Calorimetric investigations. in multi-component salt systems
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1 Calorimetric investigations in multi-component salt systems D. Sergeev 1, E. Yazhenskikh 1, N. Talukder 1, D. Kobertz 1, K. Hack 2, M. Müller 1 1 Forschungszentrum Jülich, IEK GTT-Technologies 1
2 Sensible Thermal Energy Storage 2
3 Scheme of Solar Power Plant Receiver 600 C Heat transfer fluid (HTF) Hot Salt Thermal energy storage Cold Salt 280 C Heliostat Heat Exchanger Power Block Electricity 3
4 Scheme of Solar Power Plant Receiver Heat transfer fluid Heliostat Heat Exchanger Power Block Electricity 4
5 Thermal Energy Storage Receiver Project Name: Extresol 3 (EX 3) Country: Spain Start Year: m 14 m kg 40%KNO 3 60%NaNO 3 Solar Field Inlet Temp: 293 C Solar Field Outlet Temp: 393 C Solar Field Temp Difference: 100 C Storage Type: 2 tank indirect Storage Capacity: 7.5 hour(s) Thermal Storage Description: 28,500 tons of molten salt. 60% sodium nitrate, 40% potassium Heliostat nitrate. 1,010 MWh. Tanks are 14 m high and 36 m in diameter. Heat Exchanger Electricity Power Block 5
6 Enthalpy Increment Solar Field Inlet Temp: 293 C Solar Field Outlet Temp: 393 C Solar Field Temp Difference: 100 C 36 m 14 m Receiver 40KNO 3 60NaNO 3 Latent Heat at the melting point 221 C kg 40%KNO 3 60%NaNO 3 Heliostat Heat Exchanger Power Block Electricity 6
7 Enthalpy Increment Solar Field Inlet Temp: 293 C Solar Field Outlet Temp: 393 C Solar Field Temp Difference: 100 C 36 m Receiver 40KNO 3 60NaNO 3 14 m H H Sensible Latent kg 40%KNO 3 60%NaNO 3 Sensible T Heliostat Heat Exchanger Power Block Electricity 7
8 Cascaded Latent Heat Storage Temperature of HTF is decreasing T max T 2 T 1 T 1 T 4 T 3 T 2 T 3 HTF T min T max T 4 T min
![Phase Diagram of the NaCl KCl NaNO 3 KNO 3 system NaCl (801 o ) 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 KCl (771 o ) 657 C 0.8 0.9 0.9 0.8 Equivalent fraction Cl/(NO3+Cl) 0.3 0.4 0.5 0.6 0.7 scanned data [1] NaCl-KCl solid solution 0.](/docs-images/77/76269837/images/9-2.jpg "7 Univariant line 0.6 0.5 0.4 0.3 0.2 285 C 0.2 0.1 275 C 1 K 2 ClNO 3 (s) 0.1 (Na,K)NO3-HT solid solution NaNO 3 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.")
9 Phase Diagram of the NaCl KCl NaNO 3 KNO 3 system NaCl (801 o ) KCl (771 o ) 657 C Equivalent fraction Cl/(NO3+Cl) scanned data [1] NaCl-KCl solid solution 0.7 Univariant line C C 1 K 2 ClNO 3 (s) 0.1 (Na,K)NO3-HT solid solution NaNO KNO 3 (306 o ) Equivalent fraction K/(Na+K) (334 o ) R.N. Nyankovskaya, Izv. Sekt. Fiz. Khim. Anal., 21 (1952)
10 Reciprocal NaCl KCl NaNO 3 KNO 3 System NaCl (801 o ) KCl (771 o ) Equivalent fraction Cl/(NO3+Cl) scanned data [1] NaCl-KCl solid solution K 2 ClNO 3 (s) 0.1 (Na,K)NO3-HT solid solution NaNO KNO 3 (306 o ) Equivalent fraction K/(Na+K) (334 o ) [1] R.N. Nyankovskaya, Izv. Sekt. Fiz. Khim. Anal., 21 (1952)
11 Diagonal sections of the NaCl KCl NaNO 3 KNO 3 system KCl NaNO 3 NaCl KNO Liquid 650 liq_salt + (Na,K)NO3-HT + K 2 ClNO 3 (s) Liquid T, K liq_salt + (Na,K)Cl + (Na,K)NO3-HT III liq_salt + (Na,K)Cl V IV (Na,K)Cl + (Na,K)NO3-HT + (Na,K)NO3-LT (Na,K)Cl + (Na,K)NO3-HT II T, K 600 liq_salt + (Na,K)NO3-HT 550 IV liq_salt + (Na,K)Cl + (Na,K)NO3-HT III liq_salt + (Na,K)Cl 500 (Na,K)Cl + (Na,K)NO3-HT (Na,K)Cl + (Na,K)Cl#2 + (Na,K)NO3-HT II V (Na,K)Cl + (Na,K)Cl#2 + (K,Na)NO3-LT 350 (Na,K)Cl + (Na,K)NO3-LT + (K,Na)NO3-LT I 350 I KCl/(KCl+NaNO 3 ) (mol/mol) NaCl/(NaCl+KNO 3 ) (mol/mol) 7.5KCl 92.5NaNO NaCl 87.5KNO 3 11
12 Reciprocal NaCl KCl NaNO 3 KNO 3 system NaCl (801 o ) KCl (771 o ) Equivalent fraction Cl/(NO3+Cl) scanned data [1] NaCl-KCl solid solution 7.5KCl 92.5NaNO NaCl 87.5KNO C C K 2 ClNO 3 (s) 0.1 (Na,K)NO3-HT solid solution NaNO KNO 3 (306 o ) Equivalent fraction K/(Na+K) (334 o )
13 What does a thermochemist do? What my friends think What my chief thinks What my parents think What I really do 13
14 Sample Preparation Glove box Vacuum seal Closed glass containers 14
15 Differential Scanning Calorimetry DSC 404C Netzsch Sample holder 15
16 Differential Scanning Calorimetry Pans 0.7 C Experimental baseline Heater Constant heat rate K/min Theoretical baseline T, μv T, μv Differential thermocouple 16
17 Differential Scanning Calorimetry Pans 2.2 C DSC DSC Heater Constant heat rate K/min Sample (50 200mg) T, μv T, μv Differential thermocouple 17
18 Heat Capacity where m mass of the substance (g), DSC difference signal (μv, heat capacity of a reference. 18
19 DSC curves Reference: Sapphire, heat rate 10 K/min, Gas: nitrogen Reference: Sapphire, heat rate 10 K/min, Gas: helium 19
20 Heat capacity of the 12.5NaCl 87.5KNO 3 20
21 700 Heat capacity of the 12.5NaCl 87.5KNO3 Liquid liq_salt + (Na,K)NO3-HT + K2ClNO3(s) liq_salt + (Na,K)NO3-HT + (Na,K)Cl + (Na,K)NO3-HT V liq_salt + (Na,K)Cl + (Na,K)NO3-HT T, K liq_salt + (Na,K)Cl IV 550 III 500 (Na,K)Cl + (Na,K)NO3-HT (Na,K)Cl + (Na (Na,K)Cl + (Na,K)Cl#2 + (Na,K)NO3-HT 450 II 400 (Na,K)Cl + (Na,K)Cl#2 + (K,Na)NO3-LT 350 I NaCl/(NaCl+KNO3) (mol/mol) 21
22 Heat capacity of the 12.5NaCl 87.5KNO liq_salt + (Na,K)NO3-HT + K 3 2 ClNO 3 Liquid (s) T, K 600 liq_salt + (Na,K)NO3-HT 550 IV liq_salt + (Na,K)Cl + (Na,K)NO3-HT 500 (Na,K)Cl + (Na,K)NO3-HT (Na,K)Cl + (Na,K)NO3-HT III (Na,K)Cl + (Na liq_salt + (Na,K)Cl (Na,K)Cl + (Na,K)Cl#2 + (Na,K)NO3-HT 400 (Na,K)Cl + (Na,K)Cl#2 + (K,Na)NO3-LT II V? 350 I NaCl/(NaCl+KNO 3 ) (mol/mol)? 12 J mol 1 K 1 22
23 Heat capacity of the 7.5KCl 92.5NaNO Liquid liq_salt + (Na,K)Cl V T, K 500 liq_salt + (Na,K)Cl + (Na,K)NO3-HT III IV (Na,K)Cl + (Na,K)NO3-HT (Na,K)Cl + (Na,K)NO3-HT + (Na,K)NO3-LT II 350 (Na,K)Cl + (Na,K)NO3-LT + (K,Na)NO3-LT I KCl/(KCl+NaNO 3 ) (mol/mol) 23
24 Heat capacity of the 7.5KCl 92.5NaNO Liquid 3 T, K liq_salt + (Na,K)Cl + (Na,K)NO3-HT III liq_salt + (Na,K)Cl V IV (Na,K)Cl + (Na,K)NO3-HT? (Na,K)Cl + (Na,K)NO3-HT + (Na,K)NO3-LT II 350 (Na,K)Cl + (Na,K)NO3-LT + (K,Na)NO3-LT I KCl/(KCl+NaNO 3 ) (mol/mol)? 21 J mol 1 K 1 24
25 Drop Calorimeter mhtc 96 Seteram 25
26 Drop Calorimetric Detector Ceramic vessel Thermopile of 34 thermocouples Furnace thermocouple Reference 26
27 Sample (10 100mg) at room temperature Drop Calorimetry Heat Flow (μv) at a constant T Experimental data Hot zone, constant temperature T 27
28 Enthalpy Increment.. where m mass of the substance (g), measured peak area (μv s, (H T H ) r enthalpy increment of a reference. 28
29 Enthalpy increment in the 12.5NaCl 87.5KNO 3 29
30 Enthalpy increment of the 12.5NaCl 87.5KNO 3 mixture?? 12 J mol 1 K 1 30
31 Enthalpy increment of the 7.5KCl 92.5NaNO 3 mixture? DSC : Heat rate 10 K/min? 21 J mol 1 K 1 31
32 Calculation of C p in the FactSage, where φ is phase index, and n φ is phase fraction of each phase. 32
33 Enthalpy increment of the 12.5NaCl 87.5KNO 3 mixture,, 33
34 Enthalpy increment of the 12.5NaCl 87.5KNO 3 mixture 2.3 kj/mol 7.0 kj/mol 12.2 kj/mol 3.6 kj/mol 34
35 Drop Calorimetry Sample (1500 mg) in closed glass container Heat rate 0.5 K/min 35
36 Slow Heating Rate Thermal Analysis 36
37 Slow Heating Rate Thermal Analysis 37
38 Enthalpy increment of the 12.5NaCl 87.5KNO 3 mixture 3.9 kj/mol 3.6 kj/mol 38
39 Enthalpy increment of the 12.5NaCl 87.5KNO 3 mixture 4.5 kj/mol 7.7 kj/mol 12.2 kj/mol 39
40 Cascaded Latent Heat Storage NaCl KCl 282 C 335 C C 303 C C C C C C 221 C 335 C NaNO 3 KNO 3 40
41 Cascaded Latent Heat Storage Sensible 2x Latent Sensible Sensible Latent Sensible 40KNO 3 60NaNO 3 41
42 Conclusions Three calorimetric methods were used for determination of thermodynamic characteristics: DSC, DROP and SHRTA The combination of these methods allows calculating the phase transition enthalpies of continuous reactions DSC (Netzsch) usually gives lower results of phase transition enthalpies Calculated heat capacity cannot reproduce experimental data of phase transition regions Experimental and calculated data of enthalpy increment show very good agreement Our database allows for calculating of thermodynamic properties of the reciprocal NaCl KCl NaNO 3 KNO 3 system with a low uncertainty Four compositions on the univariant line suggested as potential PCMs 42
43 Jülich Solar Tower in NRW, Germany Money Isn t All You re Saving Thank you for your kind attention! 43
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