Density, Viscosity, and N2O Solubility of Aqueous ... - ACS Publications

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Density, Viscosity, and N2O Solubility of Aqueous 2‑(Methylamino)ethanol Solution Xiao Luo,† Liusong Su,† Hongxia Gao,*,†,‡ Xitian Wu,† Raphael O. Idem,†,‡ Paitoon Tontiwachwuthikul,*,†,‡ and Zhiwu Liang*,†,‡ †

Joint International Center for CO2 Capture and Storage (iCCS), College of Chemistry and Chemical Engineering, Hunan University, Changsha, 410082, P. R. China ‡ Clean Energy Technologies Research Institute (CETRI), Industrial and Process Systems Engineering, University of Regina, Regina, Saskatchewan S4S 0A2, Canada S Supporting Information *

ABSTRACT: In the present work, the density and viscosity of 2-(methylamino)ethanol (MAE) solution were measured over the temperature range of 293.15 to 323.15 K with MAE mass fractions of w1 = 0.075, 0.15, 0.225, and 0.30 and CO2 loadings varying between 0 and 0.677 mol CO2/mol MAE. The physical solubility of N2O in aqueous MAE solution was measured in a stirred cell reactor over the temperature range of 289.31− 348.18 K with MAE mass fraction w1 = 0.075, 0.15, 0.225, 0.30, 0.375, 0.45, 0.60, 0.75, and 1. The experimental density data for both CO2 loaded and unloaded aqueous MAE solutions were fitted by Redlich−Kister equation. The Weiland’s model was used to correlate the viscosity data of aqueous MAE solution. Finally, N2O solubility data were correlated by using an empirical polynomial model and compared with both the semiempirical model and the Redlich−Kister equation.

1. INTRODUCTION In recent years, increasing attention has been focused on greenhouse gas (GHG) emissions to the atmosphere and its effects on global warming and climate change. Carbon dioxide (CO2) is the most abundant of the GHGs caused by human activities.1 Chemical absorption method with amines has proven to be the most effective technology for removing CO2 and has been widely used for CO2 removal from large point exhaust gas streams of industrial processes.2 In general, amines are types of weakly alkaline solvents which can react reversibly with the acid gas, CO2, to form an unstable salt. When the temperature is increased, the solvent is regenerated, and the CO2 is released. Currently, the most studied and well-known commercial alkanolamines are monoethanolamine (MEA) and methyldiethanolamine (MDEA). MEA is a primary amine which has the advantages of low molecular weight, fast absorption rate, low cost, and reasonable thermal stability. However, it shows some disadvantages in its industrial application such as the ease of foaming, high corrosion rate, and high regeneration energy consumption. On the other hand, MDEA is a tertiary amine and has a higher loading capacity, low corrosion rate, high resistance to thermal and chemical degradation, and high energy efficiency for its regeneration. However, it has low absorption and masstransfer rates. These two classes of amine have different reaction mechanisms which lead to different properties. Primary amines such as MEA can react with CO2 to form a stable carbamate, resulting in limiting the total loading capacity to © 2016 American Chemical Society

0.5 mol CO2/mol MEA, while secondary amines such as DEA and sterically hindered amines such as AMP can form unstable carbamate that will eventually hydrolyze to bicarbonate and free amine, which makes such amines to absorb more CO2. 2-(Methylamino)ethanol (MAE), a secondary amine, has already been proven to be a potential absorbent for CO2 capture by some researchers.3,4 MAE combines the characteristics of primary and tertiary amines of a high reaction rate with CO2and high CO2 capture capacity, respectively.5,6 Mimura et al.7 studied the reaction kinetics between CO2 and sterically hindered secondary alkanolamines, such as MAE, ethylaminoethanol (EAE), and butylamino ethanolamine (BAE), the results showed that MAE presents a higher reaction rate with CO2 than the primary alkanolamine monoethanolamine (MEA) and the secondary alkanolamines EAE and BAE. Folgueira et al.8 have studied the hydrodynamic behavior and the mass-transfer performance of CO2 with aqueous MAE solution in a bubble column reactor (BCR), as well as the reaction mechanism using analysis by NMR technology. The results showed that the carbamate and bicarbonate are the main products at low and high CO2 loadings, respectively. With high CO2 loading, bicarbonate mainly comes from carbamate hydrolysis and protonated amine, thus allowing for more CO2 absorption. Therefore, MAE shows an attractive behavior with higher Received: June 17, 2016 Accepted: December 16, 2016 Published: December 30, 2016 129

DOI: 10.1021/acs.jced.6b00504 J. Chem. Eng. Data 2017, 62, 129−140

Journal of Chemical & Engineering Data

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carbon dioxide loading and higher reaction rate. Huang et al.9 proved the formation of carbamate is unstable which allows for a higher absorption capacity. Hawar et al.3 measured the equilibrium solubility of CO2 in aqueous MAE solutions with concentration of 1.0, 2.0, and 4.0 M at CO2 partial pressures ranging from 1 to 100 kPa at 303, 313, and 333 K using a stirred cell reactor. The experimental solubility of CO2 in MAE solution were compared with that in MEA, DEA, AMPD, and MDEA solutions, and the results showed that MAE exhibited a

higher absorption capacity as compared with MEA and DEA and were similar to that of AMPD and MDEA at high CO2 partial pressures but exceeded all of them at low partial pressures. Kumar et al.10 investigated the equilibrium solubility of CO2 into aqueous solution of aqueous MAE solutions at different molalities (0.968, 1.574, 2.240, and 3.125 mol·kg−1) of solvent, temperatures at 303.1, 313.1, and 323.1 K, and total CO2 pressure in the range of 1−350 kPa. These researchers established MAE as a potential solvent either to the gas-treating industry or to the gas-treating research community. This work further verified the theory of Pacheco5 and Garciá Abuiń 6 that MAE combined the advantages of primary amines, tertiary amines, and sterically hindered amines. The density and viscosity of amine solutions are the key parameters in modeling the absorber and regenerator since these properties affect the hydrodynamics and mass transfer coefficients,11,12 while the physical solubility of CO2 in amine solutions is an essential parameter when developing the reaction kinetics as well as the thermodynamics model. Currently, there is still no literature that reports data of density, viscosity, and CO2 physical solubility of the aqueous MAE solution. However, physical solubility cannot be measured directly13 due to the chemical reactions that occur between CO2 and amine solutions. To measure and to estimate the CO2 solubility in aqueous amine solutions, the “N2O analogy” method is used. It was originally proposed by Clarke14 and verified by Laddha,15 since N2O is similar to CO2 in molecular volume, configuration, and electronic structure, and it is a nonreactive gas in amine solutions. The calculation equation is shown as follows:

Figure 1. Structure of MAE.

Table 1. Chemical Sample Information

a

chemical name

CAS number

source

initial purity

purification method

MAEa CO2 N2O

109-83-1 124-38-9 10028-97-2

Macklin company Rizhen Gas Co. Ltd. Rizhen Gas Co. Ltd.

≥99%b ≥99%c ≥99.99%c

none none none

2-(Methylamino)ethanol. bMass fraction. cVolume fraction.

⎛ HeCO − H O ⎞ 2 2 ⎟⎟ HeCO2 − amine = He N2O − amine⎜⎜ He ⎝ N2O − H2O ⎠

(1)

Table 2. Experimental Values of Henry’s Law Constant of CO2 and N2O in Water at Different Temperatures T and Pressuresa

Figure 2. Deviations (μexp − μcal)/μexp for MAE + water between experimental viscosity data and predicted values from Weiland’s model in this work and comparing with the literature at different temperature. (Black symbols are the values in this work, and the red symbols are come from Li et al.23).

T/K

HeCO2−H2O (Pa·m3·mol−1)

T/K

HeN2O−H2O (Pa·m3·mol−1)

294.57 298.86 314.22 326.65 345.57

2838.0 3085.9 4148.9 5231.9 7540.6

290.75 301.95 317.43 333.15 351.44

3444.6 4778.1 6583.0 8942.4 12075.4

a

Expanded uncertainties at 95% confidence are U(T) = 0.02 K, U(P) = 1 kPa, and U(He) = 36 Pa·m3·mol−1.

Figure 3. Diagram of physical solubility apparatus. 130



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where He represents Henry’s law constant of gas into solvent, and the subscripts indicate different gases and solvents.

In this work, the density and viscosity of MAE solutions were measured over the temperature range of 293.15−323.15 K with MAE mass fractions w1 = 0.075, 0.15, 0.225, and 0.30 and CO2

Figure 4. Henry’s law constant of CO2 in water: this work comparing literature data.11,18,26

Figure 5. Henry’s law constant of N2O in water: this work comparing literature data.11,18,26,28

Table 3. Density ρ (kg·m−3) of MAE (1) + H2O (2) + CO2 (3) with MAE Mass Fraction w1 = 0.075−0.30 (on a CO2-Free Basis) from T = 293.15 to 323.15 K and Different CO2 Loading α, and Equivalent CO2 Molality b3 at a Pressure of 101.325 kPaa T/K −1

w1b

α

b3 (mol·kg )

293.15

298.15

303.15

308.15

313.15

318.15

323.15

0.075

0.000 0.102 0.164 0.255 0.357 0.399 0.474 0.548 0.644 0.000 0.076 0.104 0.237 0.309 0.416 0.517 0.640 0.677 0.000 0.048 0.122 0.238 0.368 0.396 0.498 0.599 0.657 0.000 0.089 0.128 0.254 0.371 0.396 0.535

0.000 0.102 0.164 0.256 0.358 0.400 0.475 0.549 0.645 0.000 0.152 0.208 0.475 0.620 0.834 1.036 1.283 1.358 0.000 0.145 0.367 0.716 1.107 1.189 1.497 1.801 1.976 0.000 0.358 0.512 1.017 1.489 1.588 2.145

997.66 1003.69 1008.17 1013.18 1019.88 1023.00 1024.69 1026.54 1034.36 997.93 1006.44 1010.32 1025.97 1029.66 1037.74 1047.79 1055.48 1057.11 999.00 1006.43 1017.99 1035.00 1050.13 1055.17 1067.62 1073.45 1079.79 1001.69 1016.25 1024.17 1044.79 1063.80 1070.03 1092.50

996.35 1002.33 1006.76 1011.61 1018.29 1021.37 1023.06 1024.93 1032.27 996.35 1004.83 1008.70 1022.26 1027.87 1035.85 1045.87 1053.60 1055.24 997.03 1004.42 1015.98 1033.01 1048.02 1053.01 1065.37 1071.25 1077.62 999.21 1013.83 1021.77 1042.43 1061.41 1067.62 1090.00

994.81 1000.74 1005.13 1009.91 1016.48 1019.53 1021.24 1023.12 1032.77 994.57 1003.01 1006.87 1020.35 1025.87 1033.78 1043.78 1051.54 1053.19 994.90 1002.23 1013.80 1030.83 1045.74 1050.69 1062.98 1068.90 1075.28 996.58 1011.28 1019.23 1039.93 1058.89 1065.08 1087.40

993.06 998.94 1003.29 1008.02 1014.50 1017.53 1019.24 1021.14 1030.98 992.60 1001.01 1004.85 1018.26 1023.68 1031.56 1041.54 1049.34 1051.00 992.58 999.89 1011.46 1028.49 1043.33 1048.25 1060.50 1066.44 1072.83 993.80 1008.60 1016.57 1037.33 1056.26 1062.43 1084.73

991.11 996.96 1001.26 1005.93 1012.36 1015.38 1019.09 1019.00 1029.03 990.45 999.91 1002.67 1016.00 1021.32 1029.20 1039.17 1047.01 1048.69 990.11 997.41 1008.98 1026.02 1040.79 1045.69 1057.90 1063.87 1070.29 990.81 1005.81 1013.79 1034.60 1053.54 1059.70 1081.97

988.99 994.79 999.06 1003.69 1010.07 1013.07 1014.78 1016.70 1024.67 988.13 996.49 1000.31 1013.58 1018.81 1026.72 1036.67 1044.56 1046.25 987.49 994.78 1006.36 1023.40 1038.14 1043.03 1055.21 1061.19 1067.64 987.70 1002.91 1010.90 1031.77 1050.72 1056.88 1079.12

986.70 992.46 996.70 1001.29 1007.62 1010.60 1012.32 1014.25 1022.27 985.66 993.98 997.80 1011.03 1016.19 1024.10 1034.04 1041.99 1043.70 984.71 992.02 1003.16 1020.67 1035.38 1040.25 1052.40 1058.42 1064.90 984.50 999.90 1007.91 1028.84 1047.81 1053.96 1076.18

0.15

0.225

0.30

c

c

a Expanded uncertainties at 95% confidence are U(T) = 0.02 K, U(P) = 1 kPa, U(w1) = 0.002, U(ρ) = 5.84 kg·m−3, U(α) = 0.02, and U(b3) = 0.1 mol·kg−1. bw1 is the mass fraction of MAE on a CO2-free basis as w1 = m1/(m1 + m2). cα is CO2 loading, which was defined as α = n3/n1, mole CO2/mol MAE, and the equivalent CO2 molality is b3 = n3/(m1 + m2) = αw1/M1, mol·kg−1.

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Table 4. Regressed Parameters for Redlich−Kister Equation in eqs 8 to 10 for the Density of MAE (1) + H2O (2)

a

T/K

A0

A1

A2

A3

293.15 298.15 303.15 308.15 313.15 318.15 323.15

−0.00172 −0.00280 −0.00285 −0.00220 −0.00068 0.00172 0.00510

0.05730 0.05435 0.05358 0.05365 0.05467 0.05682 0.06040

0.09607 0.09826 0.09853 0.09836 0.09717 0.09480 0.09143

0.04164 0.04540 0.04705 0.04741 0.04660 0.04436 0.04054

AARD %a 7.908 9.919 7.719 9.510 6.104 8.378 8.533

× × × × × × ×

10−3 10−3 10−3 10−3 10−3 10−3 10−3

n

AARD% = 100/n ∑k = 1 |ρkexp − ρkcal /ρkexp |

Table 5. Temperature Dependence Coefficient (ak) of Redlich−Kister Coefficients (Ak) for the Density of MAE (1) + H2O (2) A0 A1 A2 A3

a0

a1

1.5457 2.2277 −1.7761 −2.6228

−0.01027 −0.01422 0.01232 0.01737

a2 1.703 2.325 −2.024 −2.824

× × × ×

Figure 6. Density of CO2 unloaded aqueous MAE solution as a function of MAE mass fraction: Symbols refer to experimental data, and solid lines are calculated values by the Redlich−Kister equation in eqs 8 to 10 and the parameters in Table 5.

AARD % 10−5 10−5 10−5 10−5

1.858 0.223 0.131 0.451

loadings varying from 0 to 0.677 mol CO2/mol MAE. The physical solubility of N2O in aqueous MAE solution was measured in a stirred cell reactor over the temperature range of 289.31−348.18 K with MAE mass fraction w1 = 0.075, 0.15, 0.225, 0.30, 0.375, 0.45, 0.60, 0.75, and 1. The research objective of this work is first to obtain experimental data on physical property of aqueous MAE solutions as described above. Second, a series of models are described to correlate all the experimental data. The experimental density data for CO2 unloaded and loaded systems were correlated by Redlich−Kister equation16 as a function of temperature, MAE concentration and CO2 loading. Weiland’s model17 was used to predict the viscosity data of aqueous MAE solution. The solubility of N2O in MAE solution was correlated by using a empirical polynomial model,18 and compared with both the semiempirical model19 and Redlich−Kister equation.16

Figure 7. Parity plot of measured and predicted densities of CO2 unloaded MAE solution using the Redlich−Kister equation.

2. EXPERIMENTAL SECTION 2.1. Materials. MAE (≥99% purity, CAS No. 109-83-1) was obtained from Macklin company (Shanghai, China) and was used without further purification. The formula of MAE is CH3NHCH2CH2OH, and its structure is as shown in Figure 1. A series of unloaded MAE solutions were prepared by adding deionized water obtained from the Ultrapure Water System to a certain weighed quantities of MAE on an analytical balance (PA413, Ohaus Pioneer) with resolution of 0.0001 g. The concentration of MAE was validated by titration with standard HCl using methyl orange indicator. A variety of CO2-loaded solutions were prepared as follows: a large batch of amine of known concentration was made up, then loaded with CO2 by bubbling CO2 gas at 1 atm pressure through sintered glass Dreschel head for several hours until the solvent loaded to the desired CO2 loading. The extent of CO2 loading depended on the duration. The actual CO2 loading of the solution was verified by titration, of which the details of the experimental apparatus, procedure, and methods were described previously by Ji.20 CO2 and N2O were supplied by Changsha Rizhen Gas Co. Ltd., China, with purities of 99% and 99.99%, respectively. Descriptions of MAE, CO2, and N2O are given in Table 1.

Figure 8. Excess molar volumes of CO2 unloaded solution as a function of MAE mass fraction at various temperatures.

2.2. Density. In the present work, the densities of aqueous AME solution were measured by an Anton Paar DMA-4500 density meter with accuracy of 0.00001 g/cm3 for density and 0.01 K for temperature. The equipment was cleaned by acetone and methanol before injecting the sample. Also, before injection, the equipment was well dried. Injections, cleaning, and drying were done automatically. Before every sample measurement, calibration should be done by using distilled water, and the results were compared with the values provided by Anton Paar 132



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Table 6. Regressed Parameters of the Redlich−Kister Equation in eq 12, for the Density of MAE (1) + H2O (2) + CO2 (3) T/K

A0

A1

A2

A3

a

AARD %

293.15 298.15 303.15 308.15 313.15 318.15 323.15

0.01556 0.01575 0.01587 0.01600 0.01606 0.01608 0.01608

0.0338 0.0324 0.03165 0.03095 0.0306 0.0305 0.03084

0.01015 0.00870 0.00780 0.00730 0.00727 0.00760 0.00815

0.00120 0.00106 0.00096 0.00090 0.00088 0.00090 0.00095

2.2690 2.2650 2.2616 2.2565 2.2490 2.2427 2.2362

0.276 0.213 0.215 0.198 0.228 0.196 0.245

diagrams are shown in Supporting Information. The obtained density and viscosity values in this work were good agreement with those in the reference with AARDs of 0.33% and 5.55%, respectively. Thus, the obtained density and viscosity data in this work were reliable. 2.4. Solubility of N2O. The N2O solubility was measured in an apparatus which consists of a jacketed stirred glass reactor (VR) with volume of 2.358 L and a stainless steel gas holding vessel (Vv) with volume of 1.710 L, as show in Figure 3. Before the experiment, the reactor and the vessel were degassed by vacuum until the pressure was less than 1 kPa. Then a certain amount of amine solution (about half of the reactor volume, record as VS) was sucked into the reactor. Meanwhile, N2O was added to the gas holding vessel from a N2O cylinder. After vapor−liquid equilibrium was established at the set temperature, the pressures of reactor and gas holding vessel were recorded as PR1 and PV1, respectively. Then N2O gas was added into the reactor from a gas holding vessel by opening the valve between the reactor and the vessel just for a short period of time. Equilibrium was reached after several hours (but depend on temperature) with an agitation speed of 700 rpm. The pressure of reactor and vessel were recorded automatically and continuously using two pressure transducers with uncertainty of 0.1% of full scale (500 kPa). The temperature of reactor and

Table 7. Coefficient of the Temperature Dependence of Redlich−Kister Coefficients (Ak) for the Density of MAE (1) + H2O (2) + CO2 (3) A0 A1 A2 A3 a

a0

a1

−0.06103 0.63318 0.799438 0.076488 1.16037

0.00048267 −0.00381 −0.00507874 −0.00048227 0.00822

a2 −7.550 6.024 8.140 7.690 −1.514

× × × × ×

AARD % 10−7 10−6 10−6 10−7 10−5

0.120 0.164 0.781 0.464 0.027

in the instruction manual. The uncertainty should be accepted when the deviation between them were within ±0.00001 g/cm3. 2.3. Viscosity. The viscosity of aqueous AME solution was measured using Lovis 2000 M/ME from Anton Paar with an accuracy of 0.5% for viscosity and 0.02 K for temperature. Methanol and acetone were used to clean the equipment. Samples were prepared carefully and introduced to the X-sampler DMA 4500 M and Lovis 2000 at the same time, and the temperature conditions were set. In order to evaluate the instruments of density meter and viscometer, the density and viscosity of CO2-unloaded MAE solution measured at varied temperatures and concentrations in the present work were compared with the data in the available literature,21−25 as shown in Figure 2, and the comparison

Figure 9. Experimental density for CO2 loaded and unloaded MAE solution as a function of CO2 loadings at various temperatures for a: w1 = 0.075, b: w1 = 0.15, c: w1 = 0.225, d: w1 = 0.30. Symbols refer to experimental data, and solid lines are calculated values by eq 12. 133



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vessel were measured by two PT100 temperature probes with an uncertainty of ±0.1 K. The agitation was driven by a magnetic stirrer, and the agitation speed was controlled by the panel box. The total N2O added into the reactor was calculated by the pressure change of gas holding vessel before and after adding N2O, which can be described as = n Nadded 2O

VV ⎛ PV1 P ⎞ − V2 ⎟ ⎜ R ⎝ TV1Z1 TV2Z 2 ⎠

(2)

where PV1 and PV2 are the pressure of the vessel before and after feeding N2O (Pa); TV1 and TV2 are the temperatures of the vessel before and after adding N2O (K); Z1 and Z2 are the compressibility factors of N2O at the temperature of TV1 and TV2, respectively, which can be calculated by the Peng− Robinson equation of state. The amount of N2O in the gas phase of the reactor can be calculated by n Ng 2O =

PN2O(VR − VS) Z R RTR

(3)

where TR is the temperature of the reactor after reaching equilibrium, ZR is the compressibility factor of N2O in the reactor after reaching equilibrium, and VR and VS are the volumes of reactor and the added solvent. Also, PN2O is the partial pressure of N2O in the reactor which can be calculated by PN2O = PR2 − PR1

(4)

where PR1 is the pressure before feeding N2O at the set temperature of TR, which is the vapor pressure of the solvent at temperature of TR, and PR2 is the measured pressure of reactor after reaching equilibrium. The amount of N2O in the liquid phase can be calculated by the difference between N2O added and that in the gas phase, as given in eq 5.

n Nl 2O = n Nadded − n Ng 2O 2O

Figure 10. Deviations (ρexp − ρcal)/ρexp of experimental density data and calculated values from eq 12 with parameters from Table 7 as a function of (a: temperature, b: MAE mass fraction, c: CO2 loading).

(5)

The concentration of N2O in the liquid phase can be calculated by C N2O =

procedure are reliable and produce repeatable results. Consequently, it can be used to measure the solubility of gases in liquids.

n Nl 2O Vs

(6)

3. RESULTS AND DISCUSSION 3.1. Density. The measured density values of aqueous MAE solution in CO2 unloaded and loaded system at 293.15, 298.15, 303.15, 308.15, 313.15, 318.15, and 323.15 K with MAE mass fraction w1 = 0.075, 0.15, 0.225, and 0.30 and CO2 loading varying between 0 and 0.677 mol CO2/mol MAE are given in Table 3. As expected, the density decrease with increasing temperature and increase with the increasing CO2 loading, but the dependence of MAE concentrations is more complicated. The Redlich−Kister equation16 is frequently used to correlate properties of binary solutions such as the density, viscosity, refractive index, and N2O physical solubility of amine solution.26,29,30 In this work, the Redlich−Kister equation was used to correlate the density data for aqueous MAE solution at various concentrations, temperatures, and CO2 loadings. It is defined via the excess molar volume which can be found in eqs 8 to 10.

Therefore, the solubility is expressed by Henry’s law constant, as in the following equation

PN2O = He N2OC N2O

(7)

The unit of HeN2O is Pa·m3·mol−1. All of the operating conditions such as temperature and pressure were recorded and controlled by Labview software of the data acquisition system. To validate the solubility apparatus and the experimental procedure of this measurement, the solubility of N2O and CO2 in water at 289.03 to 351.43 K were measured and compared with the data in the available literature. The comparisons were made between the measurements obtained in this work and the experimental data of Hartono et al.,26 Versteeg et al.,18 Li et al.,27 and Tsai et al.,28 as listed in Table 2 and shown in Figure 4 for the solubility of CO2 and in Figure 5 for N2O in water, and the experimental data were shown in Supporting Information. It can be seen that the solubility values between the literature results and those of the present work are similar, which indicates that both the apparatus and the experimental

ρunloaded /kg·m−3 = 134

x1M1/kg·mol‐1 + x 2M 2 /kg·mol‐1 V /m 3·mol−1

(8)



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Table 8. Viscosity μ (mPa·s) of MAE (1) + H2O (2) + CO2 (3) with MAE Mass Fraction w1 = 0.075−0.30 (on a CO2-Free Basis) from T = 293.15 to 323.15 K and Different CO2 Loading α, and Equivalent CO2 Molality b3 at a Pressure of 101.325 kPaa T/K w1b

αc

b3c (mol·kg−1)

293.15

298.15

303.15

308.15

313.15

318.15

323.15

0.075

0.000 0.102 0.164 0.255 0.357 0.399 0.474 0.548 0.644 0.000 0.076 0.104 0.237 0.309 0.416 0.517 0.640 0.677 0.000 0.048 0.122 0.238 0.368 0.396 0.498 0.599 0.657 0.000 0.089 0.128 0.254 0.371 0.396 0.535

0.000 0.102 0.164 0.256 0.358 0.400 0.475 0.549 0.645 0.000 0.152 0.208 0.475 0.620 0.834 1.036 1.283 1.358 0.000 0.145 0.367 0.716 1.107 1.189 1.497 1.801 1.976 0.000 0.358 0.512 1.017 1.489 1.588 2.145

1.390 1.401 1.403 1.414 1.423 1.430 1.426 1.422 1.418 1.875 1.936 1.934 1.971 1.993 2.002 2.014 2.106 2.109 2.702 2.798 2.854 2.994 3.130 3.108 3.174 3.274 3.279 3.973 4.213 4.341 4.636 5.074 5.139 5.457

1.217 1.229 1.231 1.242 1.250 1.259 1.257 1.256 1.255 1.639 1.668 1.670 1.710 1.730 1.733 1.797 1.835 1.864 2.367 2.406 2.454 2.535 2.660 2.645 2.709 2.725 2.763 3.335 3.567 3.668 3.978 4.253 4.353 4.612

1.075 1.087 1.091 1.098 1.101 1.110 1.107 1.113 1.119 1.426 1.455 1.459 1.497 1.517 1.522 1.547 1.581 1.609 2.020 2.097 2.148 2.186 2.299 2.288 2.351 2.368 2.408 2.886 3.078 3.177 3.356 3.603 3.685 3.919

0.958 0.966 0.974 0.979 0.982 0.989 0.981 0.987 0.994 1.263 1.281 1.285 1.323 1.341 1.349 1.373 1.391 1.391 1.744 1.812 1.860 1.903 2.005 1.998 2.058 2.080 2.114 2.461 2.611 2.692 2.867 3.083 3.143 3.374

0.859 0.868 0.876 0.877 0.877 0.884 0.885 0.886 0.889 1.151 1.131 1.142 1.178 1.195 1.205 1.229 1.238 1.231 1.521 1.581 1.628 1.671 1.764 1.761 1.818 1.838 1.872 2.157 2.234 2.316 2.470 2.663 2.707 2.934

0.777 0.785 0.792 0.799 0.787 0.793 0.794 0.798 0.802 1.022 1.037 1.042 1.056 1.072 1.083 1.107 1.117 1.112 1.409 1.412 1.437 1.480 1.565 1.564 1.617 1.640 1.672 1.902 2.007 2.074 2.154 2.325 2.407 2.567

0.707 0.714 0.721 0.728 0.722 0.724 0.725 0.729 0.733 0.993 0.936 0.942 0.954 0.969 0.980 1.002 1.014 1.010 1.288 1.256 1.277 1.321 1.398 1.399 1.448 1.470 1.501 1.727 1.768 1.829 1.896 2.049 2.090 2.268

0.15

0.225

0.30

a Expanded uncertainties at 95% confidence are U(T) = 0.02 K, U(P) = 1 kPa, U(w1) = 0.002, U(μ) = 0.082 mPa·s, U(α) = 0.02, and U(b3) = 0.1 mol·kg−1. bw1 is the mass fraction of MAE on a CO2-free basis as w1 = m1/(m1 + m2). cα is the CO2 loading which was defined as α = n3/n1, mole CO2/mol MAE, and the equivalent CO2 molality is b3 = n3/(m1 + m2) = αw1/M1, mol·kg−1.

Table 9. Regressed Parameters for Weiland’s Model in eq 13 for the Viscosity of MAE (1) + H2O (2) + CO2 (3)

V E/m 3·mol−1 = V /m 3·mol−1 − (x1V1/m 3·mol−11 + x 2V2/m 3·mol−1)

(9)

a b c d e f g AARD %a

n

V E/m 3·mol−1 = 10−3 x1x 2 ∑ Ak (x1 − x 2)k k=0

(10)

where ρunloaded is the density of solution for CO2 unloaded system, V and VE are molar volume and excess molar volume, Vi, xi, and Mi are the molar volume, mole fraction, and molecular weight, respectively, for component i (1 for MAE, 2 for water). The adjustable parameters Ak are the Redlich−Kister coefficients, which are dependent on temperature. The regression results are presented in Table 4. The temperature dependence of the Redlich−Kister coefficients, Ak, can be represented by polynomials (eq 11). For the density of MAE (1) + H2O (2) system, a third-order polynomial was found sufficient when correlated by nonlinear regression. The regressed parameters are given in Table 5.

a

0.047932 11.072662 2.46365 1.58 × 10−6 0.013049 −0.0075732 2.38438 1.922 n

AARD% = 100/n ∑k = 1 |μkexp − μkcal | /μkexp . n

Ak =

∑ ak(T /Κ)k k=0

(11)

Figure 6 shows the experimental density data and calculated values by the Redlich−Kister equation as a function of MAE concentration at different temperatures. The calculated density from eqs 8 to 10 fitted the experimental data of this work very 135



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Figure 11. Experimental viscosity for CO2 loaded and unloaded MAE solution as a function of CO2 loading at various temperatures for a: w1 = 0.075, b: w1 = 0.15, c: w1 = 0.225, d: w1 = 0.30. Symbols refer to experimental data, and solid lines are calculated values by eq 13. ■, 293.15 K; ●, 298.15 K; ▲, 303.15 K; ▼, 308.15 K; ◆, 313.15 K; ◀, 318.15 K; ▶, 323.15 K.

Figure 9 shows the series of experimental density data and calculated values by eq 12 as a function of CO2 loading at different temperatures. The differences between the experimental and calculated values from eq 12 are plotted in Figure 10 as a function of temperature, MAE mass fraction, and CO2 loading. Based on Figures 9 and 10, it can be concluded that the calculated density from eq 12 fitted very well with the experimental data with producing an AARD of 0.231% and the largest deviations are less than 1%. 3.2. Viscosity. The experimentally measured viscosity of both CO2 unloaded and loaded aqueous MAE solution at different temperatures (293.15, 298.15, 303.15, 308.15, 313.15, 318.15, and 323.15 K) with MAE mass fractions of w1 = 0.075, 0.15, 0.225, and 0.30 and CO2 loadings varying between 0 and 0.677 mol CO2/mol MAE are listed in Table 8. The viscosity data were correlated by the model suggested by Weiland et al.,17 which can be expressed as

well, which indicates that the Redlich−Kister equation can be applied to correlate the density of CO2 unloaded MAE solution. Figure 7 is a parity plot of the experimental density data against the calculated results with eqs 8 to 10, which show an average absolute relative deviation (AARD) of 0.666%. As can be seen in Figure 6, the density becomes higher with increasing MAE concentration especially in the low temperature range. This behavior could be related to volume contraction when two liquid species mix. Figure 8 displays the concentration dependency of excess molar volumes at various temperatures. At all of the temperatures, the excess molar volume curves are negative and become more negative at the low temperatures. Negative excess molar volume values indicate a volume contraction when two liquid species mix. Pal et al.31 concluded that volume contraction is due to the ability of the −OH group to form hydrogen bonds with water molecules. Hydrogen bonds become weaker with increasing temperature, which results in less volume contraction. The ternary density data for CO2-loaded aqueous MAE solution can also be correlated by the Redlich−Kister equation if an item that describes how much CO2 is added in the solution is introduced, as reported by Zhang.32 This is shown in eq 12. ρ /kg·m−3 = ρunloaded /kg·m ‐3·(1 + aαx1)

μ/mPa·s μH O /mPa·s 2

⎛ [(aw1 + b)(T /K) + (cw1 + d)][α(ew1 + fT /K + g ) + 1]w1 ⎞ = exp⎜ ⎟ (T /K)2 ⎝ ⎠

(13)

where w1 is the mass fraction of MAE on a CO2-free basis (%), μ is the viscosity of the MAE solution, and μH2O is that of water, which is taken from Weast33 and shown in eq 14. The correlation parameters a−g are given in Table 9.

(12)

where ρ is the density of solution for CO2 loaded and unloaded system, α is CO2 loading (mole CO2/mol MAE), x1 is the mole fraction of MAE, and a is an adjustable parameter. The value of Ak and a can be obtained by fitting the experimental density data by Excel programming solving method at different temperatures. The regressed parameter, Ak, and the temperature dependence, ak, along with their corresponding values of AARD are given in Tables 6 and 7, respectively.

log

μH O /mPa·s 2

μH O,20 /mPa·s 2

=

1.322(20 − (T /K − 273.15) − 0.001053(T /K − 273.15 − 20)2 ) (T /K − 273.15) + 105

(14) 136



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Figure 11 shows the series of experimental viscosity data and calculated values by eq 13 as a function of CO2 loading at different temperatures. As can be seen in Figure 11, the viscosity of MAE solution increased with increasing MAE concentration and CO2 loading and decreased with increasing temperature. The deviations between the measured viscosity and the calculated values obtained from the Weiland’s model were also shown in Figure 12. It can be concluded

Table 10. Henry’s Law Constant of N2O in Pure MAE at Different Temperatures Ta T/K

HeN2O−MAE (Pa·m3·mol−1)

289.05 303.15 317.85 331.35 347.15

1137.4 1458.7 1820.6 2333.3 2886.8

a Expanded uncertainties at 95% confidence are U(T) = 0.02 K, U(P) = 1 kPa, and U(He) = 36 Pa·m3·mol−1.

Figure 13. Solubility of N2O in pure MAE, pure MEA,19 and pure MDEA.19 Symbols are experimental data, and solid lines are predicted results by eq 15.

⎛ b ⎞ He N2O − MAE/P ·m 3·mol−1 = b1 exp⎜ 2 ⎟ ⎝ T /K ⎠

(15)

As expected, HeN2O−MAE increased with temperature increasing. Conversely, the solubility of N2O in pure MAE decreased with temperature increasing. Moreover, comparisons were made between N2O in pure MAE and in pure MEA19 and pure MDEA,19 as shown in Figure 13. It can be seen that HeN2O in pure MAE is lower than that in pure MEA and MDEA, which indicates solubility of N2O in pure MAE is higher than that in pure MEA and MDEA. The values of b1 and b2 can be obtained by nonlinear regression, which can be established as b1 = 3.246 × 105 Pa·m3·mol−1 and b2 = −1638.57 K. 3.3.3. Solubility of N2O in Aqueous MAE Solution. The solubility of N2O in aqueous MAE solution at different MAE mass fractions w1 = 0.075, 0.15, 0.225, 0.30, 0.375, 0.45, 0.60, 0.75, and 1 were measured at different temperatures (289.31−348.18 K). The experimental results are given in Table 11 and plotted in Figure 14, and the experimental data were shown in Supporting Information. It can be observed that HeN2O in MAE solution increased with increasing temperature. The dependency of concentrations is more complex. Generally, HeN2O increases slowly with increasing MAE concentration in the lower concentration range at a given temperature but decreases with increasing MAE concentration in the higher concentration range and show a maximum value at around w1 = 0.35 to 0.45. This behavior could be explained on the basis of increasing density with increasing MAE concentration in the middle concentration range. A higher density or denser packing of solution results in less room for CO2 to dissolve in the solution.

Figure 12. Deviations (μexp − μcal)/μexp of experimental viscosity data and calculated values from eq 13 with parameters from Table 9 as a function of (a: temperature, b: MAE mass fraction, c: CO2 loading).

from Figures 11 and 12 that the average absolute relative deviation (AARD = 1.922%) between the predictions of the fitted correction and the measured values can be negligible in the chemical engineering calculations and the largest deviation was less than 8%. 3.3. Solubility of N2O. 3.3.1. Solubility of N2O in Pure MAE. The solubility data of N2O into pure MAE solvent at the temperature range from 289.05 to 347.15 K are presented in Table 10 and plotted in Figure 13, and the experimental data are shown in Supporting Information. The solubility of N2O in pure MAE solvent can be correlated as an exponential function proposed by Wang et al.,19 which can be expressed as follows: 137



Article

Table 11. Henry’s Law Constant HeN2O (Pa·m3·mol−1) of N2O in MAE Solution for MAE (1) + H2O (2) from T = 289.31 to 348.18 K and MAE Mass Fraction from w1 = 0.075 to 0.75a,b w1 0.075

0.15

0.225

0.30

0.45

0.60

0.75

3985.4 5676.7 6762.1 8178.7 9946.6

4161.3 5135.1 6226.5 6940.1 8253.0

2680.6 3619.9 4225.6 4838.9 6182.3

−1

HeN2O (Pa·m ·mol )

T/K 289.31 302.88 318.19 332.87 348.18

0.375 3

3467.3 5058.2 6529.2 8002.1 10750.0

3475.8 5423.1 6948.9 8642.9 11201.3

4094.8 5310.5 6557.9 8313.7 11428.0

4357.1 5316.3 6621.7 8317.1 11854.0

4044.2 5913.3 7204.2 8489.7 11532.0

Expanded uncertainties at 95% confidence are U(T) = 0.02 K, U(P) = 1 kPa, U(w1) = 0.002, and U(He) = 36 Pa·m3·mol−1. bw1 is the mass fraction of MAE on aqueous solution as w1 = m1/(m1 + m2). a

Table 13. Fitting Coefficients of Temperature-Dependence Coefficients (Ai) for Henry’s Law Constant of N2O in MAE (1) + H2O (2) by the Empirical Polynomial Model in eq 11 A0 A1 A2 A3 A4

a1

a2

AARD %

−29719.0 25313.0 −102991.5 239325.1 −142043.8

114.0 −85.2 417.5 −973.5 565.1

2.40 0.12 0.65 0.37 0.53

Figure 14. Henry’s law constant of N2O in MAE solution as a function of MAE mass fraction (w1) at different temperatures. Symbols refer to experimental data, and solid lines are predicted values by the empirical model from eq 16.

In addition, from the micro point of view, hydrogen bonds would be formed, and volume contraction will occur happen when two liquid species mix as mentioned in the Density section. The stronger the hydrogen bonds, the less the capacity for solvent to hold the gas, resulting in the increase in Henry’s law constant with increasing MAE concentration in the middle concentration range. In this paper, an empirical polynomial model was tested for the solubility of N2O in aqueous MAE solution. The empirical polynomial model, presented by Versteeg and Swaaij,18 is based on fitting the solubility data against the composition at different temperatures. This can be expressed as He N2O − MAE/Pa·m 3·mol−1 =

Figure 15. Parity plot of comparison between experimental data and predicted results of N2O solubility in aqueous MAE solutions by using different models.

i

∑ Aiw1

were regarded as sufficient. The regression results for Ai coefficients can be obtained by fitting the experimental solubility data with Excel programming solving method as a function of MAE concentration, which can be found in Table 12, and the predicted results are plotted in Figure 14.

(16)

i=0

where Ai are the temperature-dependent coefficients, which can be determined at a certain temperature by regression. For the N2O solubility in aqueous MAE solution, fourth-order polynomials

Table 12. Regressed Coefficient (Ai) for the Empirical Polynomial Model in eq 16 for Henry’s Law Constant of N2O in MAE (1) + H2O (2)

a

T/K

A0

A1

A2

A3

A4

AARD %a

289.31 302.88 318.19 332.87 348.18

3275.94 4818.64 6622.10 8178.82 11057.00

655.36 −501.70 −1805.83 −3057.55 −4338.6

17788.27 23167.34 29873.58 36205.40 41843.14

−42314.51 −54969.32 −70721.15 −85016.62 −99546.50

21625.65 28891.93 37163.04 46155.39 54262.59

5.015 4.119 3.624 1.481 4.213

n

AARD% = 100/n ∑k = 1 |Hekexp − Hekcal| /Hekexp. 138



Article

Team Development Plan (MOE-No. IRT1238), National Key Technology R&D Program (MOST-No. 2014BAC18B04), and China Outstanding Engineer Training Plan for Students of Chemical Engineering & Technology in Hunan University (MOE-No. 2011-40) are gratefully acknowledged.

The temperature dependence of the regressed coefficients, Ai, can be correlated by eq 11. For the solubility of MAE + H2O system, a second-order polynomial was found to be sufficient (shown in Table 13). Figure 15 is a parity chart that shows the deviation of experimental results and predicted value from eq 16 and Table 13. Comparing with that of semiempirical model and Redlich−Kister equation (shown in Supporting Information), it can be concluded that empirical polynomial model shows the best fitting result with an AARD of 4.54%, while the other two show AARDs of 6.41% and 5.06%, respectively.

Notes

The authors declare no competing financial interest.

■

4. CONCLUSIONS This paper reports experimental data for the density and viscosity of aqueous MAE solution over the temperature range of 293.15−323.15 K with MAE mass fraction w1 = 0.075, 0.15, 0.225, and 0.30 and CO2 loading between 0 and 0.677 mol CO2/mol MAE. Also, the N2O solubility into MAE solution over the temperature range from 289.31 to 348.18 K which covers the whole MAE concentration range in mass fraction is reported. Several models were used to correlate the experimental data. It can be concluded that 1. Density decreased with increasing temperature but increased with increasing CO2 loading. Also, density increased with MAE composition and increased especially at low temperatures. The density of CO2 unloaded and loaded aqueous MAE solution were fitted with the Redlich−Kister equation and show an AARD of 0.666% and 0.231%, respectively. 2. Viscosity increased with increasing MAE concentration and CO2 loading but decreased with increasing temperature. The CO2 unloaded and loaded viscosity data were correlated by Weiland’s model, and this yielded an AARD of 2.111%. 3. Henry’s law constant of N2O in aqueous MAE solution is strongly dependent on both the concentration and the temperature. Solubility data were correlated by an empirical polynomial model, with an AARD of 4.54%.

■

ASSOCIATED CONTENT

S Supporting Information *

The Supporting Information is available free of charge on the ACS Publications website at DOI: 10.1021/acs.jced.6b00504. Comparison diagram between density and viscosity data with the literature, experimental data for Henry’s Law constant, and correlation of solubility data by semiempirical model and Redlich−Kister equation (PDF)

■

REFERENCES

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AUTHOR INFORMATION

Corresponding Authors

*Tel.: +86-13618481627; fax: +86-731-88573033. E-mail address: [email protected] (Z. Liang). *Fax: +86-15116365674. E-mail address: [email protected] and [email protected] (P. Tontiwachwuthikul). ORCID

Zhiwu Liang: 0000-0003-1935-0759 Funding

The financial support of the National Natural Science Foundation of China (NSFC-Nos. U1362112, 21406057, 51521006, and 21536003), Natural Science Foundation of Hunan Province, China (No. 2016JJ2015), Innovative Research 139



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