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CHAPTER TWO
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The regeneration step, that is, the reaction with oxygen is exothermic and air must be introduced slowly so the heat of reaction can be dissipated If air is introduced quickly the heat of reaction may ignite the bed Some of the elemental sulfur produced in the regeneration step remains in the bed After several cycles this sulfur will cake over the ferric oxide, decreasing the reactivity of the bed Typically, after 10 cycles the bed must be removed and a new bed introduced into the vessel In some designs the iron sponge may be operated with continuous regeneration by injecting a small amount of air into the sour gas feed The air regenerates ferric sulfide while hydrogen sulfide is removed by ferric oxide This process is not as effective at regenerating the bed as the batch process and requires a higher-pressure air stream (Arnold and Stewart, 1999) In the process (Fig 29), the sour gas should pass down through the bed In the case where continuous regeneration is to be utilized a small concentration of air is added to the sour gas before it is processed This air serves to continuously regenerate the iron oxide, which has reacted with hydrogen sulfide, which serves to extend the on-stream life of a given tower but probably serves to decrease the total amount of sulfur that a given weight of bed will remove The number of vessels containing iron oxide can vary from one to four In a two-vessel process, one of the vessels would be on-stream removing hydrogen sulfide from the sour gas while the second vessel would either be in the regeneration cycle or having the iron sponge bed replaced
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Sweet gas To next process
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FIGURE 29 Typical iron oxide process flow sheet Maddox, R N Gas and Liquid Sweetening, 2nd ed, Campbell Petroleum Series, Norman, Okla, 1974
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Generally, the iron oxide process is suitable only for small to moderate quantities of hydrogen sulfide Approximately 90 percent of the hydrogen sulfide can be removed per bed, but bed clogging by elemental sulfur occurs and the bed must be discarded and the use of several beds in series is not usually economical Removal of larger amounts of hydrogen sulfide from gas streams requires a continuous process, such as the Ferrox process or the Stretford process The Ferrox process is based on the same chemistry as the iron oxide process except that it is fluid and continuous The Stretford process employs a solution containing vanadium salts and anthraquinone disulfonic acid (Maddox, 1974)
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NATURAL GAS
The natural gas should be wet when passing through an iron sponge bed as drying of the bed will cause the iron sponge to lose its capacity for reactivity If the gas is not already water-saturated or if the influent stream has a temperature greater than 50 C (approximately 120 F), water with soda ash is sprayed into the top of the contactor to maintain the desired moisture and alkaline conditions during operation Slurry processes were developed as alternatives to the iron sponge process Slurries of iron oxide have been used to selectively absorb hydrogen sulfide (Fox, 1981; Samuels, 1988) The chemical cost for these processes is higher than that for iron sponge process but this is partially offset by the ease and lower cost with which the contact tower can be cleaned out and recharged Obtaining approval to dispose of the spent chemicals, even if they are nonhazardous, is time consuming
274 Methanol-Based Processes Methanol is probably one of the most versatile solvents in the natural gas processing industry Historically, methanol was the first commercial organic physical solvent and has been used for hydrate inhibition, dehydration, gas sweetening, and liquids recovery (Kohl and Nielsen, 1997) Most of these applications involve low temperature where methanol s physical properties are advantageous compared with other solvents that exhibit high viscosity problems or even solids formation Operation at low temperatures tends to suppress methanol s most significant disadvantage, high solvent loss Furthermore, methanol is relatively inexpensive and easy to produce making the solvent a very attractive alternate for gas processing applications The use of methanol has been further exploited in the development of the Rectisol process either alone or as toluene-methanol mixtures to more selectively remove hydrogen sulfide and slip carbon dioxide to the overhead product (Ranke and Mohr, 1985) Toluene has an additional advantage insofar as carbonyl sulfide is more soluble in toluene than in methanol The Rectisol process was primarily developed to remove both carbon dioxide and hydrogen sulfide (along with other sulfur-containing species) from gas streams resulting from the partial oxidation of coal, oil, and petroleum residua The ability of methanol to absorb these unwanted components made it the natural solvent of choice Unfortunately, at cold temperatures, methanol also has a high affinity for hydrocarbon constituents of the gas streams For example, propane is more soluble in methanol than is carbon dioxide There are two versions of the Rectisol process (Hochgesand, 1970) the two-stage and the once-through The first step of the two-stage process is desulfurization before shift conversion; the concentrations of hydrogen sulfide and carbon dioxide are about 1 and 5 percent by volume, respectively Regeneration of the methanol following the desulfurization of the feed gas produces high sulfur feed for sulfur recovery The once-through process is only applicable for high pressure partial oxidation products The once-through process is also applicable when the hydrogen sulfide to carbon dioxide content is unfavorable, in the neighborhood of 1:50 (Esteban et al, 2000) Recently, a process using methanol has been developed in which the simultaneous capability to dehydrate, to remove acid gas, and to control hydrocarbon dew point (Rojey and Larue, 1988; Rojey et al, 1990) The IFPEXOL-1 is used for water removal and hydrocarbon dew point control; the IFPEXOL-2 process is used for acid gas removal The novel concept behind the IFPEXOL-l process is to use a portion of the water-saturated inlet feed to recover the methanol from the aqueous portion of the low temperature separator That approach has solved a major problem with methanol injection in large facilities, the methanol recovery via distillation Beyond that very simple discovery, the cold section of the process is remarkably similar to a basic methanol injection process Modifications to the process include water washing the hydrocarbon liquid from the low temperature separator
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