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The Cool Flame Combustion of the Isomeric Hexanes

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The Cool Flame Combustion of the Isomeric Hexanes THE COOL FLAME COMBUSTION OF THE ISOMERIC HEXANES DISSERTATION Presented in Partial Fulfillment of the Requirements for the Degree Doctor of Philosophy in the Graduate School of the Ohio State University By PAUL ELLSWORTH OBERDORFER, JR., B. SC. The Ohio State University 1954 Approved by: Adviser 1 ACKNOWLEDGMENT The author is deeply grateful to Professor Cecil B. Boord whose vision made this work possible. His enthusiasm and guidance have been inspirational and of invaluable assistance to the author. The pursuance of this investigation was made financially possible by the Ohio State University Research Foundation Projects 455 and 572 under terms of contract with the U.S.A.F, Air Research and Development Command, Baltimore, Maryland, Appreciation is also extended to Dr. Kenneth W. Greenlee and the other members of the project staff for their generous assistance and advice. 11 TABLE CP CONTENTS Pag# SUMMARY AND CONCLUSIONS................................ 1 INTRODUCTION AND REVIEW CP LITERATURE.................. 4 OBJECTIVES GF THIS W O R K ................................ 24 Statement of Objectives 25 Discussion of Objectives *••••....••............... 25 EXPERIMENTAL DETAILS ................................... 32 Description of Apparatus ...••••••...................... 33 Flow Tube ...» 33 Furnace ....................*......... 33 Fuel Feed System 36 Behavior of the Cool Flame ....... 38 Analytical Procedures .................. 42 Experimental Results with the Isomeric Hexanes *.... 53 n-Hexane .................. 53 2-Kethylpentane 61 3-Methylpentane 70 2.2-Dimethylbutane .... 74 2 .3 -Dimethylbutane ................... * 80 DISCUSSION OF RESULTS......... 82 REFERENCES ..................................... 123 AUTOBIOGRAPHY.......................................... 127 lit INDEX TO TABLES Table Page 1 Flame Positions at Various Tube Temperatures for n—Hexane Combustion ••.•.•••••••••••••••••••••••• 54 2 Flame Temperature Profile for n—Hexane Combustion... 55 3 Gas Analysis for n-Hexane Combustion Products ..... 56 4 Polarographic Analysis for n-Hexane Combustion Products ................ 58 5 Chromatographic Analysis for n-Hexane Combustion Products ....... 60 6 Flame Positions at Various Tube Temperatures far 2-Methylpentane Combustion 62 7 Flame Temperature Profile for 2-Methylpentane Combustion 64 8 Gas Analysis of 2 -Methylpentane Combustion Products •. 65 9 Polarographic Analysis for 2-Methylpentane Combustion Products ..... 63 10 Chromatographic Analysis for 2-Methylpentane Combustion Products ...... 69 11 Flame Positions at Various Temperatures for 3-Methyl- pentane Combustion .................. 70 12 Flame Temperature Profile for 3-Methylpentane Combustion 71 15 Gas Analysis for 3—Methylpentane Combustion Products .... 72 i▼ Table Page 14 Polarographic Analysis for 3“Wethyip«aitane Confcustion Products 73 15 Chromatographic Analysis for 3~**sthylpentane Combustion Products •••••••••••••••••••••••••*•••••• 74 16 Flame Positions at Various Tube Temperatures for 2,2-Eftmet hylbutane Combustion ••..•.•••••••••••••••• 75 17 Flame Temperature Profile for 2,2-Dimethylbutane Combustion ••••••••••••••••............................. 76 18 Gas Analysis for 2,2-Dimethylbutane Combustion Products 77 19 Polaro graphic Analysis for 2,2—BLmethylbutane Combustion Products • 79 20 Chromatographic Analysis for 2,2—Dimethylbutane Combustion Products ••••••••••••••••••..... •••••••• 80 21 Post Cool Flame Carbon Balances 84 22 Temperature Increases at the Same Tube Temperatures. 90 23 Major Ole fin a in the Post Cool Flame Region ••.••••• 100 INDEX TO FIGURES Figure Page 1 Cool Flame Reaction Tube ••••••••••*••••••••••••••••• 34 2 Fuel Feed System ........ 37 3 Standard Polarogram 46 4 Post Cool Flame Sample Polarogram •••»*•••••••••••••• 47 5 Pro Cool Flame Sample Polarogram 46 6 2-Butylhydroperoxide Polarogrsa ••••••••••••••••••••• 49 7 Spectrograms of Post Flame Olefins •••••••••••••••••• 39 8 Cool Flame Temperature Distance Relationships ..... 8 6 9 Cool Flame Temperature Profiles •••••••••«••••••••••• 89 10 Fuel and Oxygen Consumption Patterns •••••••••••••••• 92 U Aldehyde Production Patterns ••••••••••••••••••..... 93 12 Olefin and Carbon Monoxide Production Patterns •••••• 94 13 Alkyl and Hydrogen Peroxide Production Patterns •. • • • 96 14 Fuel Characteristics vs. Cool Flame Combustion Characteristics ....... • 96 SUMMARY AND CONCLUSIONS 2 1. The utilization of a flow system in which a stabilized cool flame is produced in a straight tube under reproducible conditions is very useful for the Investigation of the chendcal nature of the early vapor phase combustion processes. 2 . Four of the five Isomeric hexanes were found to undergo the cool flame reaction. Stable cool flames were produced in each case. 2 , 3 “dimethyTbutane would not react within the temperature limits of the apparatus used in this investigation. Seme of the physical aspects of the cool flame phenomena were investigated* 3* Chemical reaction products were determined at various stages of the combustion process for each of the hexanes burned. Up to 8696 of the carbon-containing products of reaction were accounted for* 4. Formaldehyde, higher aldehydes, ketones, carbon monoxide, olefins, hydrogen peroxide and alkyl hydroperoxides were found to be universal products of cool flame combustion. 3 . The amounts of the various chemical products as well as the structure of individual compounds were found to vary with the structure of the fuel which was burned. 6 . As the number of methylene groups of an individual hexane increases the amount of cool flame reaction, as measured by oxygen consumption and moles of products formed, increases. 3 7. As the number of methylene groups of an Individual hexane increases, the temperature required to initiate a cool flame reaction in the same period of time decreases. 8 . As the number of methylene groups of an Individual hexane increases the iwitw flame temperature rise Increases. 9* As the engine performance of an individual hexane Increases the amount of cool flame reaction decreases. 10. As the engine performance of an individual hexane increases the temperature required to Initiate a cool flame reaction in the same period of time Increases. 11. As the engine performance of an individual hexane increases, the maximum flame temperature rise decreases. 12. As the number of methylene groups decreases or the engine performance of an individual hexane increases, the relative amount of olefin and carbonyl products having a greater number of carbon atoms increases while the total amount of smaller olefin and carbonyl products decreases. 13. The experimental results have been correlated with existing concepts of the mechanism of hydrocarbon oxidation. 4 INTRODUCTION AND REVIEW OF LITERATURE 5 Cool flames and luminescence phenomena have been observed and reported in the literature since the advent of modern chemistry itself. Generally speaking these phenomena are associated with the luminous incomplete vapor phase combustion of organic compounds. Luminescence differs from a cool flame in that the cool flame has a more defined shape and appearance with distinct boundaries. With a flame of any type, of course, there is an associated space velocity or rate of propagation. That is, to say, the flame is moving with respect to the gaseous mixture consuming the reactants ahead and forming products behind as it progresses through the mixture. Luminescence involves a less defined region of reaction and is spread out into a larger volume of more diffuse glow. The zone of luminescence also involves the consumption of reactants and formation of products but the boundaries ere not as distinct nor the reaction intensity as great at the boundary. In either phenomenon, the intensity of reaction, that is the temperature rise and amount of reaction, is much less than that associated with "hot" flames such as the Bunsen flame. Generally speaking cool flames involve at most a hundred or so degrees temperature increase while the hot flame temperature increase is of the order of several thousand degrees. The interest in the phenomena of cool flames and luminescence lies in the fact that their occurrence is associated with the early stages of reaction in the combustion process. Consequently, a number of investigations have been made of the cool flame phenomena for the purpose of studying the nature of the combustion or oxidation process* One of the earliest investigations of the phenomena of cool flames and luminescence was conducted by the great chemist W* H. Perkin in 1882 (l). According to Perkin the observation of lum­ inescence dates back to the time of Sir Humphrey Davy who observed that a hot spiral of platinum wire inserted into a mixture of ether and air caused a pale phosphorescent light to appear above the wire. In Perkin's investigation of the phenomena several technics were employed to produce the luminous reactions. One of the simplest was to project ether from a wash bottle onto a hot iron plate in a darkened room whereupon a considerable mass of blue flame appeared. Reportedly the blue flame would appear at temperatures between 260* and a dull red heat. At higher tempera­ tures normal ignition occurred. By boiling ether at one end of a heated glass tube, Perkin was able to momentarily isolate a cool flame. He states that the flame had a low temperature and that the fingers might be placed in it with impunity. By passing air through a bottle of ether and passing the mixture into a heated glass tube he obtained an oscillating cool flame which
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