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D. Greaves, J. Boxall, J. Mulligan, E. Sloan, C. Koh (2008)
Hydrate formation from high water content-crude oil emulsionsChemical Engineering Science, 63
E. Sloan, C. Koh (1990)
Clathrate hydrates of natural gases
D. Turner, K. Miller, E. Sloan (2009)
Methane hydrate formation and an inward growing shell model in water-in-oil dispersionsChemical Engineering Science, 64
S. Davies, J. Lachance, E. Sloan, C. Koh (2010)
High-Pressure Differential Scanning Calorimetry Measurements of the Mass Transfer Resistance across a Methane Hydrate Film as a Function of Time and SubcoolingIndustrial & Engineering Chemistry Research, 49
M. Garfinkle (2000)
The thermodynamic natural path in chemical reaction kineticsDiscrete Dynamics in Nature and Society, 4
Changsheng Xiang, B. Peng, Huang Liu, Changyu Sun, Guangjin Chen, Baojiang Sun (2013)
Hydrate Formation/Dissociation in (Natural Gas + Water + Diesel Oil) Emulsion SystemsEnergies, 6
A. Mandal, A. Samanta, A. Bera, K. Ojha (2010)
Characterization of Oil-Water Emulsion and Its Use in Enhanced Oil RecoveryIndustrial & Engineering Chemistry Research, 49
Himangshu Kakati, Shranish Kar, A. Mandal, S. Laik (2014)
Methane Hydrate Formation and Dissociation in Oil-in-Water EmulsionEnergy & Fuels, 28
Liang Mu, Shi Li, Qinglan Ma, Ke Zhang, Changyu Sun, Guangjin Chen, Bei Liu, Lan-ying Yang (2014)
Experimental and modeling investigation of kinetics of methane gas hydrate formation in water-in-oil emulsionFluid Phase Equilibria, 362
ED Sloan (2007)
10.1201/9781420008494
Shiva Talatori, T. Barth (2011)
Rate of hydrate formation in crude oil/gas/water emulsions with different water cutsJournal of Petroleum Science and Engineering, 80
A. Mandal, Shranish Kar, S. Kumar (2016)
The Synergistic Effect of a Mixed Surfactant (Tween 80 and SDBS) on Wettability Alteration of the Oil Wet Quartz SurfaceJournal of Dispersion Science and Technology, 37
A. Sinquin, X. Bredzinsky, V. Beunat (2001)
Kinetic of Hydrates Formation: Influence of Crude Oils
Hadi Roosta, Shahin Khosharay, F. Varaminian (2013)
Experimental study of methane hydrate formation kinetics with or without additives and modeling based on chemical affinityEnergy Conversion and Management, 76
H. Moradpour, A. Chapoy, B. Tohidi (2011)
Phase Inversion in Water–Oil Emulsions with and without Gas HydratesEnergy & Fuels, 25
A. Mohammadi, Hongyan Ji, R. Burgass, Ali Ali, B. Tohidi (2006)
Gas Hydrates in Oil SystemsEurosurveillance
Pet. Sci. (2016) 13:489–495 DOI 10.1007/s12182-016-0108-3 ORIGINAL PAPER Experimental and modeling study of kinetics for methane hydrate formation in a crude oil-in-water emulsion 1 1 1 1 • • • Shranish Kar Himangshu Kakati Ajay Mandal Sukumar Laik Received: 22 December 2015 / Published online: 12 July 2016 The Author(s) 2016. This article is published with open access at Springerlink.com Abstract A low-viscosity emulsion of crude oil in water 1 Introduction can be believed to be the bulk of a flow regime in a pipeline. To differentiate which crude oil would and which Way back in the 1930s, natural gas hydrates were discov- would not counter the blockage of flow due to gas hydrate ered in gas transmission lines, frequently at temperatures formation in flow channels, varying amount of crude oil in above the ice point. Many chloride salts, methanol, and water emulsion without any other extraneous additives has monoethylene glycol are considered for hydrate inhibition undergone methane gas hydrate formation in an autoclave in pipelines, but the hydrate problem in pipelines is still cell. Crude oil was able to thermodynamically inhibit the growing with the deep offshore production, increase in gas hydrate formation as observed from its hydrate stability water cuts, and existence of multicomponent flow. Uneco- zone. The normalized rate of hydrate formation in the nomic thermodynamic inhibitors have been replaced by low emulsion has been calculated from an illustrative chemical dosage hydrate inhibitors (LDHI). In the hydrocarbon affinity model, which showed a decrease in the methane industry, emulsions can be encountered in almost all phases consumption (decreased normalized rate constant) with an of oil and gas production, inside the reservoirs, well bores, increase in the oil content in the emulsion. Fourier trans- and well heads and in transportation through pipelines. form infrared spectroscopy (FTIR) of the emulsion and Irrespective of the amount of water in the emulsified sys- characteristic properties of the crude oil have been used to tem, hydrates could form in the emulsion at particular find the chemical component that could be pivotal in self- pressure and temperature conditions, which consequently inhibitory characteristic of the crude oil collected from leads to plugging of pipelines due to agglomeration of the Ankleshwar, India, against a situation of clogged flow due hydrate particles into a large mass (Greaves et al. 2008;Mu to formation of gas hydrate and establish flow assurance. et al. 2014). In more stable emulsions, there is a higher rate of hydrate formation as small droplets increase the surface area of contact between gas and water. In the oil-in-water Keywords Methane gas hydrates Organic inhibitors Chemical affinity model Normalized rate constant (O/W) emulsion, the large surface contact between water Asphaltenes and gas allows maximum mass transfer which increases the gas consumption rate (Douglas et al. 2009; Xiang et al. 2013). Talatori and Barth (2011) found that the nucleation time for methane gas hydrate formation depended inversely on the driving force, i.e., subcooling at a constant water cut and expectedly, the nucleation time decreased when the water cut increased at a constant temperature & Ajay Mandal From the solubility aspect, Xiang et al. (2013) suggested mandal_ajay@hotmail.com that the solubility of gas in emulsions decreased with an Department of Petroleum Engineering, Indian School of increase in the water cut at a given pressure. Beyond these Mines, Dhanbad 826004, India physical parameters, Mohammadi et al. (2006) indicated that inherent natural components in crude oil resisted Edited by Yan-Hua Sun 123 490 Pet. Sci. (2016) 13:489–495 agglomeration and inhibited the hydrate growth by coating 2.2 Apparatus them during hydrate formation in the water-in-oil (W/O) emulsions. The details of apparatus used in this study were mentioned Crude oil as a whole is composed of saturates, aromat- in our previous work (Kakati et al. 2014). Briefly, the high pressure autoclave consisted of a constant volume hydrate ics, resins, and asphaltenes. Sinquin et al. (2001) founded that asphaltenes and organic acids have played a major role cell with a pressure rating up to 20.68 MPa. A stethoscope camera, thermocouples, and a digital pressure gauge were in the emulsion stability and, as a consequence, in hydrate agglomeration and plugging. They observed delayed for- incorporated into the cell. The cell was equipped with a PT100 probe to measure the temperature inside the cell, mation and smooth crystallization of hydrates in crude oil of higher asphaltene content and rapid crystallization of and the uncertainty of the measurement was ±0.05 C. A methane hydrates in crude oil of lower asphaltene content. magnetic stirrer with adjustable rotation speed (up to Davies et al. (2010) reported the mass transfer rates across 1000 rpm) was used to agitate the test fluid in the cell. The methane hydrate films grown at hydrocarbon-water inter- cell was dipped in a thermostatic bath filled with a ther- faces in a quiescent system, as a function of subcooling and mostatic fluid (a mixture of 85 % water and 15 % glycol) the age of the film. Hossein et al. (2011) showed the to control its temperature within the range of -10 to 60 C. Every experiment was repeated three times to check the electrical repulsive force in an O/W emulsion and the steric effect in a W/O emulsion to be the mechanism behind reproducibility. It has been found that pressure variation was within ±0.1 MPa. emulsion stabilization by asphaltenes. In the case of gas hydrates, the wax would reduce the subcooling by acting as nucleation sites and the crude oil of increased lighter 2.3 Methods fractions would increase the dissociation temperature of gas hydrates. Mu et al. (2014) studied the inversion of an 2.3.1 Preparation of emulsion emulsion with a particle analyzer and a conductivity meter during dissociation of methane hydrates. An emulsion was prepared by stirring, not just to mix the An O/W emulsion was used in this study to investigate liquids but to disperse one of them in the other. A 4-blade the effect of crude oil on thermodynamics and kinetics of impeller stirrer, (REMI RQ 20 PLUS), was used to prepare the emulsion at 2000–2500 rpm so that the oil was properly methane hydrate formation. The equilibrium pressure and temperature of hydrate formation in the emulsion were dispersed in the water for various water cuts. After mixing for 5 h, the mixture was allowed to settle in a separating measured and compared with respect to pure water system. The rate of hydrate formation has been studied by a funnel to separate the emulsion for study from the heavier or waxy components which did not disperse in the con- chemical affinity model (Roosta et al. 2013). tinuous phase, i.e., water. After separating the emulsion from the separating funnel its hydrocarbon content was 2 Experimental measured in parts per million (ppm) using an Infracal TOG/TPH analyzer (Wilks) to detail the actual oil content 2.1 Material in the emulsion. Three O/W emulsion samples with the oil content of 870, 1880, 3560 ppm were prepared for the hydrate study. All the experiments were performed with 99.99 % pure methane gas (collected from the Chemtron Science Labo- 2.3.2 Procedure ratory, Navi Mumbai, India) and double-distilled water with a dynamic viscosity of 1.002 cP and specific con- ductance (j)of2 lS/cm (approximately) at 25 C. Crude Our previous work described the experimental procedure in oil was collected from the Ankleshwar field, India. All detail (Kakati et al. 2014). The cell was filled with 120 mL materials were used with no further purification or modi- of the prepared emulsion and methane gas was charged up fication of their properties. The physicochemical charac- to 11 MPa at 20 C. The cell was then cooled in steps of teristics of crude oil are given in Table 1. 2 C per hour in the programmable bath and allowed to Table 1 Physicochemical characteristics of crude oil Density at 15.5 C, Specific gravity API gravity at Viscosity at Acid number, Pour point, kg/m at 15.5 C 15.5 C, API 30 C, cP mg KOH/g C 855.60 856.10 35.77 525 0.038 18 123 Pet. Sci. (2016) 13:489–495 491 dwell for 1 h at each step to equilibrate. To observe the ester functional group present instead of carboxylic acid to dissociation of methane hydrates, the entire cell was heated justify the low acid number per gram of KOH for crude oil slowly at 1 C/h step wise so that the equilibrium of the observed by Kakati et al. (2014). A weak band known as -1 system was not disturbed. overtones showing at around 2040 cm and out of -1 To measure the inhibition time or induction time of plane—‘‘oop’’ bands from 900–675 cm suggest aromatic hydrate formation, the cell was cooled from a pressure and groups. In addition to that, carbon double bonding is con- -1 temperature condition (determined by the hydrate stability firmed from a sharp peak at 1638 cm due to –C=C zone (HSZ) experiment) where hydrate does not exist, to stretch. Furthermore, FTIR of crude oil (Mandal et al. -1 that temperature (hydrate formation temperature) where 2015) and Fig. 1 show a peak at 1410 cm which is the hydrate forms. The time taken between start of experiment effect of –C–C stretching in rings of aromatic components. (t ) and hydrate onset time (t ) is the induction time of SARA analysis of the crude oil had shown an appreciable s o hydrate formation. weight percent of aromatics and asphaltenes (Kakati et al. 2014) which augments the FTIR interpretation done here. -1 2.3.3 Fourier transform infrared spectroscopy (FTIR) A sharp peak at 1110–1000 cm represents –C–N stretch in aliphatic amines to supplement the band for N–H at -1 A Perkin-Elmer Spectrum Two, FT-IR instrument (USA) 3400–3250 cm . was used to obtain the spectra of the O/W emulsions Out of a wide range of highly complex chemical com- -1 between 400 and 4000 cm wavelength. The IR spectrum pounds, such as alkanes, aromatics, cycloalkanes, resins, of the pellet was recorded and 100 scans were collected. and asphaltenes present in the crude oil, asphaltenes, The transmittance versus wavenumber plot for the O/W waxes, and resins are believed to stabilize the O/W emul- emulsions with the oil content of 1880 and 3560 ppm, sion (Greaves et al. 2008). These act as extraneous mate- respectively, are shown in Fig. 1. The FTIR spectroscopy rials in the interfacial film of oil and water to suppress the of the crude oil has been described in our previous work by mechanism for emulsion break down and to stabilize the Mandal et al. (2015). interface (Mandal et al. 2010). On investigating the FTIR spectroscopic plot from -1 wavenumber of 4000 to 500 cm , the alkyl group was observed to be present from –C–H stretching bands in 2862 3 Results and discussion -1 and 2931 cm . This band is relevant in most organic molecules. The presence of –O–H can be anticipated from Crude oil thermodynamically inhibits the formation of -1 a broad strong band at 3430 cm . –O–H and –C–O stretch methane gas hydrate as observed in our previous work by -1 around 1369 cm indicates the presence of the carbonyl Kakati et al. (2014). group which might be due to the carboxylic acid present in the crude oil. On the other hand, this could be indicating an 3.1 Comparison of hydrate formation curve The curves of methane gas hydrate formation in O/W emulsions of different oil contents are shown with pure O/W emulsion (1880 ppm oil) 110 water in Fig. 2 and the corresponding temperature and O/W emulsion (3560 ppm oil) pressure drops are listed in Table 2. Table 2 shows that the formation temperature shifts to lower values in the O/W emulsion with respect to pure water. The pressure drop during hydrate formation in pure water is more than the corresponding pressure drop during hydrate formation in the O/W emulsion. 80 3.2 Comparison of hydrate dissociation curve The dissociation curves of gas hydrate in O/W emulsions of different oil contents are shown along with pure water in Fig. 3. In the O/W emulsion, the hydrate dissociation curve 4000 3000 2000 1000 0 moves to higher pressure for a given temperature as seen in Wavenumber, cm Fig. 3. It is important to observe here that the O/W emulsion Fig. 1 FTIR plot of transmittance versus wavelength for the O/W has shifted the equilibrium temperature substantially in the emulsions of oil content of 1880 and 3560 ppm Transmittance, % 492 Pet. Sci. (2016) 13:489–495 size of these chemicals. The hydrogen bonding of inhibitor 11.8 with water may be hindered with an increase in the inhi- 11.4 bitor size. Therefore, water molecules may not be sub- stantially restricted by the inhibitor of larger sizes to form 11.0 hydrate cages. 10.6 3.3 Chemical affinity modeling for kinetics 10.2 of hydrate formation 9.8 The chemical affinity model (Roosta et al. 2013) is one of Pure water the thermodynamic-based approaches that can be applied O/W emulsion (870 ppm oil) 9.4 for hydrate formation kinetics. This model is independent O/W emulsion (1880 ppm oil) O/W emulsion (3560 ppm oil) of the parameters such as heat and mass transfer coeffi- 9.0 cients which are difficult to determine and only macro- 282 284 286 288 290 292 294 scopic properties such as pressure and temperature are Temperature, K needed for this model. When bulk techniques such as gas Fig. 2 Temperature versus pressure profiles of methane hydrate uptake measurements in closed isothermal systems are formation in pure water and O/W emulsions used for determining the kinetics of hydrate formation, a gradual conversion of gas to hydrate is normally observed, higher pressure region or has shifted the equilibrium suggesting a relatively homogeneous process that could be pressure to a higher region thus indicating a similar action modeled using a kinetics parameter. The chemical affinity which can be due to their larger molecular structures. The approach has been used for description of chemical reac- inhibition power of these samples is due to the affinity of tions in isothermal–isochoric systems. So, it is applicable the oxygen atoms of the -O–H group for neighboring for systems with complex additives like crude oil. water molecules. Thus, water molecules are prevented For a chemical reaction, the chemical affinity (A )isa from forming hydrogen-bonded cages to capture gaseous generalized driving force which is given by the following guest molecules. It may be speculated that the extent to expression suggested by Roosta et al. (2013): form hydrogen bonds with water molecules depend on the Table 2 Hydrate formation Test sample Formation pressure, MPa Formation temperature, K Pressure drop, MPa parameters for the O/W emulsion (3560 ppm oil) and Pure water 10.03 285.27 0.93 pure water O/W emulsion 10.72 283.96 0.63 11.5 11.0 10.5 10.0 9.5 9.0 Pure water O/W emulsion (870 ppm oil) 8.5 O/W emulsion (1880 ppm oil) O/W emulsion (3560 ppm oil) 8.0 287 288 289 290 291 Temperature, K Fig. 3 Temperature versus pressure profiles of methane hydrate dissociation in the O/W emulsions and pure water Pressure, MPa Pressure, MPa Pet. Sci. (2016) 13:489–495 493 n n n ci o i A ¼ A RTlnðQ Þ; ð1Þ i i b ¼ ¼ ; ð8Þ n n n cf o f where A is the affinity of the components at their standard -1 where subscript o stands for the initial condition and sub- states, J mol , and A is only a function of temperature; Q script f for the equilibrium condition. is the activity ratio for the ith component. At the equilib- rium condition A = 0so A ¼ RTlnðKÞ in which K P V P V i o f n ¼ & n ¼ ; ð9Þ o f denotes the thermodynamic equilibrium constant. Substi- Z RT Z RT o f tuting A into Eq. (1), A can be written as, where P and P are the initial and equilibrium pressures, o f respectively. Substituting n and n into Eq. (8) and the o f A ¼RTlnðb Þ where, b ¼ : ð2Þ Q Q i i expression for b in Eq. (2), A can be calculated from Experimentally, it has been established that, the affinity P P o i A n i ci Z Z o i decay rate A is inversely proportional to time (Garfinkle ¼ ln ¼ ln : ð10Þ T ;V P P o f RT n cf Z Z 2000) which can be expressed as o f 1 Further substituting Eq. (10) into Eq. (8) the following A ¼ A þ C ; ð3Þ T ;V r 1 equation can be obtained: P P o i RT where A is the proportionality constant and denotes the n t t r ci Z Z i i o i ¼ ¼ ln exp 1 ; ð11Þ P P o f affinity rate constant; and C is any arbitrary constant. 1 n t t cf K K Z Z o f Further for a closed, fixed volume, and constant tempera- where is the kinetic parameter of this model. The ture system, the affinity decay rate can be expressed as RT absolute value of slope can be a normalized rate follows: RT constant. So, the value of this slope can be employed for oA A ¼ : ð4Þ investigating the effects of additives in the system on T ;V ot T ;V ci hydrate formation kinetics. Plotting ln versus cf Again at the equilibrium condition, the affinity decay t t i i ln exp 1 a straight line through origin with a rate is zero. Thus, considering the time needed for the t t K K system to reach the equilibrium to be t , Eq. (3) can be K slope of is obtained. Figure 4 shows the plot for all the RT expressed as three concentrations of emulsions and the linear trend line gives the slope for each of them at various stages. 1 1 A ¼ A : ð5Þ T ;V r In Fig. 4, it is observed that the slope of curves changes t t with a change in oil concentration in the O/W emulsion. From Eqs. (4) and (5), one obtains the following equation: oA 1 1 0.8 ¼A : ð6Þ ot t t T ;V y=8.0136x 0.6 Upon integrating Eq. (6) from the initial time t to the time required reaching the equilibrium t y=1.6805x A A t t i r i i 0.4 y=0.8941x ¼ ln exp 1 : ð7Þ RT RT t t K K Equation (7) can be used to correlate the parameters of 0.2 the chemical affinity model with experimental values ver- sus time. Even though the hydrate formation process is not O/W emulsion (870 ppm oil) O/W emulsion (1880 ppm oil) 0.0 a chemical reaction, A at different conditions can be O/W emulsion (3560 ppm oil) measured, by considering the extent of the hydrate for- 0.00 0.10 0.20 0.30 0.40 0.50 0.60 mation process with time in terms of pressure of gas in -ln[(t /t )exp(1-t /t )] each elapsed time. Instead of activity, the amount of gas i K i K consumed n during hydrate formation is used to show the n t t ci i i Fig. 4 ln versus ln exp 1 dimensionless plot for extent of hydrate formation. Hence, Eq. (2) is expressed in ncf tK tK the ratio, finding the rate constant RT -ln(n /n ) ci cf 494 Pet. Sci. (2016) 13:489–495 Thus, from the basic rate equation (Sloan and Koh 2007), 4 Conclusion the rate of consumption of gas can be written as From the formation and dissociation of methane hydrates Rate of consumption ¼ rate constant driving force: in the O/W emulsion, a thermodynamic inhibition was ð12Þ observed by crude oil due to a reduction of the chemical Keeping the driving force constant, the rate of consumption potential of water. The equilibrium P–T curve shifted decreases as the rate constant decreases. Thus, from the toward a higher pressure and lower temperature zone when normalized rate constant listed in Table 3, we see that there the concentration of oil in the emulsion increased. It was must be a decrease in gas consumption which was exper- inferred from the FTIR that there was less chance of the imentally seen in our previous work by Kakati et al. (2014). presence of carboxylic acid groups (or if present not in a In Fig. 5, a change in the slope of the curve is observed detectable amount). This was also suggested from the low with respect to time for a sample. This is due to different acid number of crude oil. The functional groups present rates of hydrate formation which gives different reaction were observed from the FTIR which showed –OH, aro- rates and hence different rate constants. Table 3 shows the matic, and amide groups. From this and satisfactory sta- methane hydrate formation rates in O/W emulsions. Ini- bility of the O/W emulsion, a consensus was that the tially the formation rate of hydrate is high, and then it surface active asphaltenes might be responsible for such decreases with time. organic inhibition. As a very small lag time was observed during the kinetics study, the emulsion was inferred not to be a kinetic inhibitor. The chemical affinity model showed Table 3 Rate constant of the formation of methane hydrates in O/W a decrease in the normalized rate constant for gas con- emulsions sumption as the percentage of oil increased. Oil content in the Rate constant Normalized rate O/W emulsion, ppm constant Acknowledgments We gratefully acknowledge the financial assis- tance provided by University Grants Commission, New Delhi, India, 870 K 10.53950 8.0136 under Special Assistance Program (SAP) to the Department of Pet- K 3.533986 roleum Engineering, Indian School of Mines, Dhanbad, India. K 8.474374 1881 K 2.644888 1.6805 Open Access This article is distributed under the terms of the Creative Commons Attribution 4.0 International License (http://crea K 1.220637 tivecommons.org/licenses/by/4.0/), which permits unrestricted use, K 2.241379 distribution, and reproduction in any medium, provided you give 3560 K 2.242573 0.8941 31 appropriate credit to the original author(s) and the source, provide a link to the Creative Commons license, and indicate if changes were K 0.676824 made. K 2.242573 0.6 Kinetic constants for the O/W emulsion (3560 ppm oil) References Davies SR, Lachance JW, Sloan ED, Koh CA. High-pressure 0.5 differential scanning calorimetry measurements of the mass transfer resistance across a methane hydrate film as a function of 0.4 time and subcooling. Ind Eng Chem Res. 2010;49(23):12319–26. doi:10.1021/ie1017173. 0.3 Douglas T, Miller KT, Sloan ED. Methane hydrate formation and an inward growing shell model in water-in-oil dispersions. 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Petroleum Science – Springer Journals
Published: Jul 12, 2016
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