIGURES Page Figure 1 Photomicrographs of main maceral groups in a bituminous coal ………………………………… 7 Figure 2 Yield of pyridine extracts vs. coal rank ………… 11 Figure 3 Variation of extract yield and Gieseler fluidity … 12 Figure 4 Reflectance of macerals vs. rank ………………… 15 Figure 5 Two examples of coal coke microstructure ………… 18 Figure 6 Coal preparation and testing outline steps ………… 19 Figure 7 Effect of coal rank on NMP extraction efficiency … 26 Figure 8 Reflectance (rank) vs. maximum Gieseler plasticity … 28 Figure 9 Reflectance (rank) vs. Gieseler plastic range ………… 28 Figure 10 Volatile matter vs. maximum Gieseler plasticity … 29 Figure 11 H/C atomic ratio of feed coals vs. maximum Gieseler plasticity ………………………………… 29 Figure 12 NMP extract yield vs. maximum Gieseler plasticity …. 30 Figure 13 FTIR spectra of Kingwood coal, extract, and residue … 31 Figure 14 Atomic C/H ratio vs. Har/Hal ratio of feed coals ……. 31 Figure 15 Reflectance vs. Har/Hal ratio of feed coals …………. 32 Figure 16 TGA analysis of feed coal, extract, and residue ….. 33 Figure 17 Features of maceral components in bituminous coal ….. 36 Figure 18 Estimated vitrinite content in insoluble residues ….. 39 Figure 19 Optical microscopy of NMP-etched coal ………….. 44 Figure 20 Optical microscopy of NMP-etched coal ………….. 45 vi 654 LIST OF FIGURES (Continued) Page Figure 21 Optical microscopy of NMP-etched coal ………….. 46 Figure 22 Insoluble residue from NMP extraction. ………….. 48 Figure 23 Photomicrographs of FSI cokes from feed coals ….. 53 Figure 24 Photomicrographs of FSI cokes from insoluble residues .. 54 Figure 25 Photomicrographs of FSI cokes from extracts …… 55 Figure 26 Flow diagram of the WVU coal extraction pilot plant….. 57 vii 655 LIST OF TABLES Page Table 1 Coal classification according to ASTM ………….. 8 Table 2 Maceral groups and macerals in hard coals ………….. 14 Table 3 A system of coke microscopy ………………….. 17 Table 4 Characteristics of bituminous coals ………………….. 20 Table 5 NMP-extraction of laboratory washed coals ………….. 25 Table 6 Yield of NMP-soluble extracts from bituminous coals .. 26 Table 7 Petrographic maceral and mineral classification …... 35 Table 8 Summary of petrographic analysis of coal and insoluble residue ………………………………….. 38 Table 9 Classification of non-maceral microstructures ….. 40 Table 10 Microscopic properties of NMP-soluble extracts …... 47 Table 11 Microstructures in NMP-insoluble residues …………… 49 Table 12 Reflectance of indicated samples in the order of increasing rank. …………………………………… 51 Table 13 Summary petrographic analysis of FSI coke from coal, extract, and residue …………………… 56 viii 656 1 EXECUTIVE SUMMARY The objective of the current proposal was to determine what petrographic, physical, and chemical characteristics of bituminous coals lead to the production of maximum extraction yield in N-methyl pyrrolidone (NMP). Detailed analyses of the feed coals and the examination of the coal maceral components that were solubilized by NMP were of great importance in establishing criteria for the selection of candidate coals. Normally petrographic data are determined on a volume percent basis by microscopic point techniques. Conversion of these data to a weight percent basis was made for comparison with the extract and residue weights. The characterization of extract quality and quantity as well as the coke textures and structures produced from carbonization
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