Measurement of gas evolution from PUNB bonded sand as a function of temperature

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1 University of Iowa Iowa Research Online Theses and Dissertations Suer 211 Measureent of gas evolution fro PUNB bonded sand as a function of teperature Gregory Jaes Sauels University of Iowa Copyright 211 Gregory Jaes Sauels This thesis is available at Iowa Research Online: Recoended Citation Sauels, Gregory Jaes. "Measureent of gas evolution fro PUNB bonded sand as a function of teperature." MS (Master of Science) thesis, University of Iowa, Follow this and additional works at: Part of the Mechanical Engineering Coons

2 MEASUREMENT OF GAS EVOLUTION FROM PUNB BONDED SAND AS A FUNCTION OF TEMPERATURE by Gregory Jaes Sauels A thesis subitted in partial fulfillent of the requireents for the Master of Science degree in Mechanical Engineering in the Graduate College of The University of Iowa July 211 Thesis Supervisor: Professor Christoph Beckerann

3 Graduate College The University of Iowa Iowa City, Iowa CERTIFICATE OF APPROVAL MASTER'S THESIS This is to certify that the Master's thesis of Gregory Jaes Sauels has been approved by the Exaining Coittee for the thesis requireent for the Master of Science degree in Mechanical Engineering at the July 211 graduation. Thesis Coittee: Christoph Beckerann, Thesis Supervisor Pablo Carrica Albert Ratner

4 ACKNOWLEDGEMENTS This work would not have been possible without the support of any people. I would like to express y gratitude to y advisor, Professor Christoph Beckerann, for his treendous support, guidance, and unwavering insistence that I hold yself to the highest possible standards. I would like to thank the ebers of y thesis coittee, Professors Pablo Carrica and Albert Ratner, for their advice and input. I want to extend thanks to the ebers of the Solidification Laboratory, especially Kent Carlson, Richard Hardin, and Daniel Galles, for their support and encourageent. I would like thank Peter Hatch of the University of Iowa Departent of Cheistry for his advice and expertise in the design and construction of y quartz coponents. I want to thank Professors Allan Guyon and Gary Aurand of the University of Iowa Departent of Cheical and Biocheical Engineering for their insight and generosity in allowing e to use their lab equipent. I extend thanks to Professor Scott Giese of the University of Northern Iowa Departent of Industrial Technology for providing additional experiental support. I also thank Jerry Thiel and the students at the University of Northern Iowa Metal Casting Center for their assistance with specien production. Finally, special thanks are extended to y friends and faily, especially y parents David and Joanne and y wife Lindsay, for all their love, support, and understanding during this challenging process. ii

5 ABSTRACT The cheical binders used to ake sand olds and cores therally decopose and release gas when subjected to the high teperature conditions in sand casting processes. Coputational odels that predict the evolution of the binder gas are being introduced into casting siulations in order to better predict and eliinate gas defects in etal castings. These odels require knowledge of the evolved binder gas ass and olecular weight as a function of teperature, but available gas evolution data are liited. In the present study, the ass and olecular weight of gas evolved fro PUNB bonded sand are easured as a function of teperature for use with binder gas odels. Therogravietric analysis of bonded sand is eployed to easure the binder gas ass evolution as a function of teperature for heating rates experienced in olds and cores during casting. The volue and pressure of gas evolved fro bonded sand are easured as a function of teperature in a specially designed quartz anoeter during heating and cooling in a furnace. The results fro these experients are cobined with the ideal gas law to deterine the binder gas olecular weight as a function of teperature. Therogravietric analysis reveals that the PUNB binder significantly decoposes when heated to elevated teperatures, and the PUNB binder gas ass evolution is not strongly influenced by heating rate. During heating of PUNB bonded sand at a rate of 2 C/in, the binder gas olecular weight rapidly decreases fro 375 g/ol at 115 C to 99.8 g/ol at 2 C. The olecular weight is relatively constant until 27 C, after which it decreases to 47.7 g/ol at 55 C. The olecular weight then steeply decreases to 3.3 g/ol at 585 C and then steeply increases to 47.2 g/ol at 63 C, where it reains constant until 75 C. Above 75 C, the binder gas olecular weight gradually decreases to 33.3 g/ol at 898 C. The present easureents are consistent with the olecular weights calculated using the binder gas coposition data fro previous studies. The binder gas is coposed of incondensable gases above 79 C, and the binder gas partially condenses during cooling at 165 C if the bonded sand is previously heated below 57 C. iii

6 TABLE OF CONTENTS LIST OF TABLES... vi LIST OF FIGURES... vii LIST OF NOMENCLATURE...x CHAPTER 1. INTRODUCTION Background and Motivation Objective of Present Study LITERATURE REVIEW Phenolic Urethane Binder Systes Binder Gas Molecular Weight Data Gas Evolution Tests EXPERIMENTAL METHODS Experiental Approach of Present Study Preparation of Speciens Therogravietric Analysis Gas Measureent Apparatus Metal-Only Expansion Tests Pure Gas Expansion Tests Binder Gas Evolution Tests RESULTS AND DISCUSSION Therogravietric Analysis Preliinary TGA Measureents Bonded Sand Decoposition Measureents Pure Binder Decoposition Measureents Coparison of Bonded Sand and Pure Binder Decoposition Measureents Metal-Only Expansion Measureents during Heating Pure Gas Expansion Measureents during Heating Binder Gas Measureents Binder Gas Evolution during Heating and Cooling Effects of Hydrogen Dissolution on the Binder Gas Molecular Weight Measureents Effects of Sand Expansion on the Binder Gas Molecular Weight Measureents Additional Analysis of the Measured Peak in the Binder Gas Molecular Weight during Heating Molar Evolution of the Binder Gas during Heating and Cooling Coparison of the Present Molecular Weight Measureents with the Results fro Previous Studies...58 iv

7 5. CONCLUSIONS...86 REFERENCES...88 v

8 LIST OF TABLES Table 1. Tie-averaged ass fraction and ixture olecular weight of gas coponents evolved fro PUCB and PUNB bonded sand within 2 inutes after pouring during the experients of Bates et al. and Scott et al Priary cheical coponents identified by McKinley et al. and Lytle through GC-MS analysis during 2 seconds of pyrolysis of 1.5% PUCB bonded sand and the calculated gas ixture olecular weights Cheical coponents identified by Wang et al. through GC-FID and GC- TCD analysis during TGA pyrolysis of 1.5% PUCB bonded sand at a heating rate of 1 C/in and the calculated gas ixture olecular weight Piecewise polynoial fitted to the easureents of the fraction of original binder ass reaining in bonded sand saples during TGA pyrolysis at a heating rate of 2 C/in with a total argon flow rate of 25 c 3 /in Priary sources of error in the binder gas olecular weight easureents Piecewise polynoial fitted to the binder gas olecular weight easureents obtained during heating of PUNB bonded sand saples at a rate of 2 C/in...85 vi

9 LIST OF FIGURES Figure 1. General bonding reaction equation for PUCB or PUNB binder systes Experiental technique used by Bates and Monroe to saple the gas evolved fro decoposition of bonded sand during pouring of etal castings Gas evolution tester eployed by Zhang et al Experiental ethods eployed by Bates and Monroe to easure the (a) volue and (b) pressure of gas evolved fro bonded sand Techniques for easuring binder gas evolution fro cores iersed in olten etal Scheatic of gas easureent apparatus and iportant geoetric quantities Procedure for filling GED with only liquid etal Procedure for filling GED with a gas saple and liquid etal Procedure for filling GED with a PUNB bonded sand saple and liquid etal Measured change in ass as a function of teperature typical of PUNB bonded sand saples, pure IC55 silica sand saples, the epty saple pan, and quartz rods during heating at a rate of 1 C/in with a total argon gas flow of 8 c 3 /in Measured change in the ass of quartz rods as a function of teperature during heating at rates of 2 C/in, 1 C/in, and 1 C/in Coparison of the uncorrected and corrected percentage of ass reaining as a function of teperature in a (a) 55 g PUNB bonded sand saples and (b) 7.5 g pure PUNB binder saples during heating at a rate of 1 C/in with a total argon gas flow of 8 c 3 /in Measured percentage of ass reaining in the individual coponents of PUNB bonded sand as a function of teperature during heating at a rate of 1 C/in with a total argon gas flow of 8 c 3 /in Measured fraction of original binder ass reaining in various asses of PUNB bonded sand as a function of teperature during heating at a rate of 1 C/in with a total argon gas flow of 8 c 3 /in Measured fraction of original binder ass reaining in 55 g PUNB bonded sand saples as a function of teperature during heating at rates of 2 C/in, 1 C/in, and 1 C/in with total argon gas flow rates of (a) 8 c 3 /in and (b) 25 c 3 /in...65 vii

10 16. Coparison of the fraction of original binder ass reaining in bonded sand saples as a function of teperature during heating fro the present PUNB easureents (averaged) using total argon flow rates of (a) 8 c 3 /in and (b) 25 c 3 /in with the fractions calculated fro TGA data of previous studies Measured fraction of original binder ass reaining in 7.5 g pure PUNB binder saples as a function of teperature during heating at rates of 2 C/in, 1 C/in, and 1 C/in with total argon gas flow rates of (a) 8 c 3 /in and (b) 25 c 3 /in Coparison of the fraction of original binder ass reaining in pure binder saples as a function of teperature during heating fro the present PUNB easureents (averaged) using total argon gas flow rates of (a) 8 c 3 /in and (b) 25 c 3 /in with the fraction calculated fro TGA data of Lytle for pure PUCB binder with a 55:45 ratio of Part 1 to Part Coparison of the average fraction of original binder ass reaining in 55 g PUNB bonded sand and 7.5 g pure PUNB binder saples as a function of teperature during heating at rates of 2 C/in, 1 C/in, and 1 C/in with total argon gas flow rates of (a) 8 c 3 /in and (b) 25 c 3 /in Measured etal-only height change in the GED as a function of teperature during heating at constant rates ranging fro 2 C/in to 15 C/in Liquid etal voluetric expansion coefficients calculated fro etal-only expansion in the GED and the borosilicate bulb as a function of teperature during heating Coparison of easured and predicted etal-only height change in the GED as a function of teperature during heating Measured height change as a function of teperature for all pure gas expansion tests in the GED Measured teperature difference in the GED s therocouple wells as a function of etal teperature for all pure gas expansion tests Ratio of easured to known olecular weight of (a) argon gas and (b) hydrogen gas as a function of teperature during heating Ratio of easured to known olecular weight of argon gas fro all pure argon gas expansion tests as a function of teperature Measured height change as a function of teperature during heating and cooling of different PUNB bonded sand saple asses Binder gas olecular weight easureents as a function of teperature during heating and cooling of different PUNB bonded sand saple asses...79 viii

11 29. Coparison of the easured binder gas olecular weight as a function of teperature with and without the hydrogen dissolution correction during heating of a.637 g PUNB bonded sand saple at a rate of 2 C/in Coparison of the easured to known olecular weight ratio of argon for pure argon gas saples and argon gas with a 1.18 g saple of cleaned IC55 silica sand as a function of teperature during heating Measured binder gas oles evolved per original binder ass as a function of teperature during heating and cooling of different PUNB bonded sand saple asses Coparison of the piecewise polynoial fitted to the present binder gas olecular weight easureents for a heating rate of 2 C/in with the results fro previous studies as a function of teperature...84 ix

12 LIST OF NOMENCLATURE Acronys BIO DSC GC GC-FID GC-MS GC-TCD GED HC total PU PUCB PUNB TGA TGA-MS Black Iron Oxide Differential Scanning Calorietry Gas Chroatography Gas Chroatography-Flae Ionization Detector Gas Chroatography-Mass Spectroetry Gas Chroatography-Theral Conductivity Detector Gas Evolution Device Total Hydrocarbons Phenolic Urethane Phenolic Urethane Cold-Box Phenolic Urethane No-Bake Therogravietric Analysis Therogravietric Analysis-Mass Spectroetry Sybols β voluetric expansion coefficient of the liquid etal (1/ C) con β voluetric expansion coefficient of the liquid that is constant with respect to teperature (1/ C) eff β effective voluetric expansion coefficient of the liquid etal in the GED (1/ C) ϕ ratio of the easured to known olecular weight of an ideal gas ρ density of the liquid etal (g/c 3 ) ρ density of the liquid etal at roo teperature (g/c 3 ) χ saple binder content based on total saple weight (wt. %) D 1,eff effective internal diaeter of cylinder 1 of the GED (c) D 2 f internal diaeter of cylinder 2 of the GED (c) fraction of original binder ass reaining x

13 g gravitational acceleration (/s 2 ) h 1 h 2 c h 2 g h 2 H h 1 h 2 b g d g d* g s s M Ar M b M H 2 M i M g n b P at P g P g P probe easured total etal height change in cylinder 1 of the GED (c) easured total etal height change in cylinder 2 of the GED (c) total etal height change in cylinder 2 of the GED that includes a correction for hydrogen gas dissolution into the liquid etal (c) the portion of height change in cylinder 2 of the GED due to gas evolution and/or expansion (c) height difference between the etal surfaces in cylinders 1 and 2 of the GED (c) initial liquid etal height in cylinder 1 of the GED (c) initial liquid etal height in cylinder 2 of the GED (c) total ass of evolved binder gas (g) total gas ass (g) ass of hydrogen gas dissolved into the liquid etal (g) ass of hydrogen gas dissolved into the liquid etal that is approxiated by a Taylor series (g) ass of liquid etal in the filled GED (g) saple ass easured by the TGA achine (g) total initial saple ass loaded into the TGA achine or the GED (g) olecular weight of argon gas (g/ol) olecular weight of the evolved binder gas (g/ol) olecular weight of hydrogen gas (g/ol) true olecular weight of a easured gas i (g/ol) olecular weight of an ideal gas coponent or gas ixture (g/ol) oles of evolved binder gas per original binder ass (ol/g) atospheric pressure (Pa) gas pressure (Pa) initial gas pressure (Pa) pressure fro the weight of the displaceent probe and boat (Pa) xi

14 R T T T universal gas constant (J/ol/K) difference between the easured glass and etal teperatures ( C) gas or saple teperature initial gas or saple teperature T glass easured exterior glass teperature ( C) T T T ɺ easured etal teperature ( C) easured initial etal teperature ( C) heating rate ( C/in) V fill volue contained by the filled GED at the initial teperature (c 3 ) V g gas volue (c 3 ) V g initial gas volue (c 3 ) V g change in gas volue (c 3 ) V change in volue of the liquid etal (c 3 ) xii

15 1 CHAPTER 1. INTRODUCTION 1.1 Background and Motivation Modern foundries use nonperanent olds and cores that are ade fro silica sand and held together by a resin binder to aintain the desired casting shape until the etal is poured and solidified. The bonded sand old creates the priary for of the casting, and bonded sand cores are eployed to produce cavities within the casting. A great deal of heat is transferred to the sand and resin binder when the olten etal is poured into the old. This causes the binder to pyrolyze, or therally decopose at elevated teperatures in the absence of oxygen, and a significant aount of gas evolves when the binder degrades [1]. Binder gas evolution, or siply the characteristic production of gas due to binder theral decoposition, ay be discussed in ters of the generation of binder gas ass or volue. It is well understood that binder gas evolution can profoundly influence the quality of etal castings [2-4]. Inadequate venting of the binder gas fro the old and eployed cores will increase the tendency to for casting porosity defects, which are gas bubbles that becoe trapped in the etal during solidification [1]. The two types of porosity defects ost coonly associated with binder gas evolution are blowholes and pinholes [5-9]. The evolved binder gas will penetrate the olten etal s surface if the gas pressure exceeds the local etallostatic pressure, which causes blowholes to for if the gas does not escape fro the etal before solidification occurs [1,9]. The solubility of gas in the liquid etal decreases as the etal solidifies, and pinholes for when dissolved gas is rejected fro solution and trapped in the etal during solidification. Binder gas generation at the old-etal interface (defined here as the locations where the old or core contact the etal) ay lead to increased dissolution of gas in the etal, thereby increasing the tendency for pinholes to for as the liquid etal solidifies [1,9]. Bonded sand olds and cores are pereable and ay have porosities as high as 5% [9]. The gas evolved in the old usually has aple opportunity to diffuse away

16 2 fro the old-etal interface through the porous space in the old. However, gas defects ay still for due to the binder gas generation in the old. In the case of cores, the area of the core prints (insets in the old for holding cores in place) provides the only eans for the gas to escape the cores without passing through the liquid etal. In addition, a sand core is heated uch faster than the old (causing ore coplete binder decoposition and greater gas evolution in the core) because the core is typically surrounded on any sides by hot etal and the core is uch saller copared to the old [1]. Many variables influence the foration of gas defects in castings; however, the conditions that proote the foration of binder gas defects during casting are ore often found in cores than in the old. Defects caused by binder gas evolution result in large aounts of scrap and are of great concern to the etal casting industry. In response to these issues, coputational odels that predict binder gas evolution during casting have been incorporated into etal casting siulations in order to better predict the occurrence of gas defects (for exaple, References [1-12]). Accurate prediction of such defects allows for better design of sand olds and cores for the production of quality castings. Crucial eleents required for the use and validation of binder gas evolution odels are the ass and olecular weight of the evolved gas as a function of teperature. Unfortunately, teperature-resolved binder gas ass evolution and olecular weight data corresponding to the conditions experienced during sand casting processes are extreely liited. 1.2 Objective of Present Study The objective of this study is to easure the ass and olecular weight of the gas evolved during decoposition of phenolic urethane no-bake bonded sand as a function of teperature at conditions siilar to those experienced during actual sand casting processes. The experiental results will provide iproved input and validation data for binder gas evolution odels used in casting siulations.

17 3 CHAPTER 2. LITERATURE REVIEW 2.1 Phenolic Urethane Binder Systes A wide variety of cheical binder systes are available for the production of olds and cores used in the sand casting process. The phenolic urethane (PU) syste is the ost coonly used synthetic binder syste in the United States [13]. The PU binder syste is a three-part syste that cobines a phenol-foraldehyde resin dissolved in solvents (Part 1), a polyeric isocyanate dissolved in solvents (Part 2), and a tertiary aine catalyst (Part 3) to produce a urethane bond. The general reaction equation for the PU syste can be seen in Figure 1. The solvents are eployed to reduce the viscosity and increase the reactivity of the binder coponents [13,14]. The catalyst acts to control and accelerate the reaction between the phenolic resin and the isocyanate [13]. The PU syste can be further divided into phenolic urethane cold-box (PUCB) and phenolic urethane no-bake (PUNB) processes, with the priary difference between these ethods being the anner in which the catalyst is introduced to the syste. The PUCB process involves coating sand with the Part 1 and Part 2 coponents, shaping and copacting the sand-binder ixture into the desired for, vaporizing the Part 3 catalyst and blowing it through the sand-binder ixture, and blowing air through the bonded sand to reove any residual gaseous catalyst. The PUNB process involves cobining the Part 1 coponent with the Part 3 catalyst as a liquid, coating the sand with the resin-catalyst ixture, adding the Part 2 coponent to the coated sand, shaping and copacting the sand-binder ixture into the desired for, and allowing the bonded sand to cure. The PUCB catalyst is designed to function priarily as a reaction accelerant, while the PUNB catalyst acts to predictably control and accelerate the bonding reaction [15,16]. The cheical forulations eployed in Parts 1-3 for the PUCB and PUNB processes are different. This is ainly due to the difference in which the catalyst is added to the sand-binder ixture. However, the PUCB and PUNB systes are based on the sae urethane bonding cheistry illustrated in Figure 1 [13,14]. This siilarity allows

18 4 the coposition and olecular weight of the gas evolved fro these systes to be reasonably copared. 2.2 Binder Gas Molecular Weight Data Knowledge of the evolved binder gas coposition facilitates deterination of the gas s olecular weight. Unfortunately, however, teperature-resolved binder gas coposition data are quite liited. Early studies by Bates and Scott [17,18], Bates and Monroe [19], and Scott et al. [2] involved pouring aluinu, gray iron, and steel into olds ade using different binder systes and periodically sapling the gas generated at the old-etal interface. The experiental setup used to saple the gas in Reference [19] is illustrated in Figure 2, and this ethod was essentially the sae as those eployed in References [17], [18], and [2]. Bonded sand was raed inside a Büchner funnel fitted with a vent tube, and the funnel was raed into the drag of the sand old. The inlet of the vent tube was positioned to be 6.35 (.25 in) fro the old-etal interface. The opposite end of the tube was attached to a hypoderic needle. Once the casting was poured, gas evolved fro the bonded sand inside the funnel, and the binder gas was sapled by inserting evacuated glass tubes into the vent tube s hypoderic needle. The gas saples were analyzed by gas chroatography (GC) coupled with either a flae ionization detector (GC-FID) or a theral conductivity detector (GC-TCD) to deterine the volue concentrations (%V/V) of hydrogen, oxygen, nitrogen, carbon onoxide, carbon dioxide, and the total hydrocarbons (HC total ) in the binder gas. HC total was easured as the equivalent concentration of ethane. The average coposition and ixture olecular weight of the gas evolved within two inutes after pouring etal into PUCB and PUNB bonded sand olds are shown in Table 1. The reported volue concentrations are converted to ass fractions for the present analysis. The olecular weights calculated fro the average gas copositions within the first two inutes after pouring should

19 5 roughly correspond to the pouring teperatures of the etal [21]. The results in Table 1 show that in general the binder gas generated during pouring of the gray iron and steel castings was ostly coprised of carbon onoxide and carbon dioxide, had varying aounts of nitrogen and hydrocarbons, and low aounts of hydrogen and oxygen. The binder gas fro the aluinu castings, poured at significantly lower teperatures than the gray iron and steel castings, was coprised alost entirely of oxygen and nitrogen. This indicates that the evolution of binder gas within the first two inutes after pouring the aluinu castings was insufficient to replace the air atosphere originally in the olds, iplying that hydrogen, carbon onoxide, carbon dioxide, and hydrocarbons significantly evolve at higher teperatures. Unfortunately, the binder gas likely experienced soe condensation before it escaped the test old and was collected, aking the easured coposition not entirely representative of the actual binder gas coposition. In addition, the binder gas saples had the opportunity to cool inside the collection tubes prior to injection of the saples into the gas chroatograph, which likely caused the binder gas to condense before it could be analyzed. Regardless of these issues, the olecular weight data calculated fro References [17-2] are useful for coparison against the present olecular weight easureents. More recently, McKinley et al. [22] (with detailed inforation and analysis available in the work of Lytle [23]) perfored flash pyrolysis of 1.5% PUCB bonded sand and used gas chroatography-ass spectroetry (GC-MS) to analyze the evolved binder gas. 1 g saples of PUCB bonded sand were rapidly heated to 5, 7, and 9 C in a heliu atosphere and held at these teperatures for various periods of tie. The pyrolysis products were swept directly into the gas chroatograph, and gas species ranging fro 1 g/ol to 425 g/ol were detected by the ass spectroeter. The ass fraction of the priary coponents eitted fro the PUCB bonded sand during 2 seconds of pyrolysis at 7 C and 9 C and the ixture olecular weights calculated fro the coposition data are shown in Table 2. The coponents in Table 2 coprise

20 6 ore than 99% of the easured gas species at each teperature, with the reaining gases being high olecular weight copounds. It can be seen fro Table 2 that, besides carbon onoxide, the ajor species evolved are hydrocarbons. In addition, the binder gas coposition experiences significant changes between 7 C and 9 C. None of the coponents listed in Table 2 were detected during pyrolysis at 5 C. However, the olecular weight of the gas ixture evolved at 5 C was calculated to be 137 g/ol. The gas coponents evolved fro bonded sand will freely ix throughout the casting process, and Reference [22] acknowledges that the evolved binder gas coponents will interact with one another and ay cobine to for new copounds. Therefore, the gas species separation required for thorough GC analysis deviates fro the conditions experienced during actual casting processes. Despite this fact, the detailed coposition data fro References [22] and [23] currently provide the only eans to directly obtain teperature-resolved olecular weight data for gas evolved fro bonded sand used in casting processes. Very recently, Wang et al. [24] perfored pyrolysis of 1.5% PUCB bonded sand in a therogravietric analyzer fro 2 C to 9 C at a heating rate of 1 C/in with a total nitrogen gas flow rate of 6 c 3 /in. Granular activated carbon tubes and Tedlar gas sapling bags were used to collect the binder gas fro the analyzer throughout the heating process. The contents of the granular activated carbon tubes were analyzed by GC-FID, and the contents of the gas sapling bags were analyzed by both GC-FID and GC-TCD. Separate therogravietric analysis (TGA) experients were eployed to easure the ass loss in PUCB bonded sand fro theral decoposition, which is equivalent to the evolved binder gas ass. Unfortunately, the coponents detected in the binder gas evolved fro bonded sand during TGA pyrolysis only accounted for 21% of the generated binder gas ass. The investigators reported that significant aounts of liquid pyrolysis products collected within the TGA achine, thereby preventing these copounds fro being analyzed. As in References [17-2], the analysis of the gas was

21 7 perfored well after the gas was collected, which ay have caused additional error in the easureent of the gas coposition. The ass fractions of the easured coponents eitted fro the PUCB bonded sand (relative to the total generated binder gas ass easured fro TGA of bonded sand) and the corresponding gas ixture olecular weight are shown in Table 3. The calculated olecular weight is not particularly useful because it represents only a sall portion of the gas coponents evolved fro the bonded sand. In addition, the calculated olecular weight is not teperature-resolved, which prevents it fro being directly copared with the present binder gas olecular weight easureents. Reference [24] also perfored TGA pyrolysis coupled with ass spectroetry (TGA-MS) to deterine the teperatures at which ajor binder gas coponents evolved. Again, however, condensation of the binder gas likely prevented this analysis ethod fro fully characterizing the binder gas olecular weight as a function of teperature. Coparison of the results fro Tables 1 through 3 offers additional insight into the nature of the binder gas evolution for PU systes. References [23] and [24] did not detect any oxygen or nitrogen in the binder gas. Therefore, it sees quite plausible that the nitrogen and oxygen easured in References [17-2] during all casting experients were actually fro the residual air in the old. The significant hydrocarbon content at 7 C reported by References [22] and [23] also contradicts the results of References [17-2] at 75 C (aluinu castings). In addition, the uncharacterized portion of the binder gas ass (79% of the total evolved gas ass) in Reference [24] ost likely contained coplex hydrocarbons and other organic copounds. There is agreeent between the previous studies on the presence (although not the relative quantity) of carbon onoxide and ethane in the binder gas. References [17-2] and [24] agree on the presence (though again not the relative quantity) of carbon dioxide in the binder gas. It should also be noted that the gas ixture olecular weights calculated fro the coposition data fro previous studies are relatively siilar in agnitude.

22 8 Even though coupling GC with any one of the any types of gas detectors provides the eans to analytically deterine the binder gas coposition and olecular weight, this technique is not well suited to generate the agnitude of teperatureresolved olecular weight data required in binder gas odels. TGA coupled with a gas detector allows for ore reasonable easureent of the gas coposition (or the gas olecular weight when TGA-MS is eployed) as a function of teperature. As exeplified by the TGA and GC experients in Reference [24], however, condensation of the binder gas prior to analysis ay draatically affect the binder gas easureents. Eliination of binder gas condensation fro the TGA syste likely requires coplex odification of the analysis equipent, which is undesirable. 2.3 Gas Evolution Tests Deterination of the binder gas olecular weight as a function of teperature fro additional binder gas coposition easureents is ipractical due to the previously described experiental difficulties, analysis coplexity, and high equipent costs. The second ethod for deterining the binder gas olecular weight is to use the ideal gas law in conjunction with easureents of the evolved binder gas ass, volue, and pressure as a function of teperature. TGA of bonded sand facilitates deterination of the binder gas ass evolution as a function of teperature. The experiental difficulty lies in easuring the volue and pressure of the evolved gas as a function of teperature under conditions siilar to those experienced during actual casting processes. Dietert et al. [25], Moore and Mason [26] and Zhang et al. [27] used siilar apparatuses to easure the pressure generated by gas evolved fro bonded sand heated in a furnace. The gas pressure could then be converted to gas volue by a calibration ethod. The device s interior surfaces were aintained above 11 C to liit gas condensation and the bonded sand saples were iersed in a nitrogen atosphere during the test. The device used by Reference [27] is shown in Figure 3. Unfortunately,

23 9 any issues prevent such a device fro being used to easure the olecular weight of the binder gas. The apparatus only allows tests to be perfored at individual furnace teperatures, which severely liits the experiental flexibility of the olecular weight easureents. Only a portion of the evolved gas volue was contained within the hot zone of the furnace, and this will likely cause nonisotherality in the evolved gas volue that would lead to inaccurate volue and pressure easureents. Furtherore, heating the gas evolution syste s interior surfaces to 11 C ay not be sufficient to prevent condensation of all the binder gas coponents. The binder gas ass easureents fro the TGA experients need to be atched with the evolved gas volue and pressure easureents as a function of teperature for use in the olecular weight calculations, but the device offers no eans to directly easure the teperature of the bonded sand and evolved binder gas. In addition, the heating rates eployed during easureent of the evolved binder gas ass, volue, and pressure as a function of teperature need to be the sae in order to properly calculate the binder gas olecular weight. The gas evolution syste does not provide the eans to control the heating rate of the bonded sand and evolved binder gas, which akes volue and pressure easureents obtained with the device unsuitable for the olecular weight calculations. The gas evolution syste eployed in References [25-27] ust undergo significant odifications before it could be used to easure the binder gas volue, pressure, and teperature for use in binder gas olecular weight calculations. In addition to analyzing the binder gas coposition, Bates and Monroe [19] easured the volue and pressure of gas evolved fro the old during pouring of gray iron, steel, and aluinu castings. Their experiental ethods for easuring the binder gas volue and pressure are shown in Figure 4. Separate funnels attached to vent tubes and filled with test sand were raed into the sand old in a siilar anner as those eployed for gas sapling as previously described. One vent tube was attached to the inlet of a bubble flow eter, and the other vent tube was connected to a pressure

24 1 transducer. After the casting was poured, the evolved gas volue was easured by onitoring the oveent of bubbles through the bubble flow eter, and the gas pressure was directly easured with the pressure transducer. A therocouple protected by a quartz sheath was also used to easure the teperature at the center of the casting. These experiental ethods have liited use in the present study. Even with odification, this approach does not easily facilitate the easureent of the gas volue and pressure at the sae location inside the bonded sand saple. The teperature of the binder gas at the inlet points of the vent tubes also needs to be easured. The bonded sand saple likely needs to be fairly large to accoodate both vent tubes as well as a teperature probe. The tendency for the binder gas to condense in the bonded sand will increase as the bonded sand saple size increases, and binder gas condensation ust be avoided in order to properly easure the binder gas olecular weight. Nonisotherality in the evolved gas along the length of the vent tube attached to the bubble flow eter ay lead to erroneous volue readings. Another proble is that the heating rate of the bonded sand and evolved binder gas cannot be controlled, and this is highly undesirable for reasons previously described. While it is valuable to study gas evolution characteristics during actual casting processes, the experiental approach of Reference [19] is ipractical for easuring the binder gas olecular weight as a function of teperature. Scarber et al. [28] developed an apparatus for easuring the gas evolution rates and evolved gas volues in cores iersed in olten etal. This apparatus is illustrated in Figure 5 (a). A cylindrical bonded sand core was printed on a sealed steel holder attached to a preheated gas line. The core was then iersed in olten etal. The gases produced fro binder decoposition flowed out of the core through the gas line and displaced oil in a preheated chaber. The displaced oil flowed out of the chaber through a vent tube and into a container positioned on a precision electronic balance. Knowledge of the oil density and the easured oil weight facilitated calculation of the evolved volue of binder gas. The gas line and oil chabers were aintained at

25 11 teperatures that would prevent water condensation, and therocouples onitored the teperatures in the gas line. Winardi et al. [29] inserted a pressure probe into the axial center of the core to easure the gas pressure inside the core during olten etal iersion. Their device is depicted in Figure 5 (b). Winardi et al. [3] later replaced the pressure probe with therocouple probes inserted at various distances fro the interface of the core and the etal. Starobin et al. [12] used the gas pressure and total collected gas volue data fro the previously described core iersion experients to calculate an effective binder gas olecular weight. The calculated value of 23 g/ol fro Reference [12] is in agreeent with the gas coposition results of References [17-2], but this value only applies to the entire volue of evolved binder gas and is unrelated to the binder gas teperature. Like all previous gas evolution easureent techniques, the core iersion apparatus described by Reference [28] ay still allow the binder gas to condense. Even though any volatiles with low boiling points and water vapor are kept fro condensing due to the preheating of the gas line and oil chaber, volatiles with high boiling points ay still be allowed to condense within the core itself, the gas lines, or in the oil chaber. The inherent design of the apparatus ay cause delays between the evolution of binder gas and the corresponding volue easureent by oil displaceent. Cobining the experiental techniques of References [29] and [3] allows for easureent of the binder gas volue and pressure as a function of teperature, but the volue easureent occurs at a location apart fro the pressure and teperature easureents. Ideal deterination of the binder gas olecular weight requires easureent of the volue of gas evolved fro the bonded sand while siultaneously easuring the pressure and teperature of that sae evolved gas volue. The lack of control over the heating rates in the core will greatly coplicate the easureent of the binder gas olecular weight for reasons previously described. Therefore, the core iersion apparatus is not suitable for easuring the binder gas olecular weight as a function of teperature.

26 12 OH + NCO Aine catalyst O O C NH Phenolic resin Polyeric isocyanate Urethane bond Figure 1: General bonding reaction equation for PUCB or PUNB binder systes [13].

27 Figure 2: Experiental technique used by Bates and Monroe [19] to saple the gas evolved fro decoposition of bonded sand during pouring of etal castings. The other sections of the casting s old are not illustrated. This sapling ethod is essentially the sae as those eployed by Bates et al. [17,18] and Scott et al. [2]. 13

28 14 Table 1: Tie-averaged ass fraction and ixture olecular weight of gas coponents evolved fro PUCB and PUNB bonded sand within 2 inutes after pouring during the experients of Bates et al. [17-19] and Scott et al. [2]. Experient Description Coponent Mass Fraction Mixture Molecular Binder Syste Metal and Average Pouring Teperature H 2 O 2 N 2 CO CO 2 HC total * Weight [g/ol] 2% PUCB 1.3% PUCB 2% PUNB Gray Iron at 1446 C Gray Iron at 1457 C Gray Iron at 1431 C % PUNB Gray Iron at 143 C % PUNB Steel at 162 C % PUNB Aluinu at 75 C *Total hydrocarbons easured as equivalent to ethane

29 15 Table 2: Priary cheical coponents identified by McKinley et al. [22] and Lytle [23] through GC-MS analysis during 2 seconds of pyrolysis of 1.5% PUCB bonded sand and the calculated gas ixture olecular weights. Coponent Cheical Forula Methane CH Carbon Monoxide CO Ethene C 2 H Propene C 3 H Propenenitrile C 3 H 3 N ,3-Butadiene C 4 H Butene C 4 H ,3-Pentadiene C 5 H Pentene C 5 H Mixture Molecular Weight of Priary Coponents [g/ol]: Mass Fraction at 7 C Mass Fraction at 9 C 36.3 at 7 C 38. at 9 C

30 16 Table 3: Cheical coponents identified by Wang et al. [24] through GC-FID and GC-TCD analysis during TGA pyrolysis of 1.5% PUCB bonded sand at a heating rate of 1 C/in and the calculated gas ixture olecular weight. Coponent Cheical Forula Mass Fraction fro 2 C to 9 C Methane CH Carbon Monoxide CO.287 Carbon Dioxide CO Hexane C 6 H 14.4 Benzene C 6 H 6.16 Toluene C 7 H 8.26 Xylene C 8 H 1.15 Phenol C 6 H 6 O.42 Cresols C 7 H 8 O.3 Methylnaphthalene C 11 H 1.19 Methyl Oleate C 19 H 36 O Other Species *.188 *Measured as equivalent to ethyl oleate Mixture Molecular Weight of Measured Coponents [g/ol]: 38.7 fro 2 C to 9 C

31 Figure 3: Gas evolution tester eployed by Zhang et al. [27]. Dietert et al. [25] and Moore and Mason [26] eployed siilar devices to study gas evolution fro bonded sand. The illustration was obtained fro Reference [31]. 17

32 18 (a) (b) Figure 4: Experiental ethods eployed by Bates and Monroe [19] to easure the (a) volue and (b) pressure of gas evolved fro bonded sand. The other sections of the castings olds are not illustrated.

33 19 Resistance Heaters heaters Oil refill funnel Refill Funnel Oil vent tube Steel holder Sand core Hot oil Beaker Beaker Precision Balance balance Furnace Furnace filled with olten etal Data acquisition syste Data Acquisition Syste (a) Steel pressure probe Gas out Iron tube Molten etal Steel holder (b) Core Figure 5: Techniques for easuring binder gas evolution fro cores iersed in olten etal: (a) displaceent apparatus developed by Scarber et al. [28] for easuring the evolved binder gas volue; (b) odification of displaceent apparatus by Winardi et al. [29] for easureent of the binder gas pressure inside the test core.

34 2 CHAPTER 3. EXPERIMENTAL METHODS 3.1 Experiental Approach of Present Study In the present study, the ass and olecular weight of the binder gas evolved during decoposition of PUNB bonded sand is easured under conditions siilar to those experienced during casting. TGA is eployed to easure the binder gas ass as a function of teperature for heating rates experienced in the old and cores during casting processes. A specially designed quartz anoeter is used to easure the binder gas volue, pressure, and teperature during heating and cooling in a furnace. These gas evolution easureents are cobined with the ideal gas law to deterine the binder gas olecular weight as a function of teperature. The bonded sand is iersed in an inert atosphere during the experients to ensure that the binder pyrolyzes, which is reflective of the binder decoposition behavior experienced during casting. Unlike in previous studies, the evolved binder gas is contained and easured entirely within the hot zone of a furnace, which eliinates the potential for undesired binder gas condensation during heating and other issues related to non-localized gas easureent. The present experiental techniques also allow for continuous easureent of the binder gas olecular weight variations with teperature. 3.2 Preparation of Speciens The PUNB bonded sand specien coposition and preparation procedure follow those eployed by Thole and Beckerann [32]. Speciens of bonded sand were prepared fro IC55 silica lake sand, black iron oxide (BIO), and a PUNB binder syste. The values for the binder content (1.25% of total ass), binder ratio (6:4 ratio of Part 1 to Part 2), catalyst percentage (8% of total binder ass), and additives (BIO, 3% of total ass) were selected based on feedback fro seven steel foundries. The sand and BIO coponents were easured using an Ohaus odel PA411 precision balance, and the binder coponents were easured using a Denver Instruents

35 21 odel S-43 precision balance. The speciens were prepared by first ixing the BIO into the sand with a KitchenAid standing ixer to ensure unifor particulate distribution. Then the binder was added according to a procedure recoended by the binder anufacturer. Part 1 (Pep Set X1) and Part 3 (Pep Set 35) were cobined in a paper cup and subsequently added to the particulate ixture. The batch was ixed for 45 seconds, and then vigorously tossed to bring the coated ixture fro the botto of the ixing bowl to the top. The batch was ixed for another 45 seconds and tossed again. After the second toss, Part 2 (Pep Set X2) was added to the batch and ixed for another 45 seconds, which was followed by a third tossing. The batch was ixed for a final 45 seconds before duping it into a box with rectangular patterns. The sand-binder ixture was raed by hand into each pattern, while aking sure the speciens were of unifor density, and allowed to set in the box before stripping (reoval of the speciens fro the pattern box). The bonded sand speciens were stripped when the copacted ixture withstood 2 psi of copressive stress without visible deforation [14]. The pattern box was capable of aking six bonded sand blocks, each with a 2.54 c (1 in) square cross-section and a c (9 in) length. The speciens were iediately sealed in plastic bags to iniize evaporation of the solvents, and the speciens were allowed to cure inside the bags for at least 24 hours prior to testing. Sall speciens of pure PUNB binder were prepared using the sae binder syste, binder ratio, and catalyst percentage as the bonded sand speciens. The pure binder speciens were prepared by first cobining Part 1 and Part 3 in a paper cup. Then Part 2 was added to the other binder coponents, and the ixture was vigorously stirred for 1 seconds. The ixture was iediately poured into a sall old with rectangular patterns. Once the liquid binder ixture solidified, the pure binder speciens were reoved fro the pattern and iediately sealed in plastic bags. Like the bonded sand speciens, the pure binder speciens were allowed to cure inside the bags for at least 24 hours before testing.

36 Therogravietric Analysis TGA was perfored on PUNB bonded sand and pure PUNB binder using a PerkinEler odel Pyris 1 therogravietric analyzer. This achine easured the ass and teperature of a saple of interest during heating at a specified rate. The PUNB bonded sand speciens were cut down into saller pieces, which were then shaped into sall cylinders using a razor blade. The PUNB bonded sand saples for TGA were approxiately 55 g, and the saples were about.45 c in diaeter and.25 c in height. The pure PUNB binder speciens were pulverized into sall particles. The pure binder saples for TGA easured approxiately 7.5 g. The TGA achine was purged with argon gas, and the total gas flow rates eployed were 8 c 3 /in (6 c 3 /in to the balance and 2 c 3 /in to the sheath) and 25 c 3 /in (15 c 3 /in to the balance and 1 c 3 /in to the sheath). The 25 c 3 /in total flow rate was specifically chosen in order to iniize nonisotherality in the saples during testing. The argon gas flow created a bias in the TGA achine s ass easureents, which necessitated separate easureent of the initial saple ass. The initial ass of each saple was easured using a Mettler-Toledo odel AB135-S analytical balance prior to testing. The saples were heated fro roo teperature to 1 C at rates of 2 C/in, 1 C/in, and 1 C/in. The heating rates for TGA were selected to reflect those experienced in the old during actual casting processes. The high heating rate of 1 C/in siulated old and core heating rates at a distance of about.5 in fro the old-etal interface, and the 2 C/in and 1 C/in heating rates siulated old and core heating rates at distances further away fro the old-etal interface. Multiple tests were perfored at each heating rate to verify repeatability of the experients. The TGA achine was allowed to self-clean periodically between tests, and the saple pans were cleaned according to the recoendations of the anufacturer. The fraction of original binder ass reaining f in a PUNB bonded sand saple

37 23 or a pure PUNB binder saple as a function of teperature during heating was calculated by f= s 1 s ( T ) ( T) χ s 1 (1) where teperature s is the saple ass easured by the TGA achine at both the initial saple T and varying saple teperature T, s is the initial saple ass easured with the analytical balance, and χ is the binder content of the saples based on the total weight percentage. The binder content for the pure binder saples was obviously 1%. The fraction of original binder ass reaining in bonded sand during heating was interpolated at intervals of.1 C fro the corresponding fractions obtained fro the TGA easureents. This allowed the easureents of the binder gas ass evolution to be atched with the easured binder gas volue and pressure (obtained fro later gas evolution experients) at discrete teperature points. 3.4 Gas Measureent Apparatus A scheatic of the apparatus developed in the present study to easure the volue, pressure, and teperature of gas during heating or cooling is shown in Figure 6. The priary coponent is the gas evolution device (GED), ade by fusing quartz cylinders and discs together. Cylinder 1 of the GED was sealed at the top and botto and had two quartz therocouple wells attached to the top surface. One therocouple well extended up fro the top of cylinder 1, while the other extended 2 c fro the top surface down into the interior of cylinder 1. Cylinder 1 had an internal diaeter of 4 c and a height of 3 c. Cylinder 2 of the GED was sealed at the botto, had an internal diaeter of 1.3 c, and had a height of 22 c. Cylinders 1 and 2 were joined by a third quartz tube, creating a container with a J-shaped cavity that acted as a anoeter. A saple of interest was loaded into cylinder 1 of the GED, and the GED was

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