Experimental Setups for Studying the Compatibility of Crude Oil

Article pubs.acs.org/EF

Experimental Setups for Studying the Compatibility of Crude Oil Blends under Dynamic Conditions Silvano Rodríguez,†,‡ Jorge Ancheyta,*,† Roque Guzmán,†,‡ and Fernando Trejo‡ †

Instituto Mexicano del Petróleo, Eje Central Lázaro Cárdenas Norte 152, Colonia San Bartolo Atepehuacan, Mexico City 07730, Mexico ‡ Instituto Politécnico Nacional, CICATA-Legaria, Legaria 694, Col. Irrigación, Mexico City 11500, Mexico ABSTRACT: Blending of different crude oils is currently carried out in the petroleum industry. However, under certain process conditions, i.e., pressure, temperature, flow regime, composition, etc., asphaltene precipitation and plugging of pipelines and process equipment commonly occur, which cause production shutdowns; therefore, special cleaning programs need to be developed. To avoid these problems, it is first necessary to evaluate the compatibility of crude oil blends through a study of asphaltene stability. Most of the available tests are focused on analyzing crude oils under standard conditions, i.e., temperature, pressure, solvent/oil ratio, or static testing; however, studies at dynamic conditions are scarce. Dynamic testing is a more representative approach to correlate experimental information with data of transportation of crude oils, where pressure, temperature, and flow regimes influence crude oil stability and compatibility. In this work, the literature reports of dynamic experimental setups are summarized and analyzed, whereby asphaltene deposition and precipitation are typically studied.

1. INTRODUCTION

It is considered that asphaltenes are dispersed in crude oils with resins around them as natural peptizers, with saturates and aromatics constituting a colloidal system.27−31 Figure 2 shows the different stages in asphaltene precipitation in which all saturate, aromatic, resin, and asphaltene (SARA) fractions are involved. When crude oil equilibrium is not altered, all oil fractions are in balance (Figure 2a); however, changes in the pressure, temperature, composition, flow, etc. modify the micellar structure, and resins unprotect asphaltenes (Figure 2b). Then, interactions between asphaltenes make the particle size grow, causing flocculation (Figure 2c), until equilibrium is no longer attained, and asphaltenes precipitate forming deposits (Figure 2d). Because of this, the production of crude oil is stopped sometimes for cleaning pipelines and process equipment.3,4,19,32−39 When crude oils with a similar nature are mixed, a blend without compatibility problems is normally expected; however, this is not always true, and tests to evaluate compatibility of blends through studying the asphaltene stability are necessary. This type of testing can also be used to study those unmixed crude oils known as self-incompatible that present insoluble asphaltenes, which, in combination with other inorganic solids as well as waxes, form sediments and can cause fouling in transport pipelines and some process equipment in the refinery, limiting its operation.40 Various authors have reported a number of experimental studies to evaluate asphaltene stability in pure crude oils or blends.41−47 Nevertheless, most of the tests are carried out at standard pressure, temperature, solvent/oil ratio, and static conditions, with the main objective of simulating the storage of crude oils. Reports of the behavior of crude oil blends under

A common approach frequently used in the petroleum industry to transport heavy crude oils is by dilution, i.e., blending heavy crude oils with lighter crude oils; however, for particular properties of the blend components under certain conditions of pressure, temperature, or flow regime, asphaltenes are prone to precipitate.1−7 Asphaltenes are aromatic in nature and rich in heteroatoms (S, N, and O) and metals, such as Fe, Ni, V, and Cu, among others.8−12 This fraction is defined in terms of its solubility; i.e., asphaltenes are soluble in aromatics and insoluble in low-molecular-weight alkanes.8,9,13−20 Asphaltenes are solid and semi-crystalline particles with an undefined boiling point,8,16 and different studies have been carried out to determine their molecular weight using various analytical tests, such as fluorescence depolarization and mass spectrometry, among others.21−23 A hypothetical asphaltene aggregate hierarchy has been proposed on the basis of results obtained via small-angle neutron scattering (SANS), smallangle X-ray scattering (SAXS), and X-ray diffraction (XRD), which follows the steps (Figure 1):24 (a) core aggregates (2 nm) through π−π stacking, (b) core aggregates forming medium aggregates (5−50 nm) by interactions with maltenes, oils, solvents, etc., and (c) core aggregates forming fractal aggregates (>100 nm) through diffusion- or reaction-limited cluster aggregation (DLCA or RLCA, respectively), which is independent of any media. Other authors reported that the asphaltene particle size ranged from 1 to 4 μm in crude oil samples diluted with heptane. However, the asphaltene particle size was independent of the heptane concentration.25 In other literature reports, it has been stated that the average size of asphaltene particles in toluene at very low concentrations was in the range of 12−22 nm and the addition of heptane gradually increased the particle size to above 1000 nm until asphaltenes are precipitated.26 © 2016 American Chemical Society

Received: July 11, 2016 Revised: September 5, 2016 Published: September 12, 2016 8216

DOI: 10.1021/acs.energyfuels.6b01698 Energy Fuels 2016, 30, 8216−8225

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Figure 1. Hypothetical representation of the hierarchy in asphaltene aggregates based on XRD, SAXS, and SANS data.24

Figure 2. Scheme of asphaltene precipitation stages: (a) equilibrium between chemical species, (b) equilibrium rupture, (c) flocculation, and (d) precipitation.

rates.48−50 The obtained results are mainly used in simulators of the database to predict asphaltene deposition during crude oil production.50−52 Dynamic systems operating with the pressure up to 7 MPa, the temperature ranging from 25 to 100 °C, the flow rate up to 0.1 m3/h, and heptane as the solvent have been reported elsewhere.53 Other dynamic systems with improved capacity have been used to study flow assurance at IFP Energies

dynamic conditions are scarce and necessary because they take into account all changes that streams undergo during transportation, such as pressure, temperature, flow rates, etc., as seen in Figure 3. There are some literature reports that are focused on flocculation and deposition of asphaltenes in dynamic experimental setups using steel pipes with a small amount of crude oil and varying pressures, temperatures, and flow 8217


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Figure 3. Typical scheme of crude oil transportation by heating (pipeline, ∼50 km × 12 in.).

Figure 4. Experimental setup of Wang et al.48

nouvelles,54 having the pipeline at a length of 140 m and inner diameter of 5 cm, operating from 0 to 50 °C and maximum pressure of 100 bar. A study focused on solvent addition to Athabasca bitumen mixtures containing water has been carried out by Amani et al.55 Solvents commonly have low densities and critical temperatures compared to water and bitumen, by which changes in the mixture phase behavior and water content in the bitumen-rich liquid phase were observed. Density predictions were acceptable at high pressures. Toluene addition to bitumen and water mixtures increased the solubility of water in the hydrocarbon-rich phase at a high temperature. Heavy crude oil transportation has become a critical problem worldwide, and much of its solution has been by dilution with lighter crude oils, which, in addition to reducing its viscosity and improving flow properties, prepares a better feed to refineries. With regard to the latter, nowadays, many refineries are processing more tight/shale oils blended with conventional crude oils; however, the high paraffin content of tight/shale oils greatly increases the potential impact of asphaltene precipitation and can have a significant negative impact on the refinery process, thus affecting product quality, unit reliability, and on-stream time.56

Rogel et al.57 analyzed several paraffinic crude oils and found the presence of asphaltenes in the precipitate as separated by filtration−centrifugation. Precipitated asphaltenes were the least insoluble asphaltenes, by which low solvent power of maltenes plays an important role. In addition, asphaltenes from paraffinic crude oils may be present in deposits along with waxes. For these reasons, the use of dynamic systems that properly simulate the transport of crude oils and blends is extremely important to identify those incompatible mixtures. In this study, different methodologies (experimental loops) reported in the literature to study asphaltene stability in crude oils or blends under dynamic conditions are summarized and analyzed.

2. EXPERIMENTAL SETUPS TO STUDY THE DYNAMIC COMPATIBILITY OF BLENDS OF CRUDE OILS It has been previously commented that experimental studies in pipelines under dynamic conditions of flow for asphaltene deposition in blends of crude oils are limited. Despite this, the few reported dynamic experimental setups are described and analyzed in the following sections. 2.1. Experimental Setup of Wang et al.48 Asphaltene precipitation from three crude oils was studied using linear alkanes (n-C5, n-C7, n-C10, and n-C15) at a constant temperature of 60 °C according to Wang et al.50 in a dynamic setup, as shown in Figure 4. In 8218


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Figure 5. Experimental setup of Broseta et al.49

Figure 6. Experimental setup of Salimi et al.50 2.2. Experimental Setup of Broseta et al.49 Figure 5 shows the experimental setup used by Broseta et al.49 Asphaltene precipitation and deposition rates are measured by pressure drop in a stainless-steel capillary tube having 0.5 mm of inner diameter and 15 m of length. The liquid can be injected at constant flow rate and specific temperature, pressure, and composition that is varied by changing the flow of liquids from 0.1 to 10 mL/min, whereas the temperature is controlled by immersion of the experimental loop in sand. Filters with 100 μm of pore diameter avoid plugging of the capillary tube. The pressure is also controlled with a regulator at the pipe exit, while asphaltene deposition enhances the pressure drop through the experimental loop. Asphaltene deposition was studied using a blend of crude oil, xylene, and heptane. It was found that the asphaltene

this loop, the deposition rate of asphaltenes is measured as the pressure drop that the crude oil undergoes through a stainless-steel capillary tube having 0.5 mm of inner diameter and 16−32 m of length. The temperature was controlled by immersion of the loop in water. The crude oil was injected using a pair of high-pressure pumps, in which the flow rate is adjusted to meet the crude oil/solvent ratio in each experiment. In this experimental setup, the flow rate can reach up to 200 mL/h. The pressure is controlled with a regulator at the pipe exit. The main conclusions of this report indicated that the flow rate and length of the pipe did not influence asphaltene deposition. The amount of precipitated asphaltenes increased when the crude oil/ solvent ratio diminished. 8219


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Figure 7. Experimental setup of Alboudwarej et al.53 flocculation point in the experimental loop was the same as that reported in conventional methods employing light transmittance, which is not adequate for low-asphaltene-content samples. The experimental loop allowed for measuring asphaltene deposition from test fluids containing 0.04 wt % asphaltenes. 2.3. Experimental Setup of Salimi et al.50 The experimental loop designed by Salimi et al.50 is depicted in Figure 6. They used an Iranian crude oil to evaluate the asphaltene deposition. Briefly, the experimental setup is made of a coiled-shape stainless-steel pipe with 3.74 mm of inner diameter and 1 m of length immersed in a heating bath. A number of pressure and temperature sensors are placed in the loop. The test fluid was a blend of crude oil and heptane previously prepared and heated before pumping inside the loop at different flow rates. After an experimental run, the tube is washed with heptane to remove non-asphaltenic materials. Then, toluene is used to remove asphaltenes deposited in tube walls, whereas the solvent is evaporated to obtain a solid residue, which is further washed with heptane, filtered, and refluxed with heptane for 2 h. The solids are dried and weighed to determine the asphaltene mass. The amount of asphaltene deposited in the loop was reported to vary inversely proportional to the flow rate and directly proportional to the asphaltene concentration in the test liquid and temperature in the tube walls. 2.4. Experimental Setup of Alboudwarej et al.53 Asphaltene deposition from Athabasca bitumen was studied by Alboudwarej et al.53 In this experimental loop (Figure 7), heptane was used to precipitate asphaltenes at different temperatures, pressures, and flow rates. The bitumen/heptane ratio was adjusted by pumping individually both bitumen and heptane. This loop is built with a tube with 19 mm of inner diameter, and it allows following asphaltene deposition by X-ray tomography [X-ray computerized axial tomography (CAT) scanner], taking images periodically from the cross-

section. In addition, a section of the tube can be separated from the loop for visual inspection and analysis of the solid deposits. It is also possible to study the asphaltene deposition in tubes made of different materials, such as stainless steel, iron, or aluminum. The flow rate can be varied up to 0.1 m3/h, while the maximum pressure, temperature, and heptane/bitumen ratio can reach 7 MPa, 100 °C, and 4 (wt/wt), respectively. Not only can heptane be used as the solvent, but also other solvents are readily used as well. Reversibility on asphaltene precipitation by redissolving them in bitumen was found. The influence of material of tube walls on asphaltene precipitation was negligible. Thus, the experimental loop was potentially useful in asphaltene deposition studies by varying different operation conditions. 2.5. Experimental Setup of Peramanu et al.58 Peramanu et 58 al. determined the asphaltene precipitation onset point by measuring the pressure drop through a stainless-steel filter with a pore diameter of 60 μm in the loop shown in Figure 8. A blend of solvents (toluene and heptane) is used along with the bituminous feed, i.e., Athabasca and Cold Lake. The feedstock is heated and mixed previously before passing the filter. The asphaltene onset point is determined when the pressure drop increases because of solid deposits in the filter. The influence of the temperature between 60 and 120 °C and type of solvent (n-C7, n-C8, n-C10, and n-C12) was studied. During the tests, different additives were used, such as aromatics, hydrogen donors, heteroatomic compounds, and surfactants. It was observed that additives retarded the asphaltene precipitation as follows: aromatics, hydrogen donors < heteroatomic compounds < surfactants. 2.6. Experimental Setup of Jamialahmadi et al.59 Jamialahmadi et al.59 studied the asphaltene precipitation by measuring the heat-transfer coefficients and thermal resistance caused by solid deposits. The experimental loop shown in Figure 9 was used, in which 8220


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Figure 8. Experimental setup of Peramanu et al.58

Figure 9. Experimental setup of Jamialahmadi et al.59 possible to vary the operation parameters as follows: flow rate (v), 0.35−2 m/s; heat flux density (q), 25−86 kW/m2; concentration of

the crude oil is pumped through an electrically heated stainless-steel tube having an inner diameter of 23.8 mm and length of 160 mm. It is 8221


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Energy & Fuels flocculated asphaltene, 0−5 kg/m3; bulk temperature (Tb), 70−85 °C; and surface temperature (Ts), 100−125 °C. Forced convection heat-transfer coefficients (αt) are calculated from changes in the surface temperature as a consequence of asphaltene deposits through the time along with the thermal resistance (RtA) and the mass of deposits in the inner tube wall (mtd) with the following equations: q αt = t Ts − Tb (1)

RAt =

1 1 − αt α0

mdt = ρd λdRAt

looking for experimental alternatives working under dynamic conditions to simulate transportation of crude oils and blends. 3.1. Comparison of Experimental Setups. The experimental setups aforementioned are used to study asphaltene precipitation through loops at different operation conditions. However, their sizes and shapes are variable, by which they are used under specific tests, as shown in Table 1. Commonly, to study asphaltene precipitation at low shear rates, a capillary tube is needed (0.25−3.74 mm of inner diameter), while to study flow assurance, a bigger diameter of pipes is required, as reported in the case of the Lyre loop, which properly simulates real operations in upstream and transport processes. Ranges of operating conditions (flow rate, pressure, temperature, test fluid, and n-alkane/oil maximum ratio) are shown in Table 2. It is observed that the fluids tested in the different loops include crude oils, blends of crude oils and bitumen, and solvents comprising n-alkanes from 5 to 15 carbon atoms. In general, each loop has been designed for a certain purpose, and all of them are useful for studying the deposition of asphaltenes. Of course, those of bigger size, higher range of operating conditions, and more infrastructure for sample characterization have more advantages over the rest. However, the results cannot be totally extrapolated to crude oil blends as a result of the complex nature of the real system. 3.2. Analysis of Variables. The effects of the type of solvent and operating conditions during studies of compatibility of blends of crude oil using the experimental setups previously described are summarized as follows. 3.2.1. Effect of the Solvent Type. Linear alkanes are used typically to precipitate asphaltenes from crude oils and to determine the asphaltene onset point, which is directly related to the crude oil stability. The higher the asphaltene stability in the crude oil, the higher the volume of required solvent. According to Peramanu et al.,58 more volume of solvent is required as its carbon number is increased, as shown in Figure 12 for Athabasca and Cold Lake bitumen at 80 °C. This was also demonstrated by Wang et al.,48 who carried out asphaltene precipitation tests using a light crude oil with American Petroleum Institute (API) gravity of 28.8° and solvents having 5−15 carbon atoms (crude oil “S” in Figure 12). 3.2.2. Effect of the Temperature. The temperature is one of the most important variables influencing the asphaltene precipitation. It is highly important to study its effect when the crude oil undergoes thermal changes during its transportation through pipelines. According to Salimi et al.,50 less asphaltene precipitation and deposition are observed at higher temperatures because they are kept soluble in the crude oil, as observed in Figure 13. Iranian crude oil rich in asphaltenes and heptane as the precipitant solvent were used. A similar conclusion was derived by Jamialahmadi et al.59 using the same crude oil but with pentane as the solvent. The higher the pentane/crude oil ratio, the higher the amount of precipitated asphaltenes, as shown in Figure 14. 3.2.3. Effect of the Flow Rate. Changes in flow regime from laminar to turbulent and vice versa are observed in crude oils when transporting through pipelines. Jamialahmadi et al.59 studied the effect of the flow rate in blends of crude oils using pentane as the solvent. Figure 15 shows the flow rate effect on the mass of asphaltene deposited at different times through the loop, shown in Figure 8. It was found that the flocculated asphaltene concentration was 3.5 kg/m3. Asphaltene precipitation and deposition decreased as the flow rate increased as a

(2) (3)

Density (ρd) and thermal conductivity (λd) of asphaltenes were considered to be 1100 kg/m3 and 0.75 W m−1 K−1, respectively. It was observed that asphaltene precipitation depends upon the flow rate, bulk and surface temperatures, and flocculated asphaltene concentration. The higher the flow rate, the lower the asphaltene deposition. The deposition rate was observed to be higher as the flocculated asphaltene concentration and surface temperature were also increased. 2.7. Multiphase Flow Assurance Innovation Centre (FACE) System to Flow Assurance Studies.60 An experimental loop with 50 m of length and 2.54 cm of inner diameter is used at the FACE. The FACE system can process a total volume of 35 L, pressure up to 100 bar, and temperature range from −10 to 50 °C. The flow rate can be changed using a pump system, which also allows for injection of the sample through several points in the loop. Figure 10 shows a schematic view of the FACE system.

Figure 10. FACE setup to flow assurance.60 2.8. Experimental Setup of IFP Energies nouvelles to Flow Assurance Studies.54 Flow assurance studies are carried out at IFP Energies nouvelles using an experimental loop (Lyre loop) with 140 m of length and 5 cm of inner diameter (Figure 11). The pressure can reach up to 100 bar, while the temperature is varied from 0 to 50 °C. This versatile system allows for studying the formation of deposits, such as asphaltenes or waxes, as well as gas hydrates. Separation of water−oil emulsions is also studied. The Lyre loop is commonly used to carry out studies focused on increasing the operation efficiency in upstream processes and crude transport avoiding pipe plugging.

3. RESULTS AND DISCUSSION The following sections discuss the results generated when studying the asphaltene deposition in the loops previously described, which work at dynamic conditions. It has to be highlighted that this information is important for those who need to conduct studies on asphaltene precipitation and are 8222


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Figure 11. Experimental IFP Energies nouvelles setup to flow assurance.54

Table 1. Characteristics of Experimental Setups for Asphaltene Deposition Tests under Dynamic Conditionsa dimension of test section

a

experimental setup

diameter (mm)

Wang et al.48 Broseta et al.49 Salimi et al.50 Alboudwarej et al.53 IFP Energies nouvelles (Lyre loop)54 Peramanu et al.58 Jamialahmadi et al.59 FACE60

0.51 (ID) 0.25 (ID) 3.74 (ID) 19.05 (OD) 50.8 (OD)

length (m)

material

detection or measurement technique

32 15 1

SS SS SS SS metallic SS SS metallic

pressure drop across a capillary tube pressure drop across a capillary tube washing method (weight of deposited asphaltenes) X-ray tomography particle size analyzer (FBRM probe) pressure drop across an in-line filter (60 μm) thermal resistance of the asphaltene deposit

140 (total)

23.8 (ID) 25.4 (OD)

0.16 50 (total)

SS, stainless steel; ID, internal diameter; and OD, outside diameter.

Table 2. Operation Conditions in Experimental Setups for Asphaltene Deposition Tests under Dynamic Conditions maximum operating conditions experimental setup

flow rate (L/h)

Wang et al.48 Broseta et al.49 Salimi et al.50 Alboudwarej et al.53 IFP Energies nouvelles (Lyre loop)54 Peramanu et al.58 Jamialahmadi et al.59 FACE60

0.005 0.6 13 100 12 1600

pressure (bar)

temperature (°C)

350 70 100 5

60 50 80 100 50 120 85

result of asphaltene particles not flocculating, so that deposition is avoided.

n-alkane/oil maximum ratio

test fluid crude oil/n-C7, n-C10, and n-C15 crude oil/xylene/n-C7 crude oil/n-C7 bitumen/n-C5 and n-C7 crude oil blends bitumen/n-C7, n-C8, n-C10, and n-C12 crude oil/n-C5 crude oil blends

1 10 10 4

(v/v) (v/v) (v/v) (w/w)

5 (v/v) 3 (v/v)

deposits that commonly plug pipelines and process equipment. Compatibility between crude oils is enhanced by keeping asphaltenes dispersed in the blend under thermodynamic and hydrodynamic equilibria. A number of reports in the literature related to asphaltene precipitation and deposition under static conditions is found. However, dynamic studies are scarce, and they have been focused on experiments with blends of crude oils, aromatic

4. CONCLUDING REMARKS Blending crude oils with different chemical natures may cause asphaltene precipitation as a result of incompatibility depending upon the amount of each crude oil in the blend and the procedure used to prepare it, making it possible to form large 8223


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Figure 12. Effect of the solvent type on asphaltene precipitation: (●) Athabasca bitumen (80 °C), (■) Cold Lake bitumen (80 °C), and (▲) crude oil “S” (60 °C).

Figure 14. Precipitation and deposition of asphaltenes at different temperatures and pentane/crude oil ratios: (◇) 28 °C, (□) 45 °C, (△) 58 °C, (×) 70 °C, and (○) 86 °C.

Figure 13. Effect of the temperature on precipitation and deposition of asphaltenes at different heptane/crude oil ratios: (◇) 0.8, (□) 1.5, (△) 3.0, (×) 5.0, and (○) 7.0.

Figure 15. Effect of the flow rate on precipitation and deposition of asphaltenes from a blend of crude oil/pentane at different times: (△) 100 h, (□) 200 h, and (◇) 300 h.

solvent (i.e., toluene), and precipitant (i.e., n-C5, n-C6, and nC7). Different from the studies at static conditions, the flow velocity may promote asphaltene redissolution and delay the deposition. In addition, at static conditions, some conclusions regarding asphaltene deposition can be derived; however, a blend of crude oils can be initially identified as incompatible through standard methods, and it could not really undergo asphaltene deposition under dynamic conditions. The reported experimental loops allow for studying the compatibility of crude oil blends in dynamic conditions and the influence of the type of crude oils, solvents, and operating conditions on asphaltene precipitation and deposition. The

main findings are the following: (a) Increasing the temperature enhances the asphaltene solubility, so that precipitation is retarded. (b) Increasing the flow rate of crude oil keeps asphaltene dispersed and flocculation delayed. (c) The higher the solvent/crude oil ratio, the higher the asphaltene precipitation and deposition. (d) A smaller amount of asphaltenes is precipitated using a solvent with a higher carbon number.

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AUTHOR INFORMATION

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*E-mail: [email protected]. 8224


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The authors declare no competing financial interest.

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