Competitive adsorption and chromatography at supercritical conditions
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1 Research Collection Doctoral Thesis Competitive adsorption and chromatography at supercritical conditions Author(s): Ottiger, Stefan P. Publication Date: 2008 Permanent Link: Rights / License: In Copyright - Non-Commercial Use Permitted This page was generated automatically upon download from the ETH Zurich Research Collection. For more information please consult the Terms of use. ETH Library
2 Diss. ETH no COMPETITIVE ADSORPTION AND CHROMATOGRAPHY AT SUPERCRITICAL CONDITIONS Dissertation submitted to the ETH ZURICH for the degree of DOCTOR OF SCIENCES presented by Stefan Pascal Ottiger Chemical Engineer, ETH Zurich born on September 26 th, 1978 Citizen of Affoltern am Albis (Zurich) Accepted on the recommendation of Prof. Dr. Marco Mazzotti (ETH Zurich), examiner Prof. Dr. Giuseppe Storti (Politecnico di Milano), co-examiner Dr. Frieder Dreisbach (Rubotherm, Bochum), co-examiner Zurich 2008
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4 Abstract Measuring supercritical adsorption is difficult and represents a scientific and technical challenge. Compared to the adsorption of pure fluids, multicomponent adsorption is still less understood. The aim of this thesis is therefore to deepen our understanding of pure and competitive adsorption at near- and supercritical conditions, both from a fundamental point of view as well as in the light of the applications CO 2 storage by Enhanced Coalbed Methane Recovery (ECBM) and Supercritical Fluid Chromatography (SFC). For this purpose, a high-pressure setup to measure competitive adsorption based on a gravimetric-chromatographic technique has been successfully designed and built. The core of this setup is a magnetic suspension balance and the reliability of adsorption measurements at near-critical conditions depends on the homogeneity of the density in the measuring cell. Therefore, the impact of changing the way it is being thermostated has been investigated and an optimum configuration has been identified. The improved setup has subsequently been used to measure near- and supercritical adsorption isotherms of CO 2 on activated carbon, of CO 2 on 13X zeolite and of N 2O on silica gel. The obtained results have been carefully discussed in terms of effects observed in the vicinity of the critical point, namely critical adsorption and critical depletion. The recent interest in geological CO 2 storage is an area where the need for high-pressure competitive adsorption data on coal is increasingly felt. The possibility of enhancing the recovery of the trapped methane in these coal seams through the injection of CO 2, has added a commercial value to the storage of CO 2. However, the gases involved do not only adsorb in the coal pores, but also dissolve in the coal structure causing it to swell. Therefore, the first step towards a better knowledge of the ECBM process is to have reliable data on the adsorption equilibria of both single- and multicomponent mixtures of CO 2, CH 4 and N 2 on coal and its swelling behavior. This study was performed on a dried coal sample from the Sulcis Coal Province (SW, Italy) and the CO 2 uptake at reservoir conditions was found to be about 10 % of its III
5 mass. The competitive adsorption isotherms showed preferential adsorption of CO 2 over CH 4 and N 2. They have been described by a model based on lattice density functional theory (DFT), which is able to predict the ternary behavior based on the pure and binary adsorption equilibria. Finally, a highpressure view cell has been used to measure swelling, showing a maximum swelling of 4 % under CO 2 and 2 % under CH 4. The obtained results and the developed techniques are the firm basis for the design and implementation of future ECBM field tests. The second application studied in this thesis is SFC, where the solubility of supercritical CO 2 is enhanced by the addition of small fractions of organic modifiers. Since preparative separations are usually performed under overloaded conditions, the adsorption isotherm usually becomes non-linear. Therefore, the parameters of a binary Langmuir isotherm and their dependence on density and modifier concentration were determined with SFC for the separation of the enantiomers of 1-phenyl-1-propanol on Chiralcel-OD. IV
6 Zusammenfassung Adsorptionsmessungen unter überkritischen Bedingungen sind schwierig durchzuführen und stellen somit eine wissenschaftliche und technische Herausforderung dar. Die Adsorption von Gemischen ist im Vergleich zu derjenigen von reinen Fluiden immer noch weniger gut verstanden. Das Ziel dieser Dissertation ist es deshalb, unser Wissen über die Gemischadsorption bei nahund überkritischen Bedingungen zu erweitern. Dies geschieht nicht nur zur Grundlagenforschung, aber auch im Hinblick auf die beiden Anwendungen CO 2-Einlagerung in Kohleflözen mit gleichzeitig erhöhter Methangewinnung (ECBM) und Überkritischer Fluid-Chromatographie (SFC). Zu diesem Zweck wurde eine Hochdruckanlage zur Messung von Gemischadsorption basierend auf einer gravimetrisch-chromatographischen Methode erfolgreich geplant und gebaut. Das Herz dieser Anlage ist eine magnetische Schwebewaage und die Verlässlichkeit von nah-kritischen Adsorptionsmessungen hängt stark von der Homogenität der Dichte in dessen Messzelle ab. Aus diesem Grund wurde der Einfluss der Art der Thermostatisierung auf die Messung untersucht und eine optimale Konfiguration identifiziert. Diese wurde zur Messung von nah-kritischen Adsorptionsisothermen von CO 2 auf Aktivkohle und Zeolith 13X und von N 2O auf Kieselgel verwendet. Die erhaltenen Resultate in der Nähe des kritischen Punktes wurden dann eingehend diskutiert, insbesondere im Hinblick auf die sogenannten Effekte kritische Adsorption und kritische Depletion. Die geologische Einlagerung von CO 2 ist ein Bereich, in welchem Daten zur Hochdruck-Gemischadsorption benötigt werden. Die CO 2-Einlagerung in Kohleflözen kann auch wirtschaftlich attraktiv sein, da sie gleichzeitig zu einer erhöhten Erdgasproduktion führt. Die involvierten Gase werden jedoch nicht nur in den Kohleporen adsorbiert, sondern auch in der Kohlenstruktur gelöst, welches zu einem Anschwellen der Kohle führt. Deshalb stellt die Untersuchung der kompetitiven Adsorptionsgleichgewichte von CO 2, CH 4 und N 2 auf Kohle und dessen Anschwellen den ersten Schritt zu einem V
7 besseren Verständnis des ECBM Prozesses dar. Dafür wurde eine Kohleprobe aus der Sulcis Kohleprovinz (SW, Italien) verwendet und eine CO 2-Aufnahme von etwa 10 % ihrer Masse bestimmt. Die Gemisch-Adsorptionsisothermen haben bestätigt, dass CO 2 bevorzugt adsorbiert wird gegenüber CH 4 und N 2. Ausserdem wurden sie erfolgreich mit einem Modell basierend auf der Gitterdichte-Theory (DFT) beschrieben, welches das ternäre Verhalten aufgrund der reinen und binären Gleichgewichte vorhersagt. Das Anschwellen der Kohle wurde schliesslich in einer Hochdrucksichtzelle gemessen und maximale Werte von 4 % unter CO 2 und 2 % unter CH 4 festgestellt. Die erhaltenen Resultate und die entwickelten Methoden stellen die Basis für die Planung und Durchführung von zukünftigen ECBM Feldversuchen dar. Die zweite in dieser Dissertation behandelte Anwendung ist SFC, bei welcher die Löslichkeit von überkritischem CO 2 durch Zugabe von geringen Mengen an organischem Modifier erhöht wird. Da präparative Trennungen normalerweise unter überladenen Bedingungen durchgeführt werden, befindet man sich oft im nicht-linearen Bereich der Adsorptionsisothermen. Deshalb wurden für die Trennung eines chiralen Gemisches von 1-Phenyl-1-propanol auf Chiralcel- OD mittels SFC die Parameter der binären Langmuir-Isotherme und deren Abhängigkeit von Dichte und Modifierkonzentration bestimmt. VI
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