Article Cite This: J. Chem. Eng. Data XXXX, XXX, XXX−XXX
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Experimental Investigation of CO2 Hydrate Formation in the Water Containing Graphite Nanoparticles and Tetra‑n‑butyl Ammonium Bromide Shidong Zhou,*,†,‡,§ Kun Jiang,† Yongli Zhao,† Yuandao Chi,*,‡ Shuli Wang,† and Guozhong Zhang§ †
Changzhou University, Changzhou, 213016, China The University of Tulsa, Tulsa, Oklahoma 74110, United States § China University of Petroleum, Huadong, Qingdao 266580, China ‡
ABSTRACT: The effects of tetra-n-butyl ammonium bromide (TBAB) and graphite nanoparticles (GN) on phase equilibrium curves, gas consumption, induction time, and ratio of water to hydrate conversion were investigated in this work. Aqueous solutions of the mixture of TBAB and GN with three concentrations of 0.04%, 0.06%, 0.08%, and 0.1% were tested in a stirred reactor. The graphite nanoparticles with a concentration of 0.08% showed the highest hydrate formation rate, revealing that 0.08% is the optimal concentration for the hydrate formation in this study. Comparing the induction time of the pure TBAB system with that of various concentrations of GN, a decrease by 16.6% of induction time at 0.08% GN concentration was observed, while the value decreased by 31.62% at a GN concentration of 0.1%. The final water to hydrate conversion reached the maximum value of 50.75% at a GN concentration of 0.08%. The concentration effect of graphite nanoparticles on the phase equilibrium curve in the presence of TBAB was also studied in this work. As reported, the concentration of graphite nanoparticles had little effect on the phase equilibrium of CO2 hydrate formation, while adding TBAB to nanofluids could greatly reduce the hydrate formation pressures. enhancement of the gas hydrate formation kinetics. Li et al.20 reported that the heat and mass transfer process of HFC134a hydrate formation was enhanced by adding nanocopper. In addition, a significant upward shift of the dissociation pressure of HFC134a hydrates in the nanofluids was observed. Chariet al.21 proved that the nanoparticles (nano hollow silica) had a significant effect on the rate of hydrate formation and the final water to hydrate conversion. Mohammadi et al.28 investigated the effect of silver nanoparticles and SDS on CO2 hydrate formation. It was reported that SDS, silver nanoparticles, and their mixture had no significant effect on the induction time and gas consumption. However, the mixture of SDS and silver nanoparticles increased the storage capacity and the final water to hydrate conversion. Govindarajet al.22 formed methane hydrates in the presence of activated carbon and nanosilica suspensions with three concentrations. It was seen that both the reagents have promoting effects on the hydrate formation, while the effect of activated carbon is more pronounced. In addition, the kinetics of hydrate formation were more favorable at higher concentrations of the nanosilica suspensions. Said et al.23 investigated the effects of Al2O3, SiO2, Ag, and Cu
1. INTRODUCTION Gas hydrates are ice-like crystalline solid compounds, which are formed by the interaction between gas molecules and water molecules under low temperature and high pressure conditions. The gas molecules interact with water molecules by means of van der Waals forces existing in hydrogen-bonded water cages, thus stabilizing the hydrate structure.1 Gas hydrates have been well-known as a critical issue in the oil and gas industries, as they can plug the transportation pipelines2−4 associated with other flow assurance problems, such as wax deposition.5−7 However, it has to be noted that the gas hydrates formation process has been utilized in several technological applications, such as the natural gas storage and transportation,8 seawater desalination,9,10 carbon capture, transport and sequestration,11−14 and so forth. Therefore, accelerating the hydrate formation rate and increasing gas storage capacity15 are the main contributing factors for commercially feasible technologies. The use of surfactants to enhance the gas hydrate kinetics has been highlighted since 1990s.16−19 More recently, the nonsurfactant-based method has gained much interest by increasing the surface area and heat and mass transfer between the liquid and gas phases, such as nanoparticles,20−23 sand packs,24 silica gels,25 foams,26 and hydrogels.27 Among all these methods, the addition of nanoparticles showed promising results toward the © XXXX American Chemical Society
Received: September 1, 2017 Accepted: December 22, 2017
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DOI: 10.1021/acs.jced.7b00785 J. Chem. Eng. Data XXXX, XXX, XXX−XXX
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Figure 1. Schematic diagram of the experimental apparatus.
nanoparticles on the kinetics of CO2−CH4 hydrate formation process. Three concentrations of each nanoparticle were utilized. It was found that nanoparticles of SiO2 had the most positive effect on CO2 gas consumption, especially at the concentration of 0.3 wt %. Cu and Al2O3 nanoparticles were observed as an intermediate effect on the gas consumption, while Ag had no significant effect. Graphite nanoparticles are acid-resistant, and have a high heat-transfer coefficient and a low price.29 Therefore, they have a promising perspective of industrial application of the hydrate technologies where acidic environment is always encountered. Graphite nanoparticles were utilized to investigate its promotion effect on hydrate formation in our previous study.29 As reported, the presence of graphite nanoparticles facilitated the hydrate formation. However, it was also found that graphite nanoparticles have a negative effect on the hydrate formation conditions by shifting up the formation pressure curve of the CO2 hydrates.30 To overcome this shortcoming, an effective thermodynamic additive is needed to improve this system. The tetra-n-butyl ammonium bromide (TBAB), as a thermodynamic promoter, has proven to significantly reduce the hydrate formation pressure.31 Therefore, for the first time, the effects of graphite nanoparticles and TBAB on phase equilibrium curves, gas consumption, induction time, and ratio of water to hydrate conversion hydrate formation were investigated in this study. In addition, the concentration effect of graphite nanoparticles on the phase equilibrium curve in the presence of TBAB was also studied.
cooling system, a hydrate reaction system, and a data acquisition system. The reactor had a volume of 500 mL, which could withstand a pressure of 30 MPa. The thermal resistance (Pt 100) had a precision of ±0.1 K (253.15−293.15 K), and the BD pressure transducer had a range of 0−10 MPa. The reaction temperature was controlled by a thermostat with the range of 258.15−268.15 K. Besides, a magnetic stirrer installed in the reactor was used to homogenize the gas−liquid system. Gas was supplied by a piston compressor from the gas cylinder in order to reach the desired system pressure condition. Aqueous solutions were pumped into the reactor by a centrifugal pump. The pressure and temperature in the reactor were collected by the data acquisition system at an interval of every second. 2.3. Procedures. The reactor was washed three times with distilled water thoroughly. The reactor was then filled with 200 mL of solution, and evacuated using a suction pump until the pressure reached −0.02 Pa. Subsequently, the reactor temperature was adjusted to the desired value using the thermostat. After that, a certain amount of CO2 was introduced into the reactor to raise the cell pressure to the set point. Finally, the magnetic stirrer was started with a speed of 300 rpm, and the experiment was started.
3. RESULTS AND DISCUSSION 3.1. Phase Equilibrium Curves of the Graphite Nanoparticles and TBAB Mixed Gas Hydrate System. A stepwise method was used to obtain the phase equilibrium data. Figure 2 shows the phase equilibrium for the mixture of TBAB with a concentration of 9.01% and graphite nanoparticles with four concentrations (0.04%, 0.06%, 0.08%, and 0.1%). Experiments were conducted at the temperature range of 282.5 K− 288.5 K and a pressure range of 0.35 MPa−2.5 MPa. As shown in Figure 2,a significant upward shift of the phase equilibrium curves of the TBAB and GN solution system was observed at a given temperature, as compared to the aqueous solution containing only TBAB. Besides, the upward shift being not significant was observed in our experiments, indicating that the concentration of graphite nanoparticles had little effect on the phase equilibrium of CO2 hydrate formation. In other words, the hydrate formation pressure in the GN+TBAB solution system was higher than that in the solution containing only TBAB. This phenomenon can be explained as follows. Graphite nanoparticles in the water increase the disorder of the water
2. EXPERIMENTAL PROGRAM 2.1. Materials. Graphite nanoparticles with a purity of 99.9% and average fineness of 50 nm were obtained from Xuzhou Jiechuang New Material Technology Co., Ltd., China. TBAB was obtained from Shanghai ShengzhongFineChemical Co., Ltd., China. Carbon dioxide, with a purity of 99.8%, used in this work was supplied by Changzhou Jinghua Industrial Gases Co., Ltd.,China. The deionized water with a resistivity of 18.25 mΩ·cm−1 was prepared in the laboratory. An accurate balance with an accuracy of ±0.0002 g was used to prepare all aqueous solutions. 2.2. Experimental Facility. The experimental facility was the same as the one used in the previous study.29 The schematic diagram of the experimental apparatus is shown in Figure 1. It consists of an intake system, a fluid system, a B
DOI: 10.1021/acs.jced.7b00785 J. Chem. Eng. Data XXXX, XXX, XXX−XXX
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Table 1. Specific Value of Phase Equilibrium for the Mixture System of TBAB with Various Graphite Nanoparticles Concentrations GN w% + TBAB 9.01% 0
0.04
Figure 2. Phase equilibrium of TBAB+GN varying with different GN concentrations.
molecules, which results in the increase of system entropy. Hence, the formation of a hydrate crystal cell requires more hydrogen-bond energy, leading to the phase equilibrium curve shift to the low-temperature and high-pressure side. In addition, some graphite nanoparticles with larger particle sizes have porous structures which could reduce the activity of water, thus increasing the hydrate formation pressure.32 However, the results mentioned above seem not to agree with the conclusion of “graphite nanoparticles have a positive effect on the gas hydrate formation” as presented in the literature.33 Actually, these two conclusions were drawn from two different aspects, namely, thermodynamics and kinetics. Graphite nanoparticles can promote hydrate formation due to its high heat transfer coefficient and specific surface area, which are two key kinetic parameters in determining the hydrate formation. However, the phase equilibrium for gas hydrates was determined by the thermodynamic process of hydrate formation. It was just a parameter to determine the hydrate formation conditions rather than the hydrate formation rate. In addition, it can be inferred from Figure 2 that the concentration of graphite nanoparticles had little effect on the phase equilibrium of CO2 hydrate formation. Table 1 shows the specific value of phase equilibrium for the mixture system of TBAB and graphite nanoparticles with various concentrations of 0.04%, 0.06%, 0.08%, and 0.1%, respectively. 3.2. Effect of GN+TBAB on CO2 Hydrate Formation. The effect of GN and TBAB on the gas consumption, induction time, and ratio of water to hydrate conversion will be discussed in this section. To obtain the effect of additives on CO2 hydrate formation, nanofluids with GN concentrations of 0.02%, 0.04%, 0.06%, 0.08% and 0.1%, were prepared. Experiments were carried out at a temperature of 277.15 K and initial pressure of 4.5 MPa with the mixing speed of 300 rpm. The amount of gas consumed is an important parameter for hydrate formation, and the following eq eq 1 is applied to calculate it.34 ΔnCO2 =
P0V0 PV − t t Z0RT0 ZtRTt
0.06
0.08
0.1
temp (K) 282.79 283.34 284.43 285.07 286.38 287.6 288.09 282.32 283.41 284.37 285.11 287.04 288.03 288.11 283.51 283.99 284.58 285.36 287.17 288.19 288.23 283.47 284.27 284.92 285.74 287.05 287.89 288.31 283.88 284.01 284.55 285.03 287.01 287.97 288.17
pressure ± uncertainty (MPa) 0.391 0.393 0.583 0.859 1.333 1.803 2.174 0.463 0.501 0.722 0.967 1.715 2.342 2.416 0.531 0.644 0.787 1.107 1.773 2.437 2.446 0.529 0.714 0.925 1.263 1.717 2.293 2.444 0.599 0.651 0.789 0.969 1.704 2.311 2.435
± ± ± ± ± ± ± ± ± ± ± ± ± ± ± ± ± ± ± ± ± ± ± ± ± ± ± ± ± ± ± ± ± ± ±
0.0011 0.0009 0.0006 0.0012 0.0011 0.0013 0.0012 0.0008 0.0011 0.0009 0.0007 0.0013 0.0014 0.0011 0.0012 0.0011 0.0009 0.0010 0.0010 0.0011 0.0014 0.0013 0.0012 0.0013 0.0009 0.0010 0.0005 0.0011 0.0010 0.0011 0.0009 0.0008 0.0012 0.0015 0.0013
recommended to calculate Vt using the following eq (eq 2)28in order to account for the reduction in the volume of gas phase inside the reactor as the hydrate formation occurs. Vt = Vcell − VS0 + VRWt − VHt
(2)
where Vcell is the volume of the reactor (500 mL). VS0 is the volume of the adding solution (200 mL). VRWt is the volume of water reacted, and VHt is the volume of hydrate conversion from water. VRWt and VHt could be acquired from eqs 3 and 4,28 respectively.
(1)
where P and T are the pressure and temperature of the reactor, respectively. R is the universal gas constant (8.314 J/(mol·K)). V is the volume of the gas phase inside the reactor. Z is the compressibility factor, which is calculated by Peng−Robinson equation of state.32 Subscripts 0 and t represent conditions of the reactor at time t = 0 and time t, respectively. It is
VRWt = M × ΔnCO2 × υwl
(3)
VH t = M × ΔnCO2 × υwMT
(4)
where M is the hydrate number. It is well-known that TBAB/ CO2 hydrate is a semiclathrate hydrate, and the hydrate number used in the work is 36.04. υlw and υMT represent the molar w volume of liquid water and empty hydrate lattice, respectively, and the specific calculation method is presented in the literature.35,36 C
DOI: 10.1021/acs.jced.7b00785 J. Chem. Eng. Data XXXX, XXX, XXX−XXX
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As shown in Figure 3, the effects of nanofluids with four different graphite nanoparticles concentration (0.02%, 0.04%,
Table 3. Effect of TBAB and Graphite Nanoparticles on the Induction Time and Final Water to Hydrate Conversion of CO2 Hydrate Formation GN concentration/(%) + TBAB (9.01%) 0 0.04 0.06 0.08 0.1
induction time ± uncertainty/(min) 4.21667 3.38333 3.51667 3 2.88333
± ± ± ± ±
0.121 0.143 0.098 0.113 0.076
final conversion/ (mol %) 44.89 46.78 48.21 50.75 47.80
then decreases as the graphite nanoparticles concentration increases. Moreover, the final conversion reached the maximum value of 50.75% at a GN concentration of 0.08%. The definition and measuring method of the induction time were described in the previous study.29 Figure 4 shows the
Figure 3. Effect of nanofluids with different GN concentration on the amount of CO2 consumed.
0.06%, 0.08%, and 0.1%) and 9.01% TBAB on the amount of CO2 consumed were investigated. It can be seen that the rate of gas consumption increases rapidly at the beginning of the reaction, and the increase slows down and reaches a stable state at the later time. This occurs because during the process of hydrate reaction, the newly formed hydrates increase the mass transfer resistance between gas and liquid, which facilitates the mass transfer efficiency of reactions. Figure 3 also shows that the maximum value of final gas uptake is obtained at nanofluids with the TBAB and 0.08% graphite nanoparticles. According to the results provided by Table 2, the final mole of gas consumed
Figure 4. Induction time of hydrate formation in the nanofluids with different GN concentration.
Table 2. Final Gas Uptake of Hydrate Formation in Nanofluid with Different GN Concentration TBAB (9.01%) + GN concentration/ (%)
mole of gas consumed in the final/ (mol)
0 0.04 0.06 0.08 0.1
0.1765 0.1839 0.1895 0.1995 0.1879
induction time of hydrate formation in the TBAB solution with five different graphite nanoparticles concentrations (0.00%, 0.04%, 0.06%, 0.08%, and 0.1%). The result shows that the induction time decreases as the graphite nanoparticles concentration increases. This occurs because nanoparticles with a large specific surface enhance the effect of mass transfer and heat transfer. Table 3 shows detailed experimental data of the induction time of CO2 hydrate formation. As compared to that in the pure TBAB system, the maximum induction time was decreased by 31.62% at a GN concentration of 0.1%, while the minimum value was decreased by 16.6% at a GN concentration of 0.06%.
in the nanofluids with the concentration of 0.08% graphite nanoparticles increases by 13% as compared to that in a pure TBAB system. In addition, the nanofluids with a graphite nanoparticles concentration of 0.08% shows the highest hydrate formation rate. Therefore, it can be concluded that the concentration of 0.08% is the optimal concentration for the hydrate formation in this work. The ratio of water to hydrate conversion is another key parameter for hydrate formation, which is defined as the mole number of water converted to the hydrate per mole of feedwater. The following eq 5 was used to calculate it. conversion =
4. CONCLUSIONS The effects of graphite nanoparticles with TBAB (9.01%) and five different concentrations (0.02%, 0.04%, 0.06%, 0.08%, and 0.1%) on hydrate phase equilibrium were investigated in this paper, and the results showed that adding graphite nanoparticles to the mixed system can greatly reduce the hydrate formation conditions, while the concentration of graphite nanoparticles had little effect on the phase equilibrium of the CO2 hydrate formation. In addition, the effects of graphite nanoparticles and TBAB on hydrate formation were studied in this paper. Three key parameters, namely the amount of gas consumed, induction time, and water to hydrate conversion were focused on in this study. The results showed that the nanofluids with graphite nanoparticles concentration of 0.08% showed the highest hydrate formation rate. In addition, the
M × ΔnCO2 n W0
(5)
Table 3 shows the effect of the mixture of TBAB and graphite nanoparticles on the ratio of final water to hydrate conversion. It can be observed that the final conversion increases initially, D
DOI: 10.1021/acs.jced.7b00785 J. Chem. Eng. Data XXXX, XXX, XXX−XXX
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induction time decreased by 16.6% at a GN concentration of 0.08%, while the maximum value decreased by 31.62% at GN concentration of 0.1%. Moreover, the final water to hydrate conversion reached the maximum value of 50.75% at a GN concentration of 0.08%. Therefore, it can be concluded that the concentration of 0.08% is the optimal concentration for the hydrate formation for this work.
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AUTHOR INFORMATION
Corresponding Authors
*E-mail:
[email protected]. *E-mail:
[email protected]. ORCID
Shidong Zhou: 0000-0001-8468-1226 Funding
The authors acknowledge the funding from the Science and Technology Innovation Foundation of the China National Petroleum Corporation (CNPC) (Grant 2016D50070607) and National Natural Science Foundation of China (Grant 51574045). Notes
The authors declare no competing financial interest.
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DOI: 10.1021/acs.jced.7b00785 J. Chem. Eng. Data XXXX, XXX, XXX−XXX
