Synthesis and Characterization of high-performance ceramic materials for hightemperature

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1 Synthesis and Characterization of high-performance ceramic materials for hightemperature CO 2 capture and hydrogen production. Location: Institute for Energy Technology (IFE), Kjeller, Norway Department of Environmental Technology Supervision: Johann Mastin (Project leader) / Asunción Aranda (Post. Doc) Introduction / State-of-the art The ZEG process as an especially promising method for producing hydrogen and electricity from natural gas with CO 2 capture (CCS) in an efficient and cost-effective way. The process combines the sorption-enhanced steam methane reforming (SE-SMR) process with high temperature solid oxide fuel cells (SOFC) for co-production of hydrogen and electricity with CO2 capture. The principle of the SE-SMR process is illustrated in Figure 1. Thus, apart from the use of a catalyst to increase the methane conversion, one of the possibilities to enlarge the hydrogen production is the capture of CO 2 while generated, which shifts the equilibrium towards products and has the additional advantage of avoiding CO 2 emissions. At this stage, a CO 2 absorbent is required, and high efforts are being done to improve calcium-oxide-based solids, since they are considered to be the most promising candidates for the SE-SMR process. The CO 2 absorption process is based on the reversible carbonation reaction of CaO at high temperature. Through this reaction, higher methane conversion at lower temperatures can be reached, which enlarges the catalysts lifetime and improves the global thermal balance of the process. The optimal operation window for the carbonation reaction is o C whilst the reverse endothermic reaction is favoured at high temperature and temperature above 850 o C is required to regenerate the sorbent at atmospheric pressure and produce an almost pure CO 2 stream.

2 Figure 1: Principle of the Sorption-Enhanced Steam Methane Reforming (SE-SMR) process based on the reversible carbonation reaction of a CaO solid sorbent. Natural CaO-based sorbents such as limestone (CaCO 3 ) or dolomite (CaMg(CO 3 ) 2 ) are usually preferred since they are largely available at relatively low cost and have a high total absorption capacity. However, long-term chemical and mechanical stability of natural sorbents are fairly poor. Natural sorbents suffer a rapid decrease of absorption capacity with increasing number of carbonation/regeneration cycles mainly due to sintering and pore closure effects. One of the key factors for the development of the SE-SMR technology is the obtaining of new synthetic CO 2 -absorbent materials with the following properties: - High total CO 2 absorption capacity, - Fast reaction at typical SE-reforming temperatures, - Long term mechanical and chemical stability - Low production cost. Institute for Energy Technology (IFE) has carried out an extensive work on developing novel ceramic sorbents for high-temperature CO 2 capture applications. The developed sorbent shows a genuine composite structure made of stable nano-particles of CaO (~100nm) homogeneously distributed in a microporous calcium aluminate matrix (fig.2). The controlled size of the nano-particles and the layered structure of the particles on the surface of the pores of the matrix are believed to significantly improve the chemical stability of the sorbent. As illustrated in Figure 2, preliminary results have shown an increased life-time (>200 cycles) in severe calcination conditions (pco 2 =0.85atm and T=925 o C) with an improved absorption capacity compared to natural dolomite. It is strongly believed that the CO 2 -sorbent, developed at IFE, meets the necessary quality improvements for hightemperature CO 2 capture: good CO 2 -absorption capacity, high chemical stability and excellent long-term durability (patent pending).

3 Figure 2: Evolution of the absorption capacity of the synthetic sorbent during multi-cycling compared to natural sorbent during (Left). Microstructure of the synthetic sorbent observed by Scanning Electron Microscopy (Right) A steam reforming catalyst is required to convert methane into CO and H 2. Nickel-based catalysts are often used because they are active and inexpensive. However, commercial Nicatalysts are designed primarily for use in fixed bed reactors and in-house testing suggests that they greatly suffer from reduced activity during regeneration at high-temperature. This loss of activity is a major problem as it will constitute an important cost of operation. To overcome the problem of handling a mixture of two solids with different chemical and physical properties and resolve the problem related to attrition of the reforming catalyst, the integration of catalyst material within the structure of a synthetic sorbent with a high resistance to attrition would constitute a major breakthrough for the industrial development of the SE-SMR process. Development of stable all-in-one particles (catalyst+sorbent+support) would facilitate the fluidization properties of the solids, decrease the overall production cost of the synthetic sorbent and significantly improve the overall economy of SE-SMR process system. Indeed, development of the all-in-one particle will reduce both reactor size and heat loss from the process, giving reduced investment cost and higher overall efficiency Another critical factor for future large-scale industrial applications is to develop an efficient agglomeration process by which the synthetic micro-powder (<50 µm) is further assembled into particles of suitable size ( µm) with the desired mechanical and chemical properties. It is believed that there is a potential for improving particle hardness/durability without compromising chemical activity and porosity, by optimizing agglomeration conditions and procedures. Thus, development of sorbent agglomerates with a high resistance to attrition and high chemical stability will improve the overall energy efficiency of the high-

4 temperature CO 2 -capture system by reducing the loss of fines by attrition and the total amount of solid in the inventory of the reactor. Project Proposal 1: Development of mechanically stable solid sorbent agglomerates for high-temperature CO 2 capture. The aim of the project is to develop a novel agglomeration technique to produce spherical ceramic beads of mixed CaO/calcium aluminate ceramic for high-temperature CO 2 capture application. Several agglomeration techniques will be tested and evaluated to determine the most suitable technique for preparation of medium size agglomerate batches. The influence of process parameters on the final microstructure of the sorbent (density, porosity) and the capture properties (reaction kinetic, absorption capacity, chemical durability) will be evaluated. The mechanical properties of the produced agglomerates/granules will be fully characterized by crushing strength and attrition measurements. Mechanical and chemical properties of the developed agglomerates will be compared to the properties of the natural sorbents and to literature data available for other sorbents. Project Proposal 2: Development of new hybrid ceramic material: catalyst/sorbent for hydrogen production and high-temperature CO2 capture. Preliminary studies have shown it is possible to integrate catalytically active nano-particles of Nickel or Rhodium within the microstructure of the sorbent particles to create an all-inone particle: hybrid CO 2 -sorbent particle with an active layer of Ni-particles. This project will focus mainly on the development of stable all-in-one particles with special emphasis on the long-term chemical properties of the sorbent particles and the long-term activity of the catalytic particles. The work will include the synthesis method optimization (impregnation/doping methods evaluation, catalyst loading, etc.) and the chemical and mechanical properties evaluation of the obtained materials. The development of such novel hybrid material would be a key step towards the commercialization of a sorption-enhanced reforming process. Available Facilities: Available experimental apparatus at IFE for those two projects are: Thermogravimetric analysis (TGA) for the performance of studies on the CO 2 sorbents, a laser scattering particle size distribution instrument, scanning electron microscope (SEM), X-ray diffraction (XRD), fluid bed agglomerator/coater, an instrument for measuring particle hardness and a benchscale fixed bed reactor, coupled with a micro-gc, for testing high-temperature reactions.

5 For more details and information take contact with: Johann Mastin (project leader) Trond Eivind Bøe (Department Head)

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