Measurement Methods for Single- and Multi-Component Gas Adsorption Equilibria

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1 Measureent Methods for Single- and Multi-Coponent Gas Adsorption Equilibria JUERGEN U. KELLER, FRIEDER DREISBACH 1), NADIA IOSSIFOVA, MARC SEELBACH, WOLFGANG ZIMMERMANN AND REINER STAUDT 2) Inst. Fluid- and Therodynaics, University of Siegen, D Siegen, Gerany 1) Rubother GbH, Bochu, Gerany 2) Inst. Non-Classical Cheistry, University of Leipzig, Leipzig, Gerany 1) 2) 1. Voluetry / Manoetry and Densietry 2. Gravietry and Densietry 3. Oscilloetry 4. Ipedance Spectroscopy 5. Calorietry and Voluetry 6. Calorietry and Spectroscopy Acknowledgeents

2 Voluetry/Manoetry and Densietry 94,22547 g Microbalance Magnetic Suspension Adsorption Chaber Peranent Magnet T Manoeter p Therostat Storage Vessel 1 Gas Supply Syste V AC Sinker T Theroeter Sorbent Storage Vessel 2 T Vacuu Pup Gas Circulation Pup Instruent for voluetric-densietric easureents of binary coadsorption equilibria of gas ixtures on porous solids without using a gas chroatograph. The sorptive gas prepared in the syste is assued to be a binary ixture with known initial olar concentrations (y* 1, y* 2 ). IFT University of Siegen, 2002.

3 Mass balances EOS Sorptive gas asses f f (, ) 1 2 (1 4) a * f i i i * * * yi p VSV i * R T Z M f f f * as 1 2 V V f f 1 2 p V i * as 1 2 i i f i f f 1 2 as s i 1, 2 (1) * * Z Z p,t, y i V M M R T Z p,t, w w V V He i 1, 2 (2) (3) (4) (5) DVMs / Theory M p M V V a * i f i 1 * s ige i He Mi Mi 1 R T Z p,t, wi (6)

4 Scheatic Diagra DGMs Installation for DGMs of Binary Coadsorption Equilibria of Preixed * * Gases (y 1, y 2 )

5 First Instruent MSB (3) First perforance of DGMs using a MSB (3) on in Lab PB-A0126 of IFT/USI

6 Mass balances Total gas ass supplied a * f i i i i 1, 2 (1) * * * a a f f * f * V * * * i wi (2) (2A) Sorptive gas asses (1, 2A, 3, 4) f f f * as 1 2 V V f f 1 2 p V * as V M M R T Z p,t, w 1 2 i as s V V He (3) (4) (5) DGMs / Theory M p M V V a * i f i 1 * s ige i He Mi Mi 1 R T Z p,t, wi (6)

7 n CO2, n tot = n CO2 + n CH4 [ol/g] University of Siegen Diagra CO2/CH n tot = n CO2 + n CH4 n CO2 y f CO2 : y f CH4 = : T = 293 K AC D 47/ Pressure p [MPa] Coadsorption equilibria of CO / CH at T 293K, y 20.4%ol, y 79.6%ol 2 4 CO CH 2 4 on AC D47 /3. Correlation by GAI : n n (bp) i 1 (bp) i, i CO, CH i i 2 4

8 Scheatic Diagra OVMs Gas supply Rotational Pendulu p p Microbalance T Polyer Sorbent T Sorption Chaber Sorption Chaber Vacuu Pup Gas Circulation Pup Experiental setup for oscilloetric-gravietric easureents

9 Theory OscilloetricMs Ideal Pendulu s 2 E E 1 2 s, 1 s E E 0 0 * * 2 1 * s Physical Pendulu,, * * *,... epty pendulu, vacuu 0 0 E * s,... pendulu and adsorbent,, vacuu E * s,... pendulu, adsorbent, adsorbate,,, gas Oscilloetric easureents of gas adsorption equilibria. Theory

10 Photo ring slit of rot. pendulu Ring slit of rotational pendulu filled with polycarbonate pellets

11 Swelling and sorption isothers of PC/CO2 g/g] a [g/g] 250 V as / ( a + s ) grav osc a V as / ( a + s ) [c 3 /g] p [MPa] Swelling and sorption isother of polycarbonate / CO 2 at 293 K

12 Gas Supply Gas Circulation Pup Capacitor Scheatic Diagra Vol-Diel-Ms p p * T * Storage Vessel V * T Adsorption Chaber Sorbent S Ipedance Analyzer IA Gas Chroatograph Vacuu Pup V, M DE MG * V (p,t) * V DE MG as f (p,t), Experiental setup for voluetric-dielectric easureents V as V He

13 Ipedanc Spectra (DAY/CO2) 5.6e e-12 Vakuu 0.01 MPa MPa MPa MPa MPa C/ F 5.4e e e e f/ khz Ipedance spectra of CO 2 on zeolite (DAY), T=298K

14 Uptake Curves MS13X/H2S 6 5 Ipedance spectroscopy Gravietry Relative uptake Tie [h] Uptake curves of H 2 S on MS 13X, T=298K

15 Scheatic Diagra SGC Scheatic diagra of a Sensor Gas Calorieter (SGC)

16 Difference Pressure [Pa] Electrical Power [W] University of Siegen Calibration SGC Tie [s] Calibration experients in the SGC 0.5J to 5J Sensor gas N 2 (1.6bar), T=298K, =10s Oh s heat release (red lines) Pressure signal (blue lines)

17 Differential heat of adsorption [kj/ol] Integral heat of adsorption [J/g] University of Siegen Heat of adsorption Na13X/CO Integral heat of adsorption Polynoal Interpolation Differental heat of adsorption Derivative of polynoial interpolation of the integral heat of adsorption Heat of Condensation for CO 2 (5,25 kj/ol) CO 2 ads. [ol/g] Heat of adsorption for CO 2 / Na13X, T=298K

18 Scheatic Diagra GSC with Capacitor Scheatics of cobined calorietric-dieletric-voluetric gas adsorption easureents Capacitor Ipedance Analyzer

19 (CI) h h0 Be bp H h0 B ( ) A 0 ba (DI) h h 0 h B H 0 Ae A ap 0 ba i k ba ( ) H h 0 0 B * A ) H h b,b a,b,a,b, H, a,a a,b,a,b, H, Min 2 i 2 k a, A, b, B (* ) Calculation of absolute adsorbed asses fro DE-C-easureents

20 Absolute and Gibbs excess asses DAY/CO2 g/g p [hpa] Absolute asses ( a ) and Gibbs excess asses ( GEV, GEG ) of CO 2 adsorbed on wessalite (DAY-zeolite) at T=298K a... Dielectric Caloric Meas. (RS, ESch, JUK)... Voluetry, He Vol. (ESch) GEV... Gravietry, He Vol. (RS) GEG

21 Gas Mixture Sorption Measureent Methods

22 Therodynaic-conference Würzburg GVC-GET Therodynaic-Conference Würzburg, 2001

Comparison of commercial and new developed adsorbent materials for pre-combustion CO 2 capture by pressure swing adsorption

Comparison of commercial and new developed adsorbent materials for pre-combustion CO 2 capture by pressure swing adsorption Johanna Schell, Nathalie Casas, Lisa Joss, Marco Mazzotti - ETH Zurich, Switzerland