Effect of Nanopore Confinement on Crude Oil Thermal-Oxidative

Article Cite This: Energy Fuels XXXX, XXX, XXX−XXX

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Effect of Nanopore Confinement on Crude Oil Thermal-Oxidative Behavior Siyuan Huang†,‡ and James J. Sheng*,†,‡ †

Key Laboratory of Oil and Gas Reservoir Geology and Exploitation, Southwest Petroleum University, Chengdu, 610500, China Department of Petroleum Engineering, Texas Tech University, Lubbock, Texas 79409, United States

Energy Fuels Downloaded from pubs.acs.org by UNIV OF SOUTH DAKOTA on 08/18/18. For personal use only.

‡

ABSTRACT: The AIP (air injection process) could be a promising technique to develop shale oil reservoirs because air has immense availability and free resources. The main differences between the AIP and conventional gas injection techniques are attributed to the complicated reactions among air, crude oil, and rock. The catalytic effect of the clay minerals on crude oil thermal-oxidative characteristics has been extensively studied; however, the confinement effect has rarely been discussed. In this study, the confinement effect of nanoscale porous media on crude oil thermal-oxidative characteristics was investigated using TGA (thermogravimetric analyzer) and DSC (differential scanning calorimetry) experiments, where the confinement environment was provided by the CPGs (controlled pore glasses). CPGs with three different pore sizes of 51, 85, and 172 nm were used. Also, the Arrhenius method was applied to investigate the crude oil oxidation kinetics during the AIP. The experimental results show that the confinement effect will not only inhibit the distillation endothermic process, but also increase the LTO (low temperature oxidation) exothermicity. Also, the confinement effect will lead to a better fuel deposition, hence increasing the HTO (high temperature oxidation) reaction intensity. It was also observed that smaller pore sized CPGs will result in a lower HTO exothermic peak temperature, which could benefit the AIP recovery performance if the HTO stage can be achieved. In addition, the activation energy values and the frequency factor values of the crude oil in both LTO and HTO stages were decreased under the confinement environment. This study can bring insights to researchers on the crude oil oxidation mechanisms under a confinement environment and help researchers to evaluate the feasibility of AIP in shale oil reservoirs.

1. INTRODUCTION Shale oil development remains a great challenge to researchers due to the current limitations on EOR (enhanced oil recovery) methods. The low injectivity of the shale formation makes chemical and water injection less desired for operation, and the high clay content in a shale reservoir may lead to shale swelling which will cause reservoir damage as well as additional cost to the operation. Therefore, the gas injection technique is preferred for the shale oil reservoir development. Traditional gas injection techniquesnitrogen injection, CO2 injection, and hydrocarbon gas injectionhave been extensively studied for developing shale oil reservoirs.1−3 However, the AIP (air injection process), as an alternative gas injection method, has rarely been discussed. The AIP could be a promising method for developing shale oil reservoirs because air has immense availability and free resources. In addition, the injected air not only will pressurize the reservoir but also react with a small amount of crude oil in situ to generate flue gas and heat. The main differences between the AIP and conventional gas injection techniques are attributed to the complicated reactions among air, oil, and rock. Based on the reaction temperature intervals, three groups of reactions are identified during the AIP: LTO (low temperature oxidation) reactions, FD (fuel deposition) reactions, and HTO (high temperature oxidation) reactions. The LTO reactions usually take place after air is introduced to the reservoir. Although the exothermicities of the LTO reactions are much milder compared to the HTO reactions, the temperature will rise and the reaction mode will shift from the LTO to the FD and HTO if the heat generation © XXXX American Chemical Society

rate is greater than the heat dissipation rate. It was claimed that the success of the AIP in the Williston Basin (United States) was mainly attributed to the thermal effect from the strong exothermic activity of the crude oil oxidation reactions.4,5 Therefore, it is crucial to understand the thermal-oxidative characteristics of the crude oil when considering the AIP technique. TGA (thermogravimetric analyzer) and DSC (differential scanning calorimetry) have been extensively applied to study the thermal-oxidative behavior of crude oil.6−19 In order to simulate the reservoir conditions and study the effect of rock samples, mixtures of crude oil with different rock samples are investigated. The effect of rock samples on the crude oil oxidation reactions are mainly recognized as the surface area effect and the catalytic effect. Physically, a larger surface area will result in more fuel deposition on the rock matrix, hence affecting the oxidation reactions. Chemically, clay minerals and metallic additives can serve as catalysts during crude oil oxidation reactions, where the catalytic effect can be reflected based on the decrement of activation energy. The activation energy can be applied to characterize the crude oil reactivity, to determine the conditions required for ignition, and to predict whether self-ignition could take place during air injection. If the activation energy of a reaction is low, it indicates that the reaction can be triggered more easily or this reaction can be Received: June 24, 2018 Revised: July 26, 2018 Published: August 6, 2018 A

DOI: 10.1021/acs.energyfuels.8b02177 Energy Fuels XXXX, XXX, XXX−XXX

Article

Energy & Fuels

Figure 1. Crude oil composition distribution.

Figure 2. Experimental workflow and sample preparation.

more readily sustained. Vossoughi et al.20 studied the effect of rock samples on crude oil combustion by TGA and DSC. The results indicate that sandstones do not have a catalytic effect on the crude oil oxidation process, while clay minerals (kaolinite) will show catalytic effect and significant surface area effect on oil oxidation. Kök21 also investigated the effect of clay minerals on crude oil oxidation, where the results show that the activation energy values were lowered with the addition of clay minerals. A more detailed study was performed by Kok,22 where the effect of clay concentration on crude oil oxidation was studied. The results show that the activation energy values decrease with the increment of clay concentration, which further proves the catalytic effect of clay minerals on crude oil oxidation reactions. He et al.23 studied the effect of metallic additives on combustion kinetic data of crude oil. The results indicate that the metallic additives have strong catalytic effects on crude oil combustion. Similar findings were reported by Pu et al.,24 where the activation energy values in both the LTO region and the HTO region decreased with the addition of metallic additives. Huang et al.11 compared the shale and sandstone effects on the crude oil oxidation reactions, where the results show that the shale cuttings will not only provide the surface area effect but also the catalytic effect. Recently, the feasibility of applying AIP to develop shale oil reservoirs was discussed by Jia and Sheng.25 Because of the high specific area and clay rich characteristics of the shale rock, it was believed that the shale formation could provide a favorable environment for oxidation exothermic activity during the AIP. As mentioned previously, the clay contents have strong catalytic effect on the crude oil exothermicity, which is favorable for the AIP performance. However, from a physical point of view, since the pore size for a typical shale reservoir varies from several nanometers to several hundred nanometers,

the thermodynamics under the nanoscale environment may not be the same as the ones for the bulk phase due to the nanopore confinement effect.26 Therefore, in order to discuss the feasibility of applying the AIP to a shale oil reservoir, it is crucial to understand the confinement effect on the crude oil oxidation reactions. In this study, the confinement effect of nanoscale porous media on crude oil thermal-oxidative characteristics is investigated by TGA and DSC experiments. This study can bring insights to researchers on the crude oil oxidation mechanisms under a confinement environment, and it can also help researchers to evaluate the feasibility of AIP in shale oil reservoirs.

2. EXPERIMENTAL METHOD In this study, the DSC tests were performed to investigate the crude oil exothermic behavior under air purging environment. The applied heating rate is 10 °C/min, the temperature range is from 25 to 600 °C, and the pressure is atmospheric pressure. The heating rate effect has been discussed in our previous work, which is to overcome the thermal hysterisis effect during the air injection and can be considered by adjusting the corresponding kinetic data.17 The TGA tests were also applied with the same operation conditions as those in the DSC tests, while the main output is the crude oil mass with respect to temperature. Only a small amount of oil sample, around 8 mg, is needed for either a TGA or a DSC test, and the Wolfcamp shale oil with 40°API was used in this study. The composition of the crude oil is presented in Figure 1. For both TGA and DSC tests, the applied air purging rate is 50 mL/min. More details about the functions and procedures of TGA and DSC tests can be found in refs 10 and 27. In order to study the confinement effect of nanoscale porous media on crude oil thermal-oxidative behavior during AIP, the CPGs (controlled pore glasses) were used as shown in Figure 2. The CPGs are made of fused silica and present as extremely fine white powders. The nanoscaled cylindrical pores are connected and highly branched among the CPGs. In this study, CPGs with pore diameters of 51, 85, B


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Energy & Fuels

Figure 3. DSC results of oil only and mixtures of oil with CPGs.

Figure 4. TGA results of oil only and mixtures of oil with CPGs.

silica, and the maximum test temperature is 600 °C, it is assumed that the mass loss and the exothermic or endothermic behavior of the mixture of oil and CPGs are only attributed to the oil, while the mass and composition of the CPGs do not change. 3.1. TGA and DSC Experiments. The TGA and DSC tests on the crude oil were performed in one of our previous studies, and were used in this study as the reference tests.10 The DSC results of oil only and mixtures of oil with CPGs are shown in Figure 3, where the y-axis shows the heat flow and the x-axis shows the temperature. The crude oil distillation process was observed at the beginning of the test, which behaved as an endothermic process. By comparing the negative heat flow values in the distillation stage between the test using crude oil only test and the tests using the mixture of oil with CPGs, it revealed that the endothermic activity of the crude oil was inhibited by the confinement effect. Two exothermic peaks were presented after the distillation stage, where the first exothermic peak was attributed to the LTO reactions and the second exothermic peak was attributed to the HTO reactions. Also, it was seen that the first exothermic peak did not change with the addition of CPGs, while the second exothermic peak shifted to a lower temperature stage after the addition of

and 172 nm were used. For the 51 nm CPGs, the particle size and pore volume are 50−80 mesh and 1.1 cm3/g. For the 85 nm CPGs, the particle size and pore volume are 200−230 mesh and 1.48 cm3/g. For the 172 nm CPGs, the particle size and pore volume are 80−200 mesh and 1.4 cm3/g. To prepare the mixtures of CPGs with oil, the dry CPGs were first placed in a small container. Then, the same weight of oil was poured on the top of the CPGs and the small container was placed in a vacuum desiccator to perform the vacuum process for around 2 h. A slow leak of air into the desiccator was applied until the system returned to atmospheric pressure, and it was assumed that the CPGs were filled with the crude oil by capillary wetting. For each test, around 8 mg of the mixture of CPGs with oil was transferred to the crucible and the crucible was then placed into the TGA or DSC. All the TGA and DSC tests were performed at least twice for repeatability.

3. RESULTS AND DISCUSSION Although extensive TGA and DSC tests have been performed on the thermal-oxidative characteristics of crude oil, the reservoir confinement effect has rarely been discussed. In this study, three different samplesa mixture of oil with 51 nm CPGs, a mixture of oil with 85 nm CPGs, and a mixture of oil with 172 nm CPGswere tested respectively by the TGA and DSC. It is noteworthy that since the CPGs are made of fused C


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Energy & Fuels

Figure 5. DTG results of oil only and mixtures of oil with CPGs.

Figure 6. DSC and DTG results of oil with 172 nm CPGs mixture.

respectively. It was seen that, after the addition of the CPGs, the mass loss rate was lowered in the low temperature stage, and the mass loss rate was increased in the high temperature stage. The reason is that the distillation was inhibited by the confinement effect, which resulted in a lower mass loss rate at the low temperature stage. On the other side, the HTO reactions intensity were enhanced with more deposited fuel after addition of the CPGs to the crude oil; hence a slightly stronger mass loss in the high temperature stage was observed. More detailed analysis about the confinement effect on sample mass loss can be seen in Figure 5. In Figure 5, the DTG (derivative of thermogravimetric) vs temperature was plotted, where two valleys were observed in the low temperature stage of the oil only sample (25−350 °C). The valleys in the DTG curves stand for the sudden mass loss behavior during the TGA tests. The mass loss in the first valley is mainly attributed to the distillation, and the mass loss in the second valley is mainly attributed to the LTO reactions.10 The high temperature stage corresponds to the HTO reactions (350−600 °C), while no obvious valley was observed in this stage. The reason is that, for a light oil, most of the components will be distilled

CPGs. For the cases where the oil was saturated in the CPGs, since less oil was distilled at the beginning, a greater exothermic intensity in the LTO reactions was shown in contrast to the oil only test, which implies that the confinement effect will not only inhibit the distillation endothermicity but also increase the LTO exothermicity. In addition, it can be observed that a smaller pore sized CPGs resulted in a lower HTO exothermic peak temperature, which could be an advantage to the AIP if the high temperature stage can be achieved. Figure 4 shows the TGA results of the tested samples, where the y-axis represents the mass remaining fraction and the x-axis shows the temperature. It can be observed that the three mixture samples presented similar mass loss behaviors and differed from that of the oil only sample. Two stages can be differentiated based on the mass loss trend in Figure 4, where the low temperature stage varies from 25 °C to around 350 °C, and the high temperature stage varies from 350 to 600 °C. By comparing the mixtures of crude oil with CPGs to the oil only sample, the confinement effect was revealed based on the mass loss rate difference in the aforementioned two stages, D


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Energy & Fuels



or oxidized in the low temperature stage; therefore, not much oil will be left in the high temperature stage. On the other side, in Figure 5, it shows that when the oil is under confinement condition, instead of presenting two valleys in the low temperature stage, a downward peak was shown after a valley. For all three sized CPGs cases, the downward peak locates in a higher temperature stage in contrast to that of the two valleys of the oil only sample. Following this downward peak, a valley was shown in the high temperature stage. Since there is no other variable except the confinement pores in this experiments, it indicates that the confinement effect would result in a better fuel deposition. Hence a more significant mass loss occurred in the high temperature stage. This also corresponds to the TGA results shown in Figure 4, where the mass loss rate of the oil only sample was greater than those of mixtures of CPGs with oil in the low temperature stage, and the mass loss rate of the oil only sample was lower than those of mixtures of CPGs with oil in the high temperature stage. In addition, it was observed that a smaller CPGs pore size will shift the high temperature reactions to a lower temperature region, which

was attributed to the better fuel deposition under a more confined environment. Figures 6−8 show the DTG and DSC results of mixtures of oil with different sized CPGs. It was observed that the LTO reaction occurs between 25 °C and around 380 °C and the HTO reaction temperature varies from 400 to 600 °C. For all three cases, it can be seen that the downward peak in DTG corresponds to the beginning of the exothermic process in DSC, and the second valley in DTG corresponds to the high temperature exothermic peak in DSC, which proved the consistency of the TGA and DSC results. 3.2. Kinetic Analysis. The kinetic data were obtained by applying the Arrhenius method to the TGA data. In the TGA tests, it was assumed that the oxidation reactions are not dependent on the oxygen concentration since only a small amount of crude oil sample is used and the surrounding air flow is excessive. A first-order reaction to crude oil was considered without the mass transfer limitation.27 The kinetic data including the activation energy and frequency factor can be obtained from the linear regression, where the activation E


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Energy & Fuels

Figure 9. Arrhenius analysis for mixture of crude oil with 172 nm CPGs.



energy can be obtained from the slope and the frequency factor can be obtained from the intercept shown in eq 1: F

i ij A yz Ea 1 dα yzz lnjjjj zz = lnjjj zzz − n T RT (1 ) d − α β k { k {

(1)


Article

Energy & Fuels Table 1. Kinetic Data of Crude Oil and Mixture of Crude Oil with CPGs, Using the Arrhenius Method sample oil only 172 nm CPGs 84 nm CPGs 51 nm CPGs

stage

slope

intercept

Ea (kJ/mol)

LTO HTO LTO HTO LTO HTO LTO HTO

−2040 −19794 −1190.7 −14295 −1183.6 −10392 −1191 −6590.2

−0.75 21.66 −2.731 14.632 −2.715 10.125 −2.6774 4.9877

16.96 164.57 9.90 118.85 9.84 86.40 9.90 54.79

where A is the frequency factor, min−1; Ea is the activation energy, kJ/mol; R is the universal gas constant, kJ/(mol K); n is the order of reaction; β is the heating rate, K/min; T is the absolute temperature, K; and α is the conversion degree, which is a normalized form of mass loss of the crude oil sample and is m −m defined by the expression α = mi − mt , where mi is the initial i

freq factor (s−1) 5.35 7.04 1.02 2.00 1.04 4.66 1.07 6.41

× × × × × × × ×

10−1 107 10−1 105 10−1 103 10−1 101

peak temperature, which could benefit the AIP recovery performance if the HTO stage can be achieved. • The activation energy values and the frequency factor values of the crude oil in both LTO and HTO stages were decreased under the confinement environment, where smaller pore sized CPGs resulted in a lower activation energy and a lower frequency factor values in the HTO stage. However, different CPGs pore sizes did not show significant effect on the crude oil kinetics in the LTO stage.

f

mass of the sample; mg; mf is the final mass of the sample, mg; and mt is the sample mass at temperature T, mg. More details about the transform of the Arrhenius equation have been well described in ref 10. Equation 1 was applied to the TGA results of the mixture of crude oil with different pore sized CPGs in LTO stage and HTO stage, respectively, and the results are shown in Figures 9−11. The detailed results are summarized in Table 1, where the activation energy values were obtained based on the slope and the frequency factor values were obtained from the intercept. It can be observed that the activation energy values in both LTO and HTO stages were decreased after addition of the CPGs, where the activation energy in the LTO stage under the confined environment is around 9.9 kJ/mol. In addition, the pore size effect of CPGs on the crude oil activation energy was revealed in the HTO stage, where a smaller CPGs pore size resulted in a lower activation energy value. However, different pore sized CPGs do not show significant effects on the crude oil activation energy in the LTO stage. On the other side, the frequency factor values were decreased after addition of the CPGs in both LTO and HTO stages. Similar to the confinement effect on the activation energy values, no significant effect was observed on the frequency factor in the LTO stage, while a smaller CPGs pore size resulted in a lower frequency factor in the HTO stage. To conclude, the confinement effect can be revealed based on the analysis of the kinetic data. When comparing between the crude oil only to the mixture of crude oil with CPGs, the confinement effect will lower the activation energy and the frequency factor values in both LTO and HTO stages. On the other hand, when comparing among different CPGs pore sizes, it was observed that a smaller pore sized environment tends to result in a lower activation energy and a lower frequency factor in the HTO stage, while the pore size effect on the crude oil kinetics in the LTO stage was not significant.

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AUTHOR INFORMATION

Corresponding Author

*Tel.: 806-834-8477. E-mail: [email protected]. ORCID

Siyuan Huang: 0000-0002-9769-9510 James J. Sheng: 0000-0002-1778-1486 Notes

The authors declare no competing financial interest.

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REFERENCES

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4. CONCLUSION The conclusions arising from this study are the following: • The confinement effect will not only inhibit the distillation endothermic process but also increase the LTO exothermic activity. • The confinement effect will lead to a better fuel deposition and thus increase the intensity of HTO reactions. In addition, smaller pore sized CPGs will result in a lower HTO exothermic G


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Effect of Nanopore Confinement on Crude Oil Thermal-Oxidative

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