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Changes in Coal Sulfur During Carbonization

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Changes in Coal Sulfur During Carbonization .A· "" ·w:. ·1 SPECIAL.REPORT OF RESEARCH Conducted in Departmery:.R.f fuel Technology ). College _of' Mineral Industries §c, · c ·; The .Pennsylvania State University ------- :: ~ I CHANGES IN COAL SULFUR DURING CARBONIZATION by RICHARD A. ANDERSON and T. S. POLANSKY An Investigatio~ donducted Under the Auspices of the COAL RESEARCH BOARD of the COMMONWEALTH OF PENNSYLVANIA Special Research Report Number SR-19 August 1, 1960 STATEMENT OF TRANSMITTAL Special Report SR-19 transmitted herewith has been prepared by the Coal Research Section of the Mineral In~ustries Experiment Station. Each of the Special Reports presents the results of a phase of one of the research projects supported by the Pennsylvania Coal Research Board or a technical discussion of related research. It is intended to present all of the important resµlts of the Coal Board research in Special Reports, although some of the results may already have been presented in progress reports. The following is a list of Special Research Reports issued previously. ·SR-1. The Crushing of Anthracite May 31, 1958 SR-2 Petrographic Composition and August 1, 1958 Sulfur Content of a Column of Pittsburgh .Seam Coal SR-3 The Thermal Decrepitation of September 15, 1958 Anthracite SR-4 The Crushing of Anthracite with November 1, 1958 ) a Jaw Crusher SR-5 Reactions of a Bituminous Coal February 1, 1959 with Sulfuric Acid SR-6 Laboratory Studies on the Grind­ April 1, 1959 abili ty of Anthracite and Other Coals SR-7 Coal Characteri.stics and Their April 15, 1959 Relationship to Combustion Techniques SR-8 The Crushing of Anthracite with April 25, 1959 an Impactor-Type Crusher .SR-9 The Igni tibi.1 i ty of Bituminous May 4, 1959 Coal (A Resume' . of a Literature Survey) SR-10 Effect of Gamma Radiation May 6, 1959 and Oxygen at Ambient Tem­ peratures on the Subsequent Plasticity of Bituminous Coals SR-11 Properties and Reactions May 11, 1959 Exhibited by Anthracite Litho­ types Un.der Thermal Stress SR-12 Removal of Mineral Matter from June 22, 1959 Anthracite by Chlorination at High Temperatures .Sll-13 Radiation Stability of a Coal .June 25, 1959 Tar Pitch SR-14 The Effect of Nuclear Reactor July 31, 1959 Irradiation During Low Tem­ perature Carbonization of Bituminous Coals SR-15 Effect of Anthracite and Gamma August 5, 1959 Radiation at Ambient Tempera­ tures on the Subsequent Plas­ ticity of Bituminous Coals SR-16 The Isothermal Kinet'ics of August 25,. 1959 Volatile Matter Relea$e from Anthracite SR-17 The Combustion of Dus.t Clouds: November 30, 1959 A Survey of the Literature SR-18 The Ignitibility of Bituminous June 15, 1960 Coal M. E. Bell, Director M. I. Experiment .Station ------ SUMMATION OF RESULTS The carbonization behavior of sulfur in the coal and its float fraction studied is summarized by the following observatiqns. (1) Pyrite decomposed initially around 350°; decomposition was most extensive between 550° and 650°, and was essentially completed at 700°C, Pyrite decomposition was markedly affected by secondary reactions with volatile matter. (2) Sulfate, present in small quantities in the parent coals, was not found in the cokes prepared above 650°C. (3) Sulfide formation incr~ased with temperature. The amount of sulfide found below 700°C did not correspond with that predicted for reactions in which one mole of ferrous sulfide is formed for each mole of pyrite decomposed. Above 750° the atomic ratio of sul­ fide sulfur to non-pyritic iron was greater than unity, indicating the existence of other inorganic sulfides, such as calcium and mag­ nesium sulfides, and/or a complex iron sulfide. (4) Iron, uncombined with sulfur and resulting from pyrite decomposition, was found in cokes from the whole coal produced at temperatures between 350° and 650°C. The nature of the data does not permit conclusions as to its existence above 650°C in these cokes. The 770°C coke of the float coal contained sulfur­ free iron, (5) The organic sulfur content d~creased during carbonization. About 153 of the original organic sulfur was decomposed and evolved at 366°C. At 650° approximately 50 to 603 of the sulfur in the cokes of the whole coal was in organic form, compared to 36.43 in the coal. Above 650° the percent organic sulfur decreased, being about 113 of the total coke sulfur at 885°C. (6) Elemental sulfur was not detected in cokes prepared below 750°C from the whole coal. Above thQS temperature small quantities of free sulfur were observed qualitatively; the amount apparently increased with temperature. It was not detected in the cokes produced from the float fraction of the whole coal. The investigation of the use of benzoin in conjtlnction with a colorimetric sulfate procedure for the quantitative determination of elemental sulfur was inconclusive. --::JI ABSTRACT Changes in the sulfur forms during carbonization of a High Volatile A rank, high sulfur, Pittsburgh Seam coal were investi­ gated. Possible effects of mineral matter content were investi­ gated by use of a float fraction of the whole coal. The coals were carbonized in a vertical, static bed unit designed to study the effects of primary and secondary reactions of the sulfur forms. Pyrite was completely decomposed at about 700°C and sul­ fate sulfur was not observed abo~e 650°C. Formation of inor­ ganic sulfides, excluding iron sulfide, was noted by the non­ stoichiometric relationship of sulfide sulfur and non-pyritic iron. Iron, uncombined' with sulfur, was observed in cokes carbonized at temperatures between 350° and 650°C. Organic sulfur began to decompose at about 366°C, and it amounted to approximately 113 of the total coke sulfur at 885°C. El­ mental sulfur was qualitatively detected in cokes produced above 700°C by benzoin, and a method for determining it quan­ titatively was investigated. TABLE OF CONTENTS Table of Contents List of Tables List of Figures I. INTRODUCTION Interrelatetl aspects of sulfur in coal and the coke industry 1 Literature review . 2 Statement of the problem................................... 8 Objectives of the investigation 9 II. PROCEDURE OF THE INVESTIGATION Description of coal and preparatiop of samples .•....•.....• 11 Part I Carbonization Studies Description o~ carbonization apparatus ...•...........•..... 12 '/: Preparation of adsorbents for :Volatiles from carbonization . 16 Carbonization ~rocedure ..•......•.....••.....•............. 16 Analytical procedures . 17 Part II Quantitative Estimation Of Free Sulfur Preparation of cokes for the addition of elemental sulfur,. 19 Apparatus for conversibn of elemental sulfur to sulfate •••. 20 Apparatus for sulfate determination •.•...•..••....••.••.•.. 20 Experimental procedure ..................................... 20 I I I • EXPERIMENTAL RESULTS Part I Effect of rapid removal of volatile matter on sulfur fo-rm distribution . • . 27 Effect of temperature on the forms of sulfur during carbonization • $ •••••••••••••••••••••••••••••••••••••••••••• 36 Occurrence of elemental sulfur ............................ 42 Carbonization of the float coal 43 Analysis of adsorbent materials •••••• 0 ••••••• 0 ••••••••••••• 44 -----::: Part II Qualitative test for free sulfur with benzoin 46 Quantitative determination of pure sulfur . ··· .......... 48 Comparison of colorimetric and gravimetric methods for sulfate determination 49 Determination of total sulfur added to cokes using the Eschka method . 50 Application of the sulfur to sulfate conversion and colorimetric determination to cokes with added sulfur ... 50 Extraction of elemental sulfur with carbon disulfide .... 52 IV. DISCUSSION OF RESULTS Part I Decomposition of organic coal sulfur ................... 54 Decomposition of pyrite . .. 55 Formation of organic, sulfide, and elemental sulfur ..... 57 Part I! Quantitative estimation of elemental sulfur ............. 67 V. SUMMARY AND CONCLUSIONS Naure of the investigation ............................. 67 Procedure of the investigation ......................... 67 Results of the investigation . 69 Conclusions . 70 Suggestions for future research ........................ 72 BIBLIOGRAPHY · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · .. · · · · · · · · · · · · · 75 APPENDIX I Carbonizer operational data'""' ................... 78 Il Modified Mott method of sulfur form analysis ..... 79 III Colorimetric sulfate determination., ............. 81 IV Determination of elemental sulfur in carbonized samples ....... 0 ......... 0 0 ....................... 82 ij ...... List of Tables Page 1. Proximate Analysis and Total Sulfur of Coal Samples 12 2. Total Sulfur, Moisture, and Ash Analyses of Cokes for the 19 Addition of Elemental Sulfur 3. Methods of Sulfur Addition and Amount of Sulfur Added to 25 Cokes · 4. Conditions Qf Benzoin Reaction Tests on Sulfurized Cokes 26 5. Proximate Analysis of Coals and Cokes and Coke Yields 28 6. Analysis of Sulfur and Iron Forms in Coals and Carbonized 30 Samples, Percent on Dry Basis 7. Distribution of Sulfur in Coals and Cokes, Percent of 31 Total Sulfur 8. Analysis of Total Sulfur and Sulfur and Iron Forms of 34 Coals and Cokes, Whole Coal Basis 9. Theoretical Amount of Iron Uncombined with Sulfur in 41 Coals and Cokes 10. Proximate Analysis of Whole and Float Coals and Cokes, 44 and Coke Yields 11. Sulfur and Iron Analysis of Whole and Float Coals and 45 Cokes 12. Total Sulfur and Volatile .Matter Analysis of Adsorbent 46 Materials 13. Results of Qualitative Test for Free Sulfur in Various 47 Coals and Cokes 14. Conditions and Results of Tests on the Quantitative Deter- 48 mination of Pure Elemental Sulfur
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