Exploring the Diversity and Dehydration Performance of New Mixed Tutton Salts (K2V1−xM’x(SO4)2(H2O)6, Where M’ = Co, Ni, Cu, and Zn) as Thermochemical Heat Storage Materials
Abstract
:1. Introduction
2. Materials and Methods
2.1. Crystals Growth
2.2. Structural Determination
2.3. Computational Studies
2.4. Thermoanalytical Studies
3. Results and Discussion
3.1. Structure Solving and Geometric Parameters
3.2. Analysis of Intermolecular Interactions by Hirshfeld Surfaces
3.3. Crystal Void Study
3.4. Thermal Characterization
3.5. Thermochemical Parameters via DSC Analysis
4. Conclusions
Supplementary Materials
Author Contributions
Funding
Data Availability Statement
Acknowledgments
Conflicts of Interest
References
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K2SO4 | VOSO4∙x(H2O) | M’SO4(H2O)n | Sample Code | ||||
---|---|---|---|---|---|---|---|
[g] | [mol/L] | [g] | [mol/L] | [g] | [mol/L] | ||
1.045 | 0.10 | 0.2505 | 0.05 | CoSO4(H2O)7 | 0.4216 | 0.05 | KVCoSOH |
1.045 | 0.10 | 0.2505 | 0.05 | NiSO4(H2O)7 | 0.4113 | 0.05 | KVNiSOH |
1.045 | 0.10 | 0.2505 | 0.05 | CuSO4(H2O)5 | 0.3745 | 0.05 | KVCuSOH |
1.045 | 0.10 | 0.2505 | 0.05 | ZnSO4(H2O)7 | 0.4313 | 0.05 | KVZnSOH |
Sample | KVCoSOH | KVNiSOH | KVCuSOH | KVZnSOH |
---|---|---|---|---|
Formula | H12K2V0.48Co0.52O14S2 | H12K2V0.47Ni0.53O14S2 | H12K2V0.44Cu0.56O14S2 | H12K2V0.49Zn0.51O14S2 |
Formula weight [g/mol] | 433.51 | 433.46 | 436.41 | 436.73 |
a [Å] | 9.033(4) | 8.985(3) | 9.094(2) | 9.028(7) |
b [Å] | 12.171(8) | 12.148(7) | 12.144(7) | 12.196(5) |
c [Å] | 6.144(7) | 6.118(8) | 6.164(9) | 6.154(7) |
α [°] | 90.00 | 90.00 | 90.00 | 90.00 |
β [°] | 104.78(7) | 104.97(4) | 104.41(6) | 104.64(9) |
γ [°] | 90.00 | 90.00 | 90.00 | 90.00 |
Volume [Å3] | 653.12(6) | 645.26(4) | 659.42(7) | 655.59(7) |
Crystalline system | Monoclinic | Monoclinic | Monoclinic | Monoclinic |
Space group | P21/a | P21/a | P21/a | P21/a |
Rwp [%] | 8.33 | 9.32 | 9.59 | 9.89 |
Rp [%] | 6.28 | 7.02 | 7.97 | 7.35 |
S | 1.11 | 1.07 | 1.65 | 1.10 |
KVCoSOH | KVNiSOH | KVCuSOH | KVZnSOH | ||||
---|---|---|---|---|---|---|---|
Bond | Length [Å] | Bond | Length [Å] | Bond | Length [Å] | Bond | Length [Å] |
V/Co–O5 | 2.116(7) | V/Ni–O5 | 2.071(2) | V/Cu–O5 | 2.129(3) | V/Zn–O5 | 2.122(2) |
V/Co–O6 | 2.127(8) | V/Ni–O6 | 2.079(8) | V/Cu–O6 | 2.133(4) | V/Zn–O6 | 2.129(3) |
V/Co–O7 | 2.031(2) | V/Ni–O7 | 2.014(5) | V/Cu–O7 | 2.030(1) | V/Zn–O7 | 2.029(3) |
S1–O1 | 1.472(5) | S1–O1 | 1.474(2) | S1–O1 | 1.470(2) | S1–O1 | 1.473(2) |
S1–O2 | 1.456(3) | S1–O2 | 1.463(2) | S1–O2 | 1.469(2) | S1–O2 | 1.462(2) |
S1–O3 | 1.471(9) | S1–O3 | 1.473(1) | S1–O3 | 1.485(2) | S1–O3 | 1.479(2) |
S1–O4 | 1.47(8) | S1–O4 | 1.479(2) | S1–O4 | 1.481(3) | S1–O4 | 1.479(3) |
Sample | Bond Angle [°] | |||
---|---|---|---|---|
M’ = Co, Ni, Cu, and Zn | KVCoSOH | KVCoSOH | KVCoSOH | KVCoSOH |
O5–V/M’–O5 * | 180.0(0) | 180.0(0) | 180.0(0) | 180.0(0) |
O5–V/M’–O6 * | 180.0(0) | 180.0(0) | 180.0(0) | 180.0(0) |
O5 *–V/M’–O6 * | 180.0(0) | 180.0(0) | 180.0(0) | 180.0(0) |
O5–V/M’–O6 | 180.0(0) | 180.0(0) | 180.0(0) | 180.0(0) |
O5 *–V/M’–O6 | 91.0(3) | 91.0(3) | 91.0(3) | 91.0(3) |
O5 *–V/M’–O7 * | 88.4(8) | 88.4(8) | 88.4(8) | 88.4(8) |
O5–V/M’–O7 | 89.3(3) | 89.3(3) | 89.3(3) | 89.3(3) |
O5–V/M’–O7 * | 91.3(4) | 91.3(4) | 91.3(4) | 91.3(4) |
O5 *–V/M’–O7 | 88.9(7) | 88.9(7) | 88.9(7) | 88.9(7) |
O6–V/M’–O6 * | 91.5(2) | 91.5(2) | 91.5(2) | 91.5(2) |
O6 *–V/M’–O7 * | 90.6(7) | 90.6(7) | 90.6(7) | 90.6(7) |
O6–V/M’–O7 * | 88.6(6) | 88.6(6) | 88.6(6) | 88.6(6) |
O6 *–V/M’–O7 | 88.9(7) | 88.9(7) | 88.9(7) | 88.9(7) |
O6–V/M’–O7 | 91.5(2) | 91.5(2) | 91.5(2) | 91.5(2) |
O1–S1–O2 | 90.6(7) | 90.6(7) | 90.6(7) | 90.6(7) |
O1–S1–O3 | 88.6(6) | 88.6(6) | 88.6(6) | 88.6(6) |
O1–S1–O4 | 91.0(3) | 91.0(3) | 91.0(3) | 91.0(3) |
O2–S1–O3 | 88.4(8) | 88.4(8) | 88.4(8) | 88.4(8) |
O2–S1–O4 | 89.3(3) | 89.3(3) | 89.3(3) | 89.3(3) |
O3–S1–O4 | 91.3(4) | 91.3(4) | 91.3(4) | 91.3(4) |
Sample | Unit Cell [Å3] | Voids [Å3] | Voids [%] | Voids Surface Area [Å2] | Globularity | Asphericity |
---|---|---|---|---|---|---|
KVCoSOH | 653.12 | 4.13 | 0.63 | 24.17 | 0.51 | 0.46 |
KVNiSOH | 645.26 | 3.41 | 0.53 | 21.32 | 0.46 | 0.47 |
KVCuSOH | 659.42 | 5.31 | 0.81 | 28.52 | 0.51 | 0.43 |
KVZnSOH | 655.59 | 4.98 | 0.76 | 27.42 | 0.47 | 0.44 |
Sample | TG | DTA | ||||
---|---|---|---|---|---|---|
ΔT [°C] | Weight Loss [%] | Weight Loss [g/mol] | Molecular Fragment | Tpeak [°C] | Thermal Event | |
KVCoSOH | 74–220 | 24.37 | 105.6 | ≈6 H2O | 85 | dehydration |
134 | dehydration | |||||
187 | dehydration | |||||
220–900 | 23.65 | 102.5 | ≈SO3 + O | 316 | crystallization | |
749 | transition | |||||
765 | V/CoSO4 melting | |||||
KVNiSOH | 85–200 | 24.01 | 104.3 | ≈6 H2O | 138 | dehydration |
200–900 | 19.98 | 73.6 | ≈SO3 | 378 | crystallization | |
520 | -- | |||||
575 | transition | |||||
635 | V/NiSO4 melting | |||||
798 | decomposition | |||||
KVCuSOH | 57–220 | 24.55 | 107.1 | ≈6 H2O | 71 | dehydration |
141 | dehydration | |||||
220–900 | 16.88 | 73.6 | ≈SO3 | 528 | transition | |
KVZnSOH | 55–220 | 25.01 | 109.18 | ≈6 H2O | 85 | dehydration |
130 | dehydration | |||||
220–900 | 19.92 | 86.99 | ≈SO3 | 499 | -- | |
515 | transition | |||||
565 | V/ZnSO4 melting |
Sample | Tpeak [°C] | ΔHexp [kJ/mol] | ΔHexp [kJ/H2O mol] | MMSalt [g/mol] | ρSalt [g/cm3] | ΔHV [GJ/m3] |
---|---|---|---|---|---|---|
KVCoSOH | 87, 161, and 172 | 189.50 | 31.58 | 433.495 | 2.224 | 0.972 |
KVNiSOH | 135 | 360.09 | 60.02 | 433.448 | 2.210 | 1.836 |
KVCuSOH | 67 and 128 | 220.30 | 36.72 | 436.398 | 2.163 | 1.091 |
KVZnSOH | 90 and 126 | 145.85 | 24.31 | 436.703 | 2.248 | 0.751 |
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Oliveira Neto, J.G.d.; Marques, J.V.; Santos, J.C.d.; Santos, A.O.d.; Lang, R. Exploring the Diversity and Dehydration Performance of New Mixed Tutton Salts (K2V1−xM’x(SO4)2(H2O)6, Where M’ = Co, Ni, Cu, and Zn) as Thermochemical Heat Storage Materials. Physchem 2024, 4, 319-333. https://doi.org/10.3390/physchem4030022
Oliveira Neto JGd, Marques JV, Santos JCd, Santos AOd, Lang R. Exploring the Diversity and Dehydration Performance of New Mixed Tutton Salts (K2V1−xM’x(SO4)2(H2O)6, Where M’ = Co, Ni, Cu, and Zn) as Thermochemical Heat Storage Materials. Physchem. 2024; 4(3):319-333. https://doi.org/10.3390/physchem4030022
Chicago/Turabian StyleOliveira Neto, João G. de, Jacivan V. Marques, Jayson C. dos Santos, Adenilson O. dos Santos, and Rossano Lang. 2024. "Exploring the Diversity and Dehydration Performance of New Mixed Tutton Salts (K2V1−xM’x(SO4)2(H2O)6, Where M’ = Co, Ni, Cu, and Zn) as Thermochemical Heat Storage Materials" Physchem 4, no. 3: 319-333. https://doi.org/10.3390/physchem4030022