inGAP - Det matematisk-naturvitenskapelige fakultet, UiO · inGAP 2007 Innovative Natural ... •...

2007inGAPInnovative Natural Gas Processes and Products P.O. box 1033 Blindern0317 OsloNorway

Phone: +47 22 85 54 46Fax: +47 22 85 54 41

[email protected]

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ANNUAL REPORT

An aerial view of the European Synchrotron Radiation facility in Grenoble.

Resume The inGAP centre of Innovative Natural Gas Processes and Products was officially launched on March 19, 2007. During the first year, focus has been set on establishing projects, building the organization and laying the basis for later achievements through construction of in-situ characterization installations, especially at the Swiss-Norwegian beamline at ESRF, Greno-ble, and through development of important techniques such as 3D-TEM and powder ALD.

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Centre vision Value creation in natural-gas processes through rational design of processes and products based on atomistic and mechanistic insight in catalyst and reactor parameters under operative conditions

Main challengesInnovation in natural gas based processes of particular interest to the industry partners, through a synergetic approach, i.e.:

• Establishing a well-functioning framework for scientific and technologi-cal cooperation between industry and academia

• Assuring transfer of knowledge between the different projects and institu-tions

• Attracting highly qualified scientists and students to work in the Centre

Centre goalsThe main Centre goal is to boost Norway’s position as a leading provider of environmentally-friendly processes based on natural gas.

Subgoals:

• To provide advanced methodology and fundamental insight into catalyst technology to industry partners, thereby promoting higher productivity in existing plants, a systematic approach to development of improved cata-lysts and processes and the basis for creating new natural gas processes and products

• Funding and research training of at least 18 PhD students and 10-12 temporary researchers

• At least 80 publications in high-ranked journals, and 80 oral and poster presentations at conferences

• Hosting an International School of Catalysis

• Personnel exchange (8 man-years) between industry and academia

• A number of patent applications

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Research plan/strategyOur strategy is to establish a cross-disciplinary centre that integrates experiments, theory and technology within the field of catalytic processes.

Industrial catalysts comprise several length scales and levels of complexity; active sites possibly being influenced by pro-moters (modifiers), possibly interacting with the support (or framework), all being incorporated into a formulated ma-trix. The very type of active site (acidic, metal, redox), pro-moters, supports (high surface, porous, crystalline, basic), binders is strongly process dependent. Therefore the pres-ent focus is on systems of particular relevance for natural gas processes; i.e., metal-support catalysts and microporous catalysts.

Each industry partner has defined a process of particular interest to them, and identified technical challenges in these processes, which are addressed in joint industry-institute-academia projects. In addition, several fundamental proj-ects have been defined to support the industry projects with topics such as; synthesis of model materials and methods development. Furthermore, investments are made in instru-ments and equipment of particular importance for the study of each of the processes.

A major goal of inGAP is to merge the various activities and partner expertise into a common pool of knowledge. Therefore, members of the management team have full in-sight into all projects, and the management team has a spe-cial responsibility of disseminating important achievements, especially on the methodology side, across the projects.

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Table of contents

Organisation ................................................... 6

Scientific activities/results .............................. 9Methods ....................................................... 10Natural Gas to Fuels .................................... 1�Natural Gas to Syngas ................................. 18Natural Gas to Petrochemicals ................... ��

International Collaboration .......................... ��

Recruitment ................................................... ��

Account ........................................................... �5

Publications .................................................... �7

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ORGANISATION Organisation structureThe inGAP centre is organised through a project based matrix. Each project has been allocated to an In-novation Area, with an Innovation Area Manager. The Innovation Areas are:

• NG (Natural Gas) to syngas

• NG to fuels

• NG to petrochemicals

• New chemistry

• Methods

The Innovation Area Managers are part of inGAP’s management team, together with the Managing Direc-tor and the Administrative Leader. The Innovation Area Managers report to the Managing Director. In order to reduce the number of persons involved in management tasks, all Innovation Area Managers are also project leaders of one project within the given innovation area.

Two types of projects have been defined:

1) Each industry partner has defined a Restricted Technology Area (RTA) project, for which they are given priority to intellectual property rights (IPR).

2) Non-RTA projects, which are of global interest to the Centre partners, mainly focusing on method de-velopment as well as preparation, characterisation and testing of model materials.

Steering BoardBoard Leader: Erling Rytter

Management teamManaging Director: Unni Olsbye

Administrative leader: Sigurd Brændeland

New chemistryLeader: Edd Blekkan

NG to fuelsLeader: Edvard Bergene

NG to syngasLeader: Bjørnar Arstad

NG to petrochemicalsLeader: Richard Blom

MethodsLeader: Poul Norby

InternationalAdvisory Board

Steering BoardBoard Leader: Erling Rytter

Management teamManaging Director: Unni Olsbye

Administrative leader: Sigurd Brændeland

New chemistryLeader: Edd Blekkan

NG to fuelsLeader: Edvard Bergene

NG to syngasLeader: Bjørnar Arstad

NG to petrochemicalsLeader: Richard Blom

MethodsLeader: Poul Norby

InternationalAdvisory Board

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From partners*: Representative Deputy

University of Oslo Helmer Fjellvåg Anders Elverhøi

NTNU Trondheim Anders Holmen Edd Blekkan

SINTEF Aage Stori Duncan Akporiaye

Statoil ASA Erling Rytter Morten Rønnekleiv

Hydro Polymers AS Steinar Kvisle Terje Fuglerud

Norsk Hydro ASA, Oil and Energy Linda Tangen Merethe Sjøvoll

Borealis Klaus-Joachim Jens Eberhard Dreher

The inGAP Steering Board had the following members in 2007:

*) Statoil and Norsk Hydro ASA have merged into “StatoilHydro ASA”, effective from 10/2007. Hydro Polymers has been acquired by Ineos and is “Ineos ChlorVinyls” since 02/2008.

An International Advisory Board (IAB) has been appointed from 01/2008, for a period of 2 years. Each Advisor covers a subject of utmost importance for the early stage of the inGAP Centre. The Advisory Board consists of the following persons (in alphabetical order):

• Prof. Ferdi Schüth, Max-Planck institute (Nanomaterials)

• Prof. Gabor Somorjai, Univ. California (Surface characterisation)

• Prof. Bert Weckhuysen, Univ. Utrecht (In situ characterisation)

The IAB will assist the Steering Board in evaluating activities and recommending long-term strategies and priorities.

inGAP’s Steering Board has members from each of the consortium partners and has the overall responsibility for all inGAP activities. For the 2 years period 2007-08, Erling Rytter is appointed as Chairman of the Steering Board.

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Partner Name Work months (150 hrs) in �007

Hydro Polymers Arne Grønvold 0.9Terje Fuglerud 0.9Steinar Kvisle 0.2Lola I. Sanna 0.2

Norsk Hydro ASA, Oil and Energy

Linda Tangen 0.3

Jens Bragdø Smith 0.1

Statoil ASA Erling Rytter 0.3Torild Skaseth 0.1Jorun Z. Albertsen 0.1Thomas Sperle 0.3

NTNU Anders Holmen 1Edd Blekkan 1De Chen 0.5Magnus Rønning 0.5Hilde Venvik 0.5

SINTEF Ivar M. Dahl 0.9Elisabeth Tangstad 1Arne Karlsson 0.6Øystein Strand 0.1Knut Torshaug 0.5Edvard Bergene 0.2Britt Sommer 0.1Pascal Dietzel 0.2Richard Blom 1.2Anne Andersen 0.5Jesper Bennetsen 1Aud Spjelkavik 0.3Bjørnar Arstad 3.5Duncan Akporiaye 0.3John Walmsley 0.3Knut A. Bøe 2Egil Bakken 0.7

UiO Unni Olsbye 9.3Sigurd Brændeland 8.6Sharmala Aravinthan 9.3Ole Swang 2Karl Petter Lillerud 2.5Poul Norby 2.5Helmer Fjellvåg 2.5

Senior personnel

The following senior personnel were active in the Centre in 2007:

Name Allocation Starting date

Madeleine Diskus University of Oslo 01.10.2007Mahsa Zokaie University of Oslo 08.11.2007

In addition to the senior personnel, two Ph.D. students were hired in inGAP in 2007:

Partners

inGAP is a consortium between the following partners:

Host institution:

• University of Oslo

Industry:

• Statoil ASA

• Hydro Polymers AS

• Norsk Hydro ASA, Oil and Energy

• Borealis

Non-industry:

• NTNU

• SINTEF

Collaboration between partnersA major goal of inGAP is to merge the various activities and partners expertise into a common pool of knowledge, in order to advance the fun-damental knowledge about selected processes and thematic areas.

Each innovation area and most projects involve scientists from several partners who are directly involved in the project work. In this way we as-sure integration between participants and transfer of competence between the different partners.

The Innovation Area Managers have full insight into the projects within their Innovation Area and assure transfer of competence both within the area and between projects which belong to different ar-eas, through regular meetings in the management team.

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SCIENTIFIC ACTIVITIES, RESULTS

2007 was the first year of functioning for inGAP. Some projects were already fully op-erational and in good progress by the end of 2007, while others were just starting. In this report, we have picked out a few examples of on-going projects, giving an impression of the type of activities in the Centre. Our strategy when starting up, was to give full priority to defining projects of special relevance to the industry partners, as well as methods building and equipment purchasing. This strategy is reflected in the reports below.

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In situ@SNBL

Aim of the project and scientific challengeThe aim of the project is to build a state of the art facility for synchrotron X-ray based in-situ studies of catalysts. As in situ studies will play a key role in many of the projects in inGAP, the construction of this facility was prioritized in the early stages of the inGAP collaboration.

The construction of the facility is now completed and op-erational. The first in situ experiments utilizing the system have been performed. The facility is truly state-of-the-art equipment for in situ studies of catalytic materials. To our knowledge, no similar system exists at a synchrotron facil-ity, and there is already significant international interest in utilizing the equipment.

One of the major challenges in studies of catalysts and cat-alytic materials is to characterize the materials under real working conditions. It is often impossible to obtain reliable structural information by extrapolation from ambient condi-tion. The only real solution is to study the materials at the temperature, pressure and chemical environment found in the catalytical reactor.

The facility was constructed at the European Synchrotron Radiation Facility in Grenoble, at the Swiss-Norwegian Beamlines. The good collaboration with the beam line personnel has been very important for the success. The beamlines are operated as a joint collaboration between Switzerland and Norway on a fifty-fifty basis, and include instrumentation for high resolution powder diffraction, X-ray absorption spectroscopy, single crystal diffraction and time resolved powder diffraction.

Synchrotron radiation is very intense electromag-netic radiation generated as a result of electrons (or positrons) being deflected by magnetic fields in a storage ring. The utiliza-tion of the high energy part of the spectrum, synchro-tron X-ray radiation, has had a great impact on in situ studies, due to the high intensity, the possibility of using high energy radiation and the high resolution ob-tainable.

Experimental techniquesFor in situ studies of catalytic materials of interest in the inGAP projects, mainly dif-fraction and X-ray absorption spectroscopy are of interest. Complimentary information about structural and chemical properties may be extracted from these experiments. The facility is aimed at providing a versatile system for in situ studies, where catalytic condi-tions of interest to the inGAP partners may be created. In ad-dition the system must be flex-ible enough to accommodate different experimental condi-tions and multi-technique ex-periments.

The experimental techniques of interest, alone or in combi-nation, are:

• High resolution powder diffraction

• X-ray absorption spectroscopy (e.g. XANES, EXAFS)

• Time resolved powder diffraction (MAR345 imaging plate system)

In addition the facility includes a mass spectrometer (MS), financed by inGAP, which is intended for online analysis of exhaust gases from the in situ experiments. This instrument will be used routinely for in situ experiments.

A Raman spectrometer is also available at SNBL, financed by the Norwegian and Swiss research councils. The Raman instrument is situated in the preparation lab with fiber optic cables to the experimental stations allowing it to be inte-grated into the in situ experiments. Raman spectroscopy is a valuable technique for in situ studies of catalytic materials, and we expect to use it extensively.

Combined experiments available include:

• Powder diffraction/Raman/MS

• XAS/Raman/MS

• High resolution powder diffraction/XAS/Raman/MSFigure 1. An aerial view of the European Synchrotron Radia-tion facility in Grenoble.

Figure 2. An example of time resolved powder diffraction data obtained during oxidation/reduc-tion.

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Status of the facilityThe requirements for the system were fairly challenging, as it must cover a wide range of temperatures, pressures and chemical environment. In addition, fast switching between gases should be possible for time resolved studies. The facility is intended to operate up to 20 atm. pressure and at temperatures up to 1000ºC. It must allow simultaneous monitoring of the reaction products using a mass spectrometer, and simultaneous collection of Raman data.

The gas system is now ready for experiments. The gas system was completed and installed during the autumn of 2007, and the mass spectrometer was installed in January 2008. The first in situ experiments utilizing the equipment were performed in December 2008.

The facility consists of a gas distribution system with 6 gas lines into the A and B station and to the preparation lab, Figure 3. A mobile gas mixing and switching system can be moved between experimental stations, Figure 4 and 5.

Figure 3. The gas distribution system outside the experi-mental hutches.

Figure 4. The mobile gas mixing and switching system.

Figure 5. The gas system installed in the experimen-tal hutch.

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Theoretical modeling

Scientific problemThe groups at SINTEF and UiO have a strong track record in exploiting the synergy between experimental and com-putational approaches, both regarding catalysis in zeotype materials [1-9] and on oxide-supported metals [10-11]. We have established that quantum chemical modeling is a valuable tool for elucidation of reaction mechanisms and for suggesting modifications to existing catalysts. Cataly-sis research groups worldwide now use quantum chemical methods to an ever-increasing extent. We have excellent experience integrating the modeling approach into chemical problem solving.

This subproject has two main foci:

• Acid-catalyzed reactions in zeotype materials.

• Reactions of relevance to natural gas conversion on oxide-supported metal catalysts.

For both classes of problems, the main challenge is to elu-cidate reaction mechanisms. When a reaction mechanism is known, proposed candidates for better catalysts may be computationally screened, allowing a better focus in subse-quent experimental testing.

ApproachMethods based on quantum mechanics are used to calculate the energy of a given system as a function of its atomistic structure. This enables us to calculate equilibrium structure, vibrational spectra, reaction energies (hence thermodynam-ics), and activation energies (hence kinetics). Generally, a reaction is reverse-engineered by calculating observable properties for a number of candidate structures and reaction paths. Comparison with experiment then affords determina-tion of structures and mechanisms.

There are two main approaches for the modeling of a solid surface: Cluster models, in which the solid is modelled by a cluster of atoms (technically a molecule) consisting of typi-cally between 10 and 50 atoms, and band structure or peri-odical models, where translational symmetry operators are used to generate an infinite solid in 1, 2 or 3 dimensions by operating on a unit cell. The centre disposes of technology to conduct both these kinds of calculations, and both will be employed, as they complement each other.

The workhorse of contemporary quantum chemistry is methods based on density functional theory (DFT). By now, their area of validity is well established. For our purposes, the most important shortcoming of DFT is its inability to model dispersion forces. While the errors arising from this may often be corrected to a good approximation by simple empirical corrections, we will also need to conduct calibra-tion studies using more accurate methods based on ab initio theory (MP2, CC).

Results The activity commenced in November, 2007. No publishable results have been achieved so far, but we are well underway with a study of olefin methylation by methanol or methyl chloride in the cavities of the zeotype materials Chabazite and SAPO-34.

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Figure 1. The charge distribution on the internal surface in a zeolite cavity.1�

References1. Arstad, B; Kolboe, S; Swang, O ”A Theoretical In-

vestigation on the Methylation of Methylbenzenes in Zeolites”, J. Phys. Chem. B 2002, 106, 12722.

2. Svelle, S.; Kolboe, S.; Olsbye, U.; Swang, O “A The-oretical Investigation of the Methylation of Methyl-benzenes and Alkenes by Halomethanes over Acidic Zeolites”, J. Phys. Chem. B 2003, 107, 5251.

3. Svelle, S; Arstad, B; Swang, O; Kolboe, S “A Theo-retical Investigation of the Methylation of Alkenes with Methanol over Acidic Zeolites”, J. Phys. Chem. B 2003, 107, 9281.

4. Arstad, B; Kolboe, S; Swang, O ”A Theoretical In-vestigation of the Alkylation of Benzene and Toluene by Ethene and Propene over Acidic Zeolites”, J. Phys. Chem. B 2004, 108, 2300.

5. Svelle. S.; Kolboe, S.; Swang, O. “Theoretical Investigation of the Dimerization of Linear Alkenes Catalyzed by Acidic Zeolites” J. Phys. Chem. B 2004, 108, 2953.

6. Arstad, B.; Kolboe, S.; Swang, O.: ”A Theoretical study of protonated Xylenes: Ethene elimination and H, C-Scrambling Reactions”, J. Phys. Org. Chem. 2004, 17, 1023.

7. Svelle, S.; Kolboe, S.; Swang, O.; Olsbye, U., “Meth-ylation of alkenes and methylbenzenes by dimethyl ether or methanol on acidic zeolites”, J. Phys. Chem. B 2005, 109, 12874.

8. Arstad, B.; Kolboe, S.; Swang, O.: ”Theoretical study of the Heptamethylbenzenium Ion: Intramolecular reactions and C2, C3, and C4 alkene elimination”, J. Phys. Chem. A 2005, 109, 8914.

9. Arstad, B.; Kolboe, S.; Swang, O. ” Theoretical study of carbon atom scrambling in benzenium ions with ethyl or isopropyl groups”, J. Phys. Org. Chem. 2006, 19, 81.

10. Jensen, M. B.; Pettersson, L. G. M.; Swang, O.; Ols-bye, U. ”CO2 Sorption on Different Sites on MgO and CaO Surfaces: A Comparative Quantum Chemical Cluster Study”, J. Phys. Chem. B 2005, 109, 16774.

11. Jensen, M. B.; Olsbye, U.; Swang, O. “Oxygen In-fluence on the Dissociative Chemisorption of Meth-ane on Nickel: A Quantum Chemical Cluster Model Study”, Chem. Phys. Lett. 2006, 432, 99.

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FT-Technology

Scientific problemStatoilHydro is currently commercializing the Gas To Liq-uid (GTL) technology [1], but there are still interesting and unresolved scientific challenges. The heart of a GTL plant is the Fischer-Tropsch (FT) reactor. Together with its part-ners StatoilHydro has chosen a slurry reactor which is a de-manding reactor type requiring a highly specialized catalyst. Through intense development work StatoilHydro’s current FT catalyst has excellent properties achieved by intelligent trial and error, but the fundamental understanding is weak in some respects. Since the catalyst has to work effectively for two years or more aging effects and how to avoid them is extremely important. In this project two aging effects are focused: declining catalytic activity over time (deactivation) and insufficient mechanical strength. Breakdown of the cat-alyst into fine material is detrimental to the process. These parameters seem trivial, but this is not the case at all. The main approach in the projects is to combine StatoilHydros unique experience in catalyst formulation and design with state of the art characterization techniques and material knowledge in the universities (UiO/NTNU) and SINTEF.

Initially these scientific challenges have been addressed by three different techniques, X-ray diffraction (XRD) of used catalyst, electron tomography (3D-Transmission Electron Microscopy (TEM)) and X-ray Photoelectron Spectroscopy (XPS).

Characterization of used catalyst systems by X-ray diffraction

Approach and resultsThere is an optimum particle size of the catalytically active species for the Fischer-Tropsch reaction. If particles of op-timal size sintered together during reaction, it would lead to a decrease in activity and concomitant change in crystal-lite size. X-ray diffraction on powder samples is a fast and powerful way to determine the crystallite size of nanoscale materials. The method was therefore chosen to investigate samples taken from a pilot plant Fischer-Tropsch reactor. It is possible to determine whether the crystallite size of the catalyst has changed during the production run by compar-ing these samples to the same catalyst before it was put to use in the reactor.

The investigation is complicated by the fact that the catalyst system is immersed in hydrocarbon wax. The wax is partial-ly crystalline and exhibit reflections which may overlap with the peaks attributable to the cobalt species of the catalyst. The same is the case for the catalyst support (Figure 1). A pattern fit of such a powder pattern will reveal the crystallite size of the catalytically active metal, which was done for the used material (Figure 2).

The lines contributed by the wax can be avoided if the mea-surement is performed at elevated temperatures at which the wax melts, thus the crystalline regions present in the solid wax. However, a more severe problem posed the discovery that the concentration of catalyst in respect to wax was too low in some samples which lead to powder patterns which could not be analyzed. The amount of the material of inter-est therefore needs to be increased in the samples. This can be done by heating the sample and physically removing the majority of the liquid wax, or chemically by removing it with a suitable organic solvent. The latter is expected to be able to remove the wax completely which will be a pre-requisite for investigation of these materials with a range of advanced methods of characterization in the future. Both methods can be performed in inert atmosphere to minimize the danger of chemically altering the material, and attempts to prepare samples amenable to the diffraction experiment in this way are currently in progress.

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Electron tomography/�D TEM

Approach and resultsIt is a challenge to visualize the nanoscale structure of cat-alyst systems directly. The Transmission Electron Micro-scope (TEM) is a powerful tool for studying materials on this scale. However, the complicated structure of heteroge-neous catalysts means that the true structure is not revealed in the two dimensional projections provided by typical TEM images. A series of images of the same area acquired over a tilt range of ~70 degrees can be aligned and reconstructed to give a data set that captures the three dimensional struc-ture of the sample. This is called electron tomography. The process is complicated technically and this activity has been to establish electron tomography inGAP project by using the field emission gun TEM at Trondheim. Investment is being made in the software necessary to perform the data-set reconstruction and modification of sample holders to allow images to be acquired at large tilt angles.

Experience in electron tomography has been gained by cooperation with the Group at Cambridge University that have pioneered the application of this technique in the physical sciences [2], work funded directly by StatoilHydro. The cooperation has been extended within a KMB project “Advanced transmission electron microscopy in catalysis” under the ESTEEM 6th Framework Programme of the Eu-ropean Commission.

An “off the shelf” solution for electron tomography of cata-lyst systems is not available.

The example shows three of the stages in performing three dimensional analysis of test Fischer Tropsch system show-ing the distribution of undreduced catalyst (cobalt oxide) on a titanium oxide substrate. The individual oxide substrate particles have a size in the range of tens of nanometers.

Figure 1. Powder X-ray diffraction pattern of used FT cata-lyst. Clearly visible are contribution of the wax (orange) and the catalyst support (grey), which overlap partly with the reflections attributable to the metal (green).

Figure 2. Profile fit of the overlapping metal and support reflection which allows the determination of the crystal-lite size.

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X-ray Photoelectron Spectroscopy (XPS)

XPS will be a powerful technique analysing both new and possibly used catalysts. Since the instrument is relatively new few results have been obtained so far.

Preparation and studies of model compoundsA PhD position at UiO has been filled by October 2007 (project leader prof. Fjellvåg). The candidate, Madeleine Diskus, has now started her experimental activity. The PhD position, funded via UiO self-contributions, has focus on utilizing the ALD (Atomic Layer Deposition) technique to deposit sub-monolayer to nm-thick monolayers of one or more oxides on a porous support (from relevant support ma-terials for real catalysts to nm/µm-porous model supports). The main target is to deposit Co and Co-M mixed oxides on such porous supports. These will indeed be interesting model materials for the FT-reaction.

Figure 3 STEM image with sample tilted by an angle of ap-proximately 70 degrees.

Figure 4 Slice through raw reconstruction of tilt series of 71 images.

Figure 5 Voxel* representation of reconstructed three dimensional data set. A voxel is a 3D pixel (see http://en.wikipedia.org/wiki/Voxel)

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Sentre for forskningsdrevet innovasjon (SFI) Norges forskningsråd

Figure 3 STEM image with sample tilted by an angle of approximately 70 degrees.

Figure 4 Slice through raw reconstruction of tilt series of 71 images.


Figure 3 STEM image with sample tilted by an angle of approximately 70 degrees.

Figure 4 Slice through raw reconstruction of tilt series of 71 images. Sentre for forskningsdrevet innovasjon (SFI) Norges forskningsråd

Figure 5 Voxel* representation of reconstructed three dimensional data set.

A voxel is a 3D pixel (see http://en.wikipedia.org/wiki/Voxel)

X-ray Photoelectron Spectroscopy (XPS) XPS will be a powerful technique analysing both new and possibly used catalysts. Since the instrument is relatively new few results have been obtained so far.

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The figures above shows XPS spectra from FT-catalysts similar to those who will be obtained in InGAP. We expect that different treatments in the in-situ high pressure gas cell will give new insights in the surface chemistry of FT catalysts.

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Before coming to the challenges of making controlled depo-sitions of model materials, it is required that the candidate gains hands-on experience with the ALD method, with a primary goal to prove ability to control process conditions for a new cation system. This work is in good progress. The system chosen is Mo-oxides, a system not earlier being de-posited by means of ALD. We expect that this work will lead to one publication during 2008, with potential for a second on a ternary Mo-M-O at the end of 2008. This work is novel and important; both because Mo has interesting applica-tions as a catalyst, but also because certain Mo-M-oxides have exciting physical properties which can be explored in future studies in our group.

So far the possibility of utilizing MoCl5 as precursor in com-bination with H2O og O3 is explored. MoCl5 is chosen owing to price and availbility. Interestingly, this precursor does not provide the desired oxide product at the so far investigated process parameters. Hence, the work provided us with im-portant analyses of mechanisms that may hinder a desired oxide growth. The focus has now been shifted to Mo(CO)6 as potential Mo-precursor. Mo-oxide growth is achieved at rather mild conditions. Studies of growth parameters are ongoing.

References1. Buller, A.T., Schanke, D., Rytter, E., Hansen, R,

Statoil Research & Technology Memoir no 8, Gas-To-Liquid Technology, 2006.

2. Arslan I, Walmsley JC, Rytter E, Bergene E, Midgley, P, Toward Three-Dimensional Nano-Engineering of Heterogeneous Catalysts, accepted for publication in the Journal of the American Chemical Society.

Figure 6. The fi gures above shows XPS spectra from FT-catalysts similar to those who will be obtained in InGAP. We expect that different treatments in the in-situ high pressure gas cell will give new insights in the surface chemistry of FT catalysts.

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Vinyl Chloride Monomer (VCM)

Ineos ChlorVinyls (previously Hydro Polymers) operate a number of plants where VCM is produced from ethene and chlorine. VCM is polymerized to PVC. VCM technology is a mature technology but there is still room for process im-provements, e.g., increased product yields, reduced by-prod-uct formation, catalyst stability, etc. Elements of this are ad-dressed in this project.

Scientific ProblemThe catalytic cycle of the oxychlorination process is shown in Scheme 1. As indicated in the Scheme, three distinct reactions steps take place: First the doubly chlori-nation of ethylene while cupper(II)chloride is reduced to cupper(I)chloride, then the re-oxidation of Cu(I) to Cu(II) by oxygen, and finally the hydrochlorolysis of the oxychlo-ride back to the original dicloride by hydrochloric acid to complete the catalytic cycle.

Although the kinetics of the total oxychlorination reaction is known, the knowledge of the mechanisms and kinetics of each individual reaction step is still largely unknown. The overall objective of the VCM project is therefore to fill in the unknown mechanistic and kinetic gaps in the oxychlorina-tion cycle and construct a microkinetic model of the process based on these findings. Such a model will provide valuable insight on how to run the oxychlorination process in an op-timal way. Even small improvements in the selectivity and yield will have large economical benefits.

ApproachA preliminary microkinetic model will be constructed based on the literature values available. From this study, also the missing knowledge will be identified. To fill in the unknown gaps, experimental ways to fill these gaps will be sought within the inGAP consortium. Of possible methods that can give further insight on the surface mechanisms involved are in situ techniques such as DRIFTS, while kinetic constants for the individual reactions can be obtained from either pulse reactions or reactions using isotope labeled gases (SSITKA) using a fixed bed reactor. Further support for choices on the intricate mechanisms of surface reactions can be obtained from molecular modeling (ab initio calculations). Our aim is to obtain a complete picture of the total process within the inGAP period.

ResultsUntil now work has been done to update the project team on the state-of-art on the oxychlorination process. A PhD student will be employed during the summer of 2008.

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Natural Gas to Petrochemicals

Vinyl Chloride Monomer (VCM)

Ineos ChlorVinyls (previously Hydro Polymers) operate a number of plants where VCM is produced from ethene and chlorine. VCM is polymerized to PVC. VCM technology is a mature technology but there is still room for process improvements, e.g., increased product yields, reduced by-product formation, catalyst stability, etc. Elements of this are addressed in this project.

Scientific Problem The catalytic cycle of the oxychlorination

process is shown in Scheme 1. As indicated in the Scheme, three distinct reactions steps take place: Fist the doubly chlorination of ethylene while cupper(II)chloride is reduced to cupper(I)chloride, then the re-oxidation of Cu(I) to Cu(II) by oxygen, and finally the hydrochlorolysis of the oxychloride back to the original dicloride by hydrochloric acid to complete the catalytic cycle.

Although the kinetics of the total oxychlorination reaction is known, the knowledge of the mechanisms and kinetics of each individual reaction step is still largely unknown. The overall objective of the VCM project is therefore to fill inn the unknown mechanistic and kinetic gaps in the oxychlorination cycle and construct a microkinetic model of the process based on these findings. Such a model will provide valuable insight on how to run the oxychlorination process in an optimal way. Even small improvements in the selectivity and yield will have large economical benefits.

ApproachA preliminary microkinetic model will be constructed based on the literature values

available. From this study, also the missing knowledge will be identified. To fill in the unknown gaps, experimental ways to fill these gaps will be sought within the inGAP consortium. Of possible methods that can give further insight on the surface mechanisms involved are in situ techniques such as DRIFTS, while kinetic constants for the individual reactions can be obtained from either pulse reactions or reactions using isotope labeled gases (SSITKA) using a fixed bed reactor. Further support for choices on the intricate mechanisms of surface reactions can be obtained from molecular modeling (ab initio calculations). Our aim is to obtain a complete picture of the total process within the inGAP period.

Results Until now work has been done to update the project team on the state-of.-art on the

oxychlorination process. A PhD student will be employed during the summer of 2008.

2 HClH2O

C2H4

C2H2Cl2 0.5 O2

2 CuCl

2 CuCl2 Cu2OCl2

Hydrochlorolysis

Cu(I) oxidationCu(II)

redu

ction

2 HClH2O

C2H4

C2H2Cl2 0.5 O2

2 CuCl

2 CuCl2 Cu2OCl2

Hydrochlorolysis

Cu(I) oxidationCu(II)

redu

ction

Scheme 1

18

Model compounds – microporous

Scientific ProblemTo obtain our vision: Rational design of new and improved catalysts based on fundamental mechanistic insight, do we need to obtain both new fundamental insight about the structure-reaction-mechanism relationship and we need to be able to synthesize the next generation catalyst that we hopefully will be able to suggest on the basis of the mecha-nistic studies. This project focus on the synthesis of SAPO-34 type materials (CHA-topology with Aluminum phos-phate lattice and with a variable degree of Si substation) There is a parallel project studying SSZ-13 type materials (CHA-topology with a silicate lattice and with a variable degree of Al substation).

The challenge is to synthesize the material with a controlled continuous T-atom substitution and at the same time con-trol the local environment around the hetero-atom [1-5].

Approach It has been claimed in the literature that both the structure directing cations used and the degree of T-atom substitu-tion affect the substitution mechanism and the stability of the final material. Synthesis of SAPO-34 type materi-als with controlled T-atom substitution is a very active re-search field at the moment,

Figure 1. T-atom substitution in AlPO-34. Left figure illustrates substitution of one P-atom with one Si-atom. This will create a charge defect and an acidic proton next to this defect. The right figure illustrates a T-atom substitution of an Al ,P-pair with two Si atoms. This will preserve the charge neutrality.

Figure 2. Location of the structure directing template ion inside the cage in the SAPO-34 structure.

NATURAL GAS TO PETROCHEMICALS

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Scientific Problem

To obtain our vision: Rational design of new and improved catalysts based on fundamental mechanistic insight, do we need to obtain both new fundamental insight about the structure reaction mechanism relationship and we need to be able to synthesize the next generation catalyst that we hopefully will be able to suggest on the basis of the mechanistic studies. This (part of the) project focus on the synthesis of SAPO-34 type materials (CHA-topology with Aluminum phosphate lattice and with a variable degree of Si substation) There is a parallel project studying SSZ-13 type materials (CHA-topology with a silicate lattice and with a variable degree of Al substation). The challenge is to synthesize the material with a controlled continuous T-atom substitution and at the same time control the local environment around the hetero-atom.


- Approach

It has been claimed in the literature that both the structure directing cations used and the degree of T-atom substitution affect the substitution mechanism and the stability of the final material. Synthesis of SAPO-34 type materials with controlled T-atom substitution is a very active research field at the moment, material stability and properties seam to be highly dependent on the structure directing template used in the synthesis. A systematic study of the combined effect of changing template and lattice composition will be pursued.





Scientific Problem



- Approach






Scientific Problem



- Approach



19

material stability and properties seem to be highly depen-dent on the structure directing template used in the synthe-sis. A systematic study of the combined effect of changing template and lattice composition will be pursued.

There is an additional scientific challenge related to the characterization of the local environment around the het-ero-atom. A considerable part of the project will therefore be devoted to characterization and to develop techniques. This part of the project is done in close collaboration with groups specialized in individual techniques. (NMR: Francis Taulelle, University of Versailles. IR: Adriano Zecchina, Tu-rin University)

It is also planned to extend the synthesis work into a study of the mechanism of the formation of the material itself. Pio-neering work done in collaboration with Francis Taulelle [2-3] will form a basis for this part of the project. A new technique for crystallization studies; In-situ AFM will also be tried. Cooperation with Mike Anderson, University of Manchester has just been initiated.

ResultsActivating the catalyst by removing the template and ion-ex-change in case inorganic ions are present, may also change the local environment and thereby the catalytic properties for this type of fragile materials (Figure 3).

Figure 3. 29Si-NMR of SAPO-34. Bottom as-synthesized material, all Si is coordinated to Al. Top calcined material. Defects have been introduced, most Si is only three coordinated.

NATURAL GAS TO PETROCHEMICALSN

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ALS


There is an additional scientific challenge related to the characterization of the local environment around the hetero-atom. A considerable part of the project will therefore be devoted to characterization and to develop techniques. This part of the project is done in close collaboration with groups specialized in individual techniques. (NMR: Francis Taulelle, University of Versailles. IR: Adriano Zecchina, Turin University)

It is also planned to extend the synthesis work into a study of the mechanism of the formation of the material itself. Pioneering work done in collaboration with Francis Taulelle [refs. 10-12] will form a basis for this part of the project. A new technique for crystallization studies; In-situ AFM will also be tried. Cooperation with Mike Anderson, University of Manchester has just been initiated.

- Results

Activating the catalyst by removing the template and ion-exchange in case inorganic ions are present, may also change the local environment and thereby the catalytic properties for this type of fragile materials.

Figure 3. 29Si-NMR of SAPO-34. Bottom as-synthesized material, al Si is coordinated to Al. Top calcined material. Defects has been introduced, most Si are only three coordinated.

�0

References1. Vistad, OB; Akporiaye, DE; Lillerud, KP “ Iden-

tification of a key precursor phase for synthesis of SAPO-34 and kinetics of formation investigated by in situ X-ray diffraction”, J Phys. Chem. B 2001 105 (50): 12437-

2 . Vistad, OB; Akporiaye, DE; Taulelle, F; Lillerud, KP, ”In Situ NMR of SAPO-34 Crystallization”, Chem. Mater. 2003, 15, 1639-1649

3 . Vistad, OB; Akporiaye, DE; Taulelle, F; Lillerud, KP. ”Morpholine, an in Situ 13C NMR pH Meter for Hydrothermal crystallogenesis of SAPO-34“, Chem. Mater. 2003, 15, 1650-1654

4 . Bordiga, S; Regli, L; Lamberti, C; Zecchina, A; Bjorgen, M; Lillerud, KP. “FTIR Adsorption Studies of H2O and CH3OH in the Isostructural H-SSZ-13 and H-SAPO-34: Formation of H-Bonded Adducts and Protonated Clusters”. J. Phys. Chem. B 2005, 109(16), 7724-7732.

5. Bordiga, S; Regli, L; Cocina, D; Lamberti, C; Bjor-gen, M; Lillerud, KP. ”Assessing the Acidity of High Silica Chabazite H-SSZ-13 by FTIR Using CO as Molecular Probe: Comparison with H-SAPO-34” J. Phys. Chem. B 2005, 109(7), 2779-2784.

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Figure 4. AFM pictures of a CHA crystal. Upper right is the calculated crystal shape with the identification of the visible surfaces. Lower right is a magnification of the 111 surface. Growth terraces with the height of 4Å are clearly visible.

�1

Sorbent enhanced steam methane reforming

Scientific problemHydrogen is considered to be a potential energy carrier in the future. However, unless hydrogen can be produced without emission of CO2, or generation of other harmful substances, the positive environmental effects are reduced. Today, large scale production of hydrogen is mainly based on processing of fossil fuel, with concomitant production

of CO2, and it will likely be so for quite many years due to large reserves of especially gas and coal. One potential en-ergy efficient process for hydrogen production with simulta-neous CO2 separation is sorption enhanced steam methane reforming (SE-SMR). SE-SMR combines catalytic produc-tion of hydrogen and CO2 from methane and steam together with an internal CO2 sorption step. This enables a continu-ous production of hydrogen together with separation of CO2 in one process step/unit. Expensive CO2 capture units can thus be omitted. The separated CO2 should subsequently be sequestrated. So far only separate parts of the SE-SMR pro-cess have been tested. Our project is aimed to demonstrate and develop a continuous hydrogen production by sorbent enhanced steam methane reforming in a lab-scale circulat-ing fluidized bed (CFB) reactor. Figure 1 shows the prin-ciple of the process and the lab reactor:

Equations 1-4 below show the main chemical reactions tak-ing place in the reformer.

CH4(g) + H2O(g) = CO(g) + 3H2(g) Reforming (1)

CO(g) + H2O(g) = CO2(g) + H2(g) Water-gas shift (2)

MO(s) + CO2(g) = MCO3(s) Sorption, MO=metal oxide (3)

CH4(g) + 2H2O(g) + MO(s) = MCO3(s) + 4H2(g) Overall (4)

Figure 1. Left: Principle of sorbent enhanced stem methane reforming. The powder in the reactor system comprises both the catalyst and the sorbent. This mixture is continuously transported between the two reactor units; one for reforming and one for regeneration of the sorbent. Right: The lab reac-tor. R2 is the reformer and R1 is the regenerator.

NATURAL GAS TO SYNGASN

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RAL G

AS TO

SYN

GAS

Used powderReg. powder

Hydrogen rich stream

Steam + CH4

850 oC 600 oC

Steam

Regeneration Methanereforming

CO2 rich stream

��

The reverse of equation 3 is taking place in the regenera-tor thus making the sorbent ready for CO2 generated in the reformer unit.

Various aspects of reactor design, influence of process pa-rameters on performance, and material development (both catalysts and sorbents) will be explored in further work.

ApproachA CFB reactor rig has been built during 2007. It comprises two connected bubbling bed reactors, connected by a riser.

ResultsA patent application on the reactor design was filed early January 2008. Initial performance tests, including full reac-tions at high temperatures, have been carried out. The reac-tor system works well as two main challenges are solved, namely continuous powder circulation and prevention of gas mixing between the reformer and regenerator units. Kinetic modeling of the reactor system is also in progress (including kinetic measurements of CO2 uptake and libera-tion from the sorbent (calcined natural dolomite) chosen for initial studies).

ReferencesThe status of the project was presented at two conferences fall 2007.

1. B. Arstad, R. Blom, E. Bakken, I.M. Dahl, J.P. Jakobsen, P. Røkke “Development of a circulating fluidized bed reactor system for sorption-enhanced methane steam reforming” Oral presentation 4th CCS Conference, Trondheim, Norway

2. B. Arstad, R. Blom, E. Bakken, I.M. Dahl, J.P. Jako-bsen, P. Røkke, J. Bennetsen, K.A. Bø “Sorbent enhanced steam methane reforming. Con-cepts and reactors” Oral presentation NKS Katalysesymposium, Oslo, Norway

NATURAL GAS TO SYNGAS

NAT

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TO S

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International collaboration

The Centre has on-going collaboration with the University of Turin (Italy), the University of Versailles (France), the Swiss-Norwegian Beamlines (SNBL) at the European Syn-chrothron Radiation Facility (ESRF) in Grenoble (France), the University of Cambridge (UK), the University of Utrecht (The Netherlands) and the Humboldt University in Berlin (Germany).

Recruitment

Recruitment has been a major challenge in 2007; by the end of the year, only 2 out of 9 vacant Ph.D. and postdoc. posi-tions had been filled. The female share of Ph.D. positions was 100%.

Prospects for 2008 look much better; by March 10, 2007, all vacant Ph.D. positions have been filled, while 3 postdoc positions are still vacant.

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Publications

The academic senior personnel in inGAP have contributed to 66 publications in 2007, all of them originating from proj-ects outside the inGAP portfolio, but still mainly relevant to inGAP’s activities.

Two M.Sc. theses have been completed in the Centre during 2007:

Bart P.C. Hereijgers “On the deactivation mecha-nism in HSAPO-34 catalyst in Methanol to Olefins Conversion” (30 study points), University of Oslo, 07/2007.

Francesca Bleken “The effect of acid strength on the MTOreaction - Conversion of methanol to hydro-carbons over H-SAPO-34 and high silica Chabazite (H-SSZ-13)” (60 study points), University of Oslo, 12/2007.

Seven presentations directly related to Centre activities have been given by inGAP personnel in 2007:

1. A. Holmen “Recent developments in direct routes for natural gas conversion” Keynote lecture EuropaCat-VIII, Åbo, Finland

2. U. Olsbye “Natural Gas Conversion - Mechanistic studies as a tool for rational catalyst design” Invited lecture UOP lecture Series, Chicago, USA

3. K.P. Lillerud “New microporous Pt-metal-organic frameworks” Invited lecture Berzelli Centre Excelent Symposium, Stockholm, Sweden

4. U. Olsbye ”Utvikling av nye prosesser for foredling av naturgass – hvordan samarbeid mellom industri og akademiske miljøer kan bidra til teknologigjennom-brudd” Invited lecture GassArena, Haugesund, Norway

5. B. Arstad, R. Blom, E. Bakken, I.M. Dahl, J.P. Jakob-sen, P. Røkke “Development of a circulating fluidized bed reactor system for sorption-enhanced methane steam reforming” Oral presentation 4th CCS Conference, Trondheim, Norway

6. F.Bleken, S.Svelle, M.Bjørgen, K.P.Lillerud, U.Olsbye “Conversion of methanol to hydrocarbons over H-SAPO-34 and high silica cha-basite” Oral presentation NKS Katalysesymposium, Oslo, Norway

7. B. Arstad, R. Blom, E. Bakken, I.M. Dahl, J.P. Jakob-sen, P. Røkke, J. Bennetsen, K.A. Bø “Sorbent enhanced steam methane reforming. Con-cepts and reactors” Oral presentation NKS Katalysesymposium, Oslo, Norway

�7

2007inGAPInnovative Natural Gas Processes and Products P.O. box 1033 Blindern0317 OsloNorway

Phone: +47 22 85 54 46Fax: +47 22 85 54 41

[email protected]

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