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Substitute Natural Gas Production with Direct Conversion of Higher Hydrocarbons

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Substitute Natural Gas Production with Direct Conversion of Higher Hydrocarbons Substitute Natural Gas Production with direct Conversion of Higher Hydrocarbons Erzeugung von Substitute Natural Gas mit direkter Umsetzung von höheren Kohlenwasserstoffen Der Technischen Fakultät der Universität Erlangen-Nürnberg zur Erlangung des Grades DOKTOR-INGENIEUR vorgelegt von Christoph Baumhakl aus Graz Als Dissertation genehmigt von der Technischen Fakultät der Friedrich-Alexander-Universität Erlangen-Nürnberg Tag der mündlichen Prüfung: 25.07.2014 Vorsitzende des Promotionsorgans: Prof. Dr.-Ing. habil. Marion Merklein Gutachter: Prof. Dr.-Ing. Jürgen Karl Prof. Dr. Wilhelm Schwieger Vorwort/Acknowledgement Die vorliegende Arbeit entstand im Zuge meiner Tätigkeit als wissenschaftlicher Mitarbeiter am Institut für Wärmetechnik der Technischen Universität Graz und am Lehrstuhl für Energieverfahrenstechnik der Friedrich-Alexander-Universität Erlangen-Nürnberg. Ich möchte an dieser Stelle ganz herzlich Herrn Prof. Jürgen Karl für seine Betreuung und Unterstützung bei dieser Arbeit bedanken. Im Besonderen aber auch für das optimale Arbeitsumfeld und den Freiraum, der mir im Rahmen meiner Arbeit geboten wurde und maßgeblich zum Gelingen beitrug. Besonderer Dank gilt auch Herrn Prof. Wilhelm Schwieger für die Übernahme des Zweitgutachtens. Großen Dank schulde ich meinem Mitstreiter im Kampf mit Vergasungsanlagen, Dr. Thomas Kienberger, für die Einführung in die Vergasung und Methansynthese und die langen Diskussionen. Meinen ehemaligen Kollegen, Dr. Lorenz Griendl, Dr. Martin Hauth, Bernhard Gatternig und Dr. Andreas Schweiger danke ich ganz herzlich für ihre Hilfestellung beim Bau und Betrieb von Versuchsanlagen. Natürlich danke ich auch allen meinen anderen Kollegen für ihre Hilfe und offenen Ohren und das freundschaftliche Verhältnis. So eine Arbeit wäre ohne die Mitarbeit von Studenten im Rahmen von verschiedensten Abschlussarbeiten nicht durchführbar. Dafür möchte ich ihnen auch ganz herzlich Danke sagen. Großer Dank gilt natürlich meinen Eltern und meiner Familie, durch deren Motivation und finanziellen Unterstützung meiner Ausbildung, ich erst so weit kommen konnte um diese Doktorarbeit zu erstellen. Dir Katrin gilt mein größter Dank; dass Du mich immer aufgeheitert und auf andere Gedanken gebracht hast und ich durch Dich immer wieder aufs Neue zu meiner Arbeit motiviert worden bin. Nürnberg, im April 2014 Christoph Baumhakl A part of the research leading to these results has received funding from the European Community’s Research Fund for Coal and Steel (RFCS) under grant agreement n° RFCR-CT-2009-00003. III IV Abstract Abstract This thesis gives a contribution to develop a methanation process for production of Substitute Natural Gas (SNG) in small-scale, decentralized facilities. Smaller plant sizes require a reduction of the plant complexity. Therefore, a reduced gas cleaning and simplified methanation process is proposed. A reduced gas cleaning effort results in remaining of certain contaminations in the synthesis gas. Consequently, the methanation catalyst must be able to deal with these species. To investigate the influence of contaminations on the methanation, suitable test setups were constructed to validate these influences experimentally. The tests were performed with artificial, bottle-mixed synthesis gas as well as with real synthesis gas from allothermal gasification of biomass and lignite. The gas composition for the tests with bottle-mixed syngas bases mainly on results from gasification tests. In a first step, bench-scale methanation tests with clean, bottle-mixed synthesis gas prove the proposed polytropic fixed bed reactor concept for methanation. Results from long-term tests show a full-conversion respectively yield down to 230°C without deactivation of the catalyst. Due to the polytropic operation of the reactor, a temperature peak originates at its inlet. It is assumed that this temperature peak provides the required heat for conversion of higher hydrocarbons. The lab-scale tests with contaminated synthesis gas investigate the influence of typical synthesis gas contaminations such as ethylene, tars and hydrogen sulfide. The tests confirm that higher hydrocarbons are directly converted within methanation. Conversion tests with ethylene and tars showed that they fully convert within the first centimeters of the reactor. Main problem thereby is the coking of the catalyst. Addition of higher 0.5 vol. % ethylene results in severe coking, whereas only minor coking occurred by addition of a representative tar mixture with a concentration of 6-12 g/Nm³. The amount of deposited carbon depends on the reactor temperatures and the water content of the syngas. A combined conversion of ethylene and tars showed lower coking compared to conversion of ethylene only. A further lowering as well as prevention of carbon deposition is possible by addition of traces (< 1 ppm) of hydrogen sulfide. In the last step, the whole SNG production process, containing gasification, gas cleaning and methanation is demonstrated in bench-scale. The simplified gas cleaning removes sufficiently dust, alkalis and sulfur species such as H2S and COS, but has probably weaknesses with organic sulfur. Therefore, the measured catalyst deactivations are high, which requires further improvements. Promising is the almost full conversion of tars during methanation with real synthesis gas. V Kurzfassung Kurzfassung Diese Arbeit beschäftigt sich mit verschiedenen Aspekten zur Entwicklung eines Prozesses zur Erzeugung von Substitute Natural Gas (SNG) in kleinen, dezentralen Anlagen. Um auch im kleineren Leistungsbereich wirtschaftlich sein zu können, muss die Anlagenkomplexität reduziert werden. Daher wird in dieser Arbeit ein Prozess mit einer reduzierten Gasreinigung und vereinfachter Methanisierung vorgeschlagen. Durch den reduzierten Gasreinigungsaufwand verbleiben bestimmte Verunreinigungen im Synthesegas und beeinflussen die Methanisierung. Zur Untersuchung des Einflusses von Verunreinigungen auf die Methansynthese wurden geeignete Versuchsanordnungen aufgebaut und die Einflüsse experimentell ermittelt. Dabei sind sowohl künstliche, flaschengemischte Synthesegase aber auch reale Synthesegase aus der thermischen Vergasung verwendet worden. Die Gaszusammensetzung bei den Tests mit flaschengemischten Gasen basiert hauptsächlich auf Ergebnissen aus Vergasungstests. In einem ersten Schritt bestätigen Tests mit sauberen, flaschengemischten Synthesegasen die Eignung des vorgeschlagenen polytropen Festbettreaktor Konzepts für die Methanisierung. Langzeittests zeigen eine Aktivität des gewählten Katalysators bis runter zu 230°C, wobei ein vollständiger Umsatz ins thermodynamische Gleichgewicht möglich ist. Zeichen für eine Deaktivierung des Katalysators waren dabei nicht erkennbar. Durch die polytrope Betriebsweise des Reaktors bildet sich ein Temperaturpeak in der Eintrittszone des Reaktors aus. Es wird vermutet, dass dieser Temperaturpeak genügend Wärme für den Umsatz von höheren Kohlenwasserstoffe im Zuge der Methanisierung liefert. Labortests mit flaschengemischten Synthesegas unter Zugabe verschiedener Verunreinigungen wie Ethylen, Teere und Schwefelwasserstoff zeigen den Einfluss dieser Komponenten auf die Methanisierung. Die Ergebnisse bestätigen, dass höhere Kohlenwasserstoff direkt im Zuge der Methansynthese umgesetzt werden. Untersuchungen des Umsatzes zeigen, dass dies innerhalb der ersten Zentimeter des Reaktors geschieht. Hauptproblem dabei ist aber die Verkokung des Katalysators. Die Zugabe von mehr als 0.5 vol. % Ethylen führt zu starker Verkokung, wohingegen Teere in Konzentrationen von 6-12 g/Nm³ nur zu geringen Kohlenstoffablagerungen am Katalysator führten. Die Menge des abgelagerten Kohlestoffs hängt von den Reaktortemperaturen aber auch dem Wasseranteil des Synthesegases ab. Ein kombinierter Umsatz von Ethylen und Teeren zeigte, im Vergleich zum Umsatz von Ethylen alleine, geringere Verkokung. Diese Verkokung lässt sich weiter reduzieren, beziehungsweise vermeiden, durch die Zugabe von geringen Mengen (< 1 ppm) Schwefelwasserstoff. Im letzten Teil der Arbeit wurde die gesamte Prozesskette der SNG-Produktion, von der Vergasung, über die Gasreinigung, bis zur Methanisierung, im Labormaßstab erprobt. Die vereinfachte Gasreinigung entfernt effektiv Staub, Alkalien und Schwefelverbindungen wie H2S und COS, hat aber wahrscheinlich Schwächen bei der Abscheidung von organischen Schwefelverbindungen. Das zeigt sich auch in den noch recht hohen Deaktivierungsraten des Katalysators. Eine weitere Optimierung der Entschwefelung ist deshalb erforderlich. Vielversprechend ist der fast vollständige Umsatz von Teere auch in den Tests mit realem Synthesegas. VI Content Content 1. Introduction ......................................................................................................................... 1 1.1. Motivation ............................................................................................................................... 1 1.2. Objectives ................................................................................................................................ 3 2. State-of-the-Art .................................................................................................................... 5 2.1. Reactor concepts for methanation ......................................................................................... 6 2.2. Large SNG plants and projects in operation ............................................................................ 9 2.2.1. Large-scale coal-to-SNG plants .......................................................................................
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