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This setup, shown in figure 1, allowed an investigation of hydration characteristics in addition to the dehydration of several thermochemical storage materials like MgCl2*6 H2O, Ca(OH)2, Zeolites and composite materials. PREPARATION OF COMPOSITE MATERIALS Composite materials as discussed in this paper were prepared from MgCl2 * 6 H2O (p.A., Merck) and graphite (p.A., Merck), copper (p.A., Merck), zeolite A and sand, respectively. For this purpose, portions of approximately 250 mg of MgCl2 * 6 H2O were mixed using mortar and pestle with similar amounts of the additive. The zeolite A was purchased from Süd Chemie AG, Moosburg, Germany. The sand used was sieved at < 250 μm before use. Grain size distribution analysis revealed a > 80% contribution of 125 – 250 μm grain size. The amounts of MgCl2 * 6 H2O in the composites were calculated from Mg measurements using Inductively Coupled Plasma – Optical Emission Spectroscopy (ICP-OES) at 285.213 nm after sonification of the composite in 10 mL hydrochloric acid (37%) for 30 min and subsequent filtration and dilution to 100 mL. PEAK POWER DEPENDENCY ON WATER VAPOUR PRESSURE AND AMOUNT OF SAMPLE USED In order to assess the dependency of the hydration reaction of MgCl2 * 6 H2O on water vapour pressure and the amount of sample used, measurements of the hydration heat fluxes of samples of 2.5, 5, 7.5 and 15 mg mass were taken out at different moist nitrogen flows ranging from 25 – 150 mL / min, corresponding to a water vapour pressure in the oven ranging from 12-22 hPa during hydration at 35°C. The temperature program used for dehydration of the samples prior to the hydration was set to ramp up from 35°C to 130°C at 1°C / min, and then to cool down at -5°C / min to 35°C. Data handling was done using the Mettler Toledo STARe Software 9.20. INFLUENCE OF HEATING RATES AND ADDITIVES ON THE DEHYDRATION TEMPERATURES Influences of graphite, zeolite, copper and sand on the dehydration reaction were investigated using a temperature program starting at 25°C and heating up to 200°C at 1°C / min. For a MgCl2 : Graphite – composite, we used 0.1°C / min and 5°C / min in addition to the measurements with 1°C / min heating rates. The onset, peak and offset temperatures of the different dehydration stages were obtained using the Mettler Toledo STARe Software 9.20. CYCLING STABILITY Investigations on the cycling stability of the TCM materials and material composites were done by multiple measurements of the integrated hydration heat fluxes of one sample during consecutive dehydration/hydration cycles. The hydration process was conducted at 35°C. The moist nitrogen gas flow was set to 125 mL/min and switched on after a settling time of 5 min to start the hydration of the sample. For dehydration, the same temperature program as for the peak power measurements was used. The amount of sample used was around 10 mg. Integration of the hydration heat fluxes over time was done manually using the Mettler Toledo STARe Software 9.20. RESULTS AND DISCUSSION During method development, problems were observed regarding residual water in the reaction chamber, leading to lower energy recovery rates due to re-hydration during cool down of the TGA/DSC-oven and a heat flow of > 0 at the start of the hydration measurements, which rendered proper integration of the peak difficult. Care must be taken to ensure the use of proper dried nitrogen as a purge gas and avoid leakage in the gas supply system. Measured heat storage capacities of the investigated materials were within range of data available in the literature, showing around 1400 kJ/kg for Ca(OH)2 and 940 kJ/kg for MgCl2*6 H2O [11, 14]. HeatPDF Image | THERMOCHEMICAL STORAGE MATERIALS RESEARCH
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