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Published:
 October 17, 2011
r
2011 American Chemical Society
 5126
 dx.doi.org/10.1021/ef200935g
|
Energy Fuels
 2011, 25, 5126
5137
ARTICLEpubs.acs.org/EF
Enhancement in Triethylene Glycol (TEG) Purity via HydrocarbonSolvent Injection to a TEG + Water System in a Batch DistillationColumn
Khadijeh Paymooni, Mohammad Reza Rahimpour,* Sona Raeissi, Mohsen Abbasi, andMohammad Saviz Baktash
Department of Chemical Engineering, School of Chemical and Petroleum Engineering, Shiraz University, Shiraz 71345, Iran
b
S
 Supporting Information
 ABSTRACT:
 Triethylene glycol (TEG) is one of the most important liquid desiccants in the natural gas dehydration industry. Inenhanced TEG regeneration processes, liquid hydrocarbons such as toluene and isooctane are added to the stripping column of natural gas dehydration unit in order to boost water volatility and regenerate TEG to higher purity. In this study, isooctane andtoluene were selected as liquid hydrocarbon solvents and the e
ff 
ect of these two solvents on TEG purity and the outlet waterconcentration from the reboiler of tray column were experimentally investigated and mathematically modeled. The vapor
liquidequilibrium calculations were performed using the NRTL activity coe
cient model and ideal gas equation of state to represent theliquid and vapor phases, respectively. Moreover, a comprehensive model was used to determine the liquid molar
 󿬂
ow rate on eachtraywhereitchangedwithtimeandtraybytray.Theimpactofvariousconcentrationsofsolventsanddi
ff 
erentoperatingconditions(total and no re
󿬂
ux) on the performance of the tray column was investigated. The modeling results were validated with theexperimental data, and good agreement was observed between them. Results showed that the least water concentration in thereboilerandthehighestTEGpuritywereachievedbyadding0.15wt%isooctaneundertotalre
󿬂
uxconditions.Theachievedresultscan provide an initial insight into designing equipments in enhanced TEG regeneration processes with hydrocarbon solventinjection.
INTRODUCTION
In this section, the main aspects of this study are outlined. Asdiscussedlater,themathematicalmodelingwascarriedoutincon- junction with experiments in order to achieve more reliable eva-luationoftriethyleneglycol(TEG)dehydrationunitperformance.
NaturalGasDehydration.
Natural gas is an important sourceof primary energy and it is saturated with water vapor undernormal production conditions.
1
The saturated water of naturalgas can cause some operational problems such as hydrate for-mation, corrosion, etc.
2
 Among different gas drying processes,absorptionisthemostcommontechniquewherethewatervaporin the gas stream is absorbed in a liquid solvent stream. Glycolsare the most widely used absorption liquids as they approximatethe properties that meet commercial application criteria. Severalglycols have been found suitable for commercial application.
3
 Actually, the main reason for glycols popularity is their superiorabsorption of water because the hydroxyl groups in glycols formsimilar associations with water molecules.
4
Triethylene glycol(TEG)hasgaineduniversalacceptance asthemostcost-effectiveglycol mainly due to more easy regeneration, less vaporizationlosses, lower capital and operating costs, higher initial theoreticaldecomposition temperature, etc.
5
TEG is used in a counter-current mass transfer operation inside a contractor to establishthe required water content in the outlet gas.
6
Bahadori and Vuthaluru developed a simple-to-use method, by employing basic algebraic equations, to correlate water removal efficiency as a function of TEG circulation rate and TEG purity for appro-priatesizingoftheabsorberatawiderangeofoperatingconditionsof TEG dehydration systems.
7
Furthermore, they developed therapid estimation of the water dew point of a natural gas stream inequilibrium with a TEG solution at various temperatures andTEG concentrations.
8
Darwish and Hilal simulated a typical pro-cess for natural gas dehydration using TEG as a desiccant using asteady state flowsheet simulator (Aspen Plus).
9
Enhanced Regeneration Process.
 In spite of previouslextensive investigations on typical natural gas dehydration units,several processes are available today while each applies differentstrategies to enhance glycol regeneration by reducing the effec-tivepartialpressureofwaterinthevaporphase.
10
Enhancedrege-neration could be the injection of stripping gas into the reboiler,azeotropic regeneration, or other processes.
11,12
Pearce et al.investigated a gas dehydration process in which glycol used asdehydrating agent is subsequently regenerated with toluene(Drizo Process).
13
The Drizo gas dehydration process uses highglycol concentrations to give low dew point temperatures andusesasolventtorecoverextractedaromatics.TheDrizotechnologhas evolved to overcome past reservations due to solvent losses,glycol losses, and glycol contamination of downstream low tem-perature ethane extraction units.
14
Batch Distillation.
 Batch distillation is characterized as a sys-tem that is difficult to design because compositions are changingcontinuouslywithtime.Thedesignofabatchdistillationcolumn
Received:
 June 26, 2011
Revised:
 October 15, 2011
 
5127
 dx.doi.org/10.1021/ef200935g |
Energy Fuels
 2011, 25,
 5126–5137
Energy & Fuels
ARTICLE
is much more complex in comparison with that of a continuousdistillation column as it requires consideration of unsteady-state behavior.Thecomplexityoftheproblemincreaseswiththenum- ber ofcomponentsinmulticomponent systems.
15
Diwekaretal.
16
presented optimization approaches using the shortcut methodfortheoptimaldesignofsingle-andmultiple-fractionbatchcolumnsoperating under constant reflux and variable reflux conditions.Tapp et al.
17
developed experimental method for obtaining dis-tillationcolumnconcentrationprofilesatfiniterefluxusingabatchapparatus. Stewart et al.
18
investigated a theoretical and experi-mentalstudy ofthe effectofcertain designvariablesonthe degreeof separation obtainable in multicomponent batch distillation.Luyben
19
investigated the effects of both design and operatingparameters by using digital simulation, number of trays, reflux ratio (bothfixed and variable), initialstill charge, relative volatility,and product purity for multicomponent batch distillation.
Objectives.
 In this study, the effect of hydrocarbon solventinjection on TEG purity in water + TEG system was investigated both experimentally and theoretically. Experiments were con-ductedinabatchtraycolumnundertotalandnorefluxoperatingconditions and various concentrations of solvents. The effect of isooctaneandtolueneadditiontoaTEG+watersystemonTEGpurity in the bottom product and TEG loss in the top product were compared. The concentration profiles of water and TEG inreboiler were determined. The modeling results were validated by the experimental data, and a good agreement was observed between them.
EXPERIMENTAL SECTION
Materials.
 The specification of materials used in experiments isreported in Table 1. Chemicals were used without further purification.
Apparatus and Procedure.
 In this study, experiments wereconducted in a batch distillation column (see Figure 1). As seen, thecolumnconsistsoftwentytrays,atotalcondenser,andreboiler.Samples were taken from the reboiler in 5 min intervals. Different operating con-ditions and concentrations of water and solvents were considered todetermine the effect of them on TEG purity. The specification of thiscolumn is reported in Table 2.In order to gain a deep insight into conducting experiments, somesamples were taken from the feed streamline to the stripping column of Farashband gas re
󿬁
nery (located in Iran) and analyzed by Karl FischerTitrator (Mettler Toledo, DL31). The analyzing results showed that the water content of rich glycol was between 7 and 10 wt %; therefore three water concentrations of 7, 10, and 15 wt % were selected for the experi-ments. Furthermore, several experiments were conducted in order torecognizethebestsolventconcentration,and0
0.05,0.1,and0.15wt%solvent concentrations were chosen inthe end. It wasworth mentioningthat a sudden blast was observed at a solvent concentration more than0.3 wt %, and solvent did not show its e
ff 
ect at concentration less than0.05%. Thus, the minimum solvent concentration of 0.05 wt % wasconsidered during the experiments. Moreover, the e
ff 
ect of re
󿬂
ux ratioon TEG purity was investigated, and two re
󿬂
ux operating conditionsincluding total re
󿬂
ux and no re
󿬂
ux were thoroughly investigated. A known amount of water, TEG, and solvents was mixed andintroduced into the reboiler. According to the controlling section of thecolumn,thecolumnwasstartedupandthemixturetook40
60minto boil in the reboiler based on the composition distribution of com-ponents. When the top tray temperature reached steady state condition(the measurement uncertainty of the thermometer which was used inexperimentswas
(
0.1
C),samplingwasperformedfor5,10,15,20,25,30, 40, 50, and 60 min. Next, the water content of bottom samples was determined via Karl Fischer titrator with the measuring range of 50 ppm to 100% water (Figure 2) and the hydrocarbon content of thetopsampleswasdeterminedviatotalorganiccarbon(TOC)(Figure3a)
Table 1. Speci
󿬁
cation of Materials Used in Experiments
chemicalcomponent purity water content supplierTEG >99% <0.3% Arak Petrochemical Compantoluene, isooctane >99% <0.01% Merck Compandistillated water Shiraz Universit
Figure 1.
 Batch distillation tray column used during the experiments.
Table 2. Speci
󿬁
cation of Tray Column
outer diameter 8 cmnumber of trays 20pressure (condenser) 101.3 kPa
 8 cm WHS 1.3 cm WLS 2.36 cm
B
 3587.2 kJ/hinitial weight fractions(TEG, isooctane/toluene, water)0.85, 0.001, 0.150.899, 0.001, 0.10.929, 0.001, 0.070.8485, 0.0015, 0.150.8985, 0.0015, 0.10.9285, 0.0015, 0.070.8495, 0.0005, 0.150.8995, 0.0005, 0.10.9295, 0.0005, 0.07
 
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 dx.doi.org/10.1021/ef200935g |
Energy Fuels
 2011, 25,
 5126–5137
Energy & Fuels
ARTICLE
andanalyzedbyVarianModel3800GC(Figure3b)fordetectingspecialhydrocarbons.ThecolumnoftheGCwas0.635cmindiameterand2min height packed by Porapak Q. Helium was used as a carrier gas, and a
󿬂
ame ionization detector (FID) was applied to obtain the compositionof hydrocarbons.
MATHEMATICAL MODELING
 A scheme of the batch distillation tray column is shown inFigure 4. Three basic assumptions are usually made in dynamicstudies of nonreactive systems:
20
 Themolarvaporholdupisnegligibleincomparisonwiththemolar liquid holdup.
 Vapor and liquid on and leaving each tray are perfectly mixed, and the liquid on a tray has a concentration equal tothat of the liquid leaving that tray.
 The theoretical equilibrium compositions are corrected formixing e
ff 
ects,
 󿬂
ow con
󿬁
guration, and mass transfer limita-tions by introducing tray e
ciency (tray e
ciency of the batch column considered in this study was 60%).
MASS AND ENERGY BALANCE EQUATIONS
Thegoverningequationsarecomposedofthetotaland partialmaterial balances andthe energybalance forthereboiler,thetrays(
󿬁
rst, intermediate, and top trays), and the total condenser. In thefollowing equations, the usual assumption was made where vapormolar hold-up was negligible compared with liquid molar hold-up whichmaygiveerroneousresultsforveryhighcolumnpressures.
21
For the reboiler, total and component material balances andthe energy balance are as follows (subscript B):d
 M 
B
d
 ¼
 L
1
 
 V 
B
 ð
1
Þ
d
ð
 M 
B
x
B,
 j
Þ
d
 ¼
 L
1
x
1,
 j
 
 V 
B
 y
B,
 j
 j
 ¼
 1,
:::
 ,
 N 
c
 ð
2
Þ
andd
ð
 M 
B
L,B
Þ
d
 ¼
 L
1
L,1
 
 V 
B
 V,B
 þ
 
B
 ð
3
Þ
The
 󿬁
rst tray (subscript 1):d
 M 
1
d
 ¼
 
B
 þ
 L
2
 
 V 
1
 
 L
1
 ð
4
Þ
Figure2.
 KarlFischerTitratorfordeterminingthewater contentofthe bottom product.
Figure 3.
 (a) TOC for determing the HC content of the top product.(b) GC for analyzing the HC content of the top product.
Figure 4.
 Scheme of the batch distillation tray column.

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