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EXPERIMENTAL STUDY OF THE VAPOUR-LIQUID EQUILIBRIA OF HI-I 2-H 2O TERNARY MIXTURES Introduction The search for new energetic vectors is of utmost importance due to the shortage of hydrocarbons and the high price reached by the oil barrel. Hydrogen appears to be a potential candidate if it can be massively produced at low cost. Among the various ways to achieve this goal, high-temperature electrolysis and thermochemical cycles, both using nuclear heat, are interesting solutions. Many studies have been devoted to thermochemical cycles since 1970 (Funk, 1976; Bamberger, 1978) and the most attractive one appears to be the iodine-sulphur one. Within the scope of studies on the massive production of hydrogen using this cycle (Norman, 1982; Vitart, 2008), the French atomic authority CEA has selected the more promising reactive distillation process (Roth, 1989; Belaissaoui, 2008) versus extractive distillation (O’Keefe, 1982) or electrodialysis (Miyamoto, 2000), in order to extract the hydrogen from the HIx phase produced by the Bunsen reaction. The scaling of this column, in which the distillation of the HIx phase and the decomposition of HI into hydrogen occur simultaneously, requires the knowledge of the vapour-liquid equilibrium, i.e. the partial pressures of the gas species HI, I 2 , H 2 O in thermodynamic equilibrium with the liquid phases of the corresponding HI-I 2 -H 2 O ternary mixtures (Engels, 1986; Doizi, 2007; Hodotsuka, 2008; Liberatore, 2008). In the liquid phase, the concentrations of the species vary in the intervals: 0.04 < [I 2 ] < 0.85 and 0.03 < [HI] < 0.2 for temperature between 20°C and 320°C and total pressures up to 50 bar. Considering the severe experimental conditions, involving concentrated and corrosive media, our study was divided into two parts corresponding to two experimental devices. The first one, the low-pressure device, enables the study of vapour-liquid equilibria in a temperature range between 20°C and 140°C and for total pressures up to 2 bar. The second one, the high-pressure device enables the study of vapour-liquid equilibria in the process domain. Based on the needs expressed, on the existing data and on the constraints imposed by the availability of hydriodic acid, an experimental campaign was carried around different groups of ternary compositions. These groups, characterised by their variable iodine and hydriodic acid contents, are represented in the ternary diagram of Figure 1. This article describes the experimental devices and provides the experimentally determined values of the total pressures and vapour phase concentrations. Figure 1 UV-vis pathlength 0.5 cm FTIR pathlength 25 cm Manometer 0-2 bar Thermocouple well Reservoir Initial choice of optical spectrometries To measure the gas phase speciation, the choice of optical spectrometries was made. These “online” techniques allow concentration measurements (Hartmann, 2009) and then partial pressures measurements without altering the gas phase composition. 192 NUCLEAR PRODUCTION OF HYDROGEN – © OECD/NEA 2010
EXPERIMENTAL STUDY OF THE VAPOUR-LIQUID EQUILIBRIA OF HI-I 2-H 2O TERNARY MIXTURES • Fourier Transform Infrared Spectrometry is used to measure H 2 O and HI concentrations. • UV visible spectrometry is used to measure I 2 concentration. The choice of these spectrometries has been validated on cells containing pure samples (H 2 O, HI, I 2 ) and HI-H 2 O binary mixtures. They have been then implemented on the two experimental devices. On the low-pressure device, the infrared measurements are performed using a Bruker Vector 22 FTIR spectrometer with a spectral resolution of 0.4 cm –1 . The major interest in this unit is the possibility to shift the infrared beam toward the outside of the apparatus and thus enable an “online” measurement. The IR configuration includes a Globar source, the Vector 22 interferometer with a KBr beam splitter and a nitrogen-cooled InSb detector. The entire optical path is under an inert nitrogen atmosphere for both the part outside the spectrometer and the Vector 22. The optical path length between the Globar source and the detector is longer than 1 m. The UV visible measurements are performed using a commercial HR 2000 high-resolution fibre optic Ocean Optics spectrophotometer equipped with a halogen light source HL2000. The detector is a linear silicon CCD array. The spectral resolution measured with a Hg-Ar calibration lamp is better than 0.2 nm. On the high-pressure device, the infrared measurements are performed using a Bruker Tensor 37 FTIR spectrometer. The IR configuration includes a NIR source, the Tensor 37 interferometer with a CaF2 beam splitter and a thermoelectrically-cooled InAs detector. The UV Visible measurements are made using a Varian Cary 300 spectrometer equipped with 600 μm core diameter optical fibres. The two experimental devices To contain the corrosive and concentrated mixtures, to allow gas phase speciation using optical spectrometries, two experimental devices were designed: a low-pressure one, and a high-pressure one. The low-pressure device shown in Figure 1 is manufactured out of quartz and Pyrex, and features a reservoir containing the liquid mixture (+solid) to be studied. This reservoir is equipped with a total pressure gauge, a Teflon valve and a connector to introduce products. The pressure gauge used is the “EBRO VM 2000 ex” model operating within a guaranteed measurement range from 0 to 2 bar up to 125°C. K-type thermocouples and platinum resistance sensors are used to measure the temperature at different positions inside the oven. Two cells, with windows made of Suprasil quality quartz, are located in the upper part of the device and allow the optical measurement of the gaseous phase concentrations of HI, I 2 and H 2 O. The first one, 250 mm long, is used for the measurement of HI and H 2 O concentrations by infrared absorption spectrometry. The second one, 5 mm long, enables the determination of the I 2 concentration measurement by UV visible absorption spectrometry. The high-pressure device is a microautoclave made of tantalum and located in a thermo-regulated oven as shown in Figure 2. It is a closed reactor with a constant volume of 140 cm 3 . The total expected pressure is about 80 bars for a temperature close to 280°C. Tantalum has been chosen as the reference material for the internal part of the reactor in order to avoid corrosion from the products under study. All connections between the different components of the reactor are sealed with 6 373 Kalrez O-rings. The associated instrumentation is composed of a set of 10 K-type thermocouples and a pressure gauge using a tantalum membrane. The stabilisation in temperature and pressure is obtained after 6 hours. The major difficulties encountered were of technological nature and led to a special design of the tantalum valve and of the pressure gauge. The experimental programme Five composition groups were studied in the low-pressure device, four composition groups in the high-pressure device as shown in Figure 3. The choice of the composition of the ternary mixtures was made in order to be representative of the different part of the reactive distillation column from bottom to top. The concentration range for iodine is between 4% and 85%. For a fixed iodine content, at least three different HI concentrations were realised around the total pressure minimum. NUCLEAR PRODUCTION OF HYDROGEN – © OECD/NEA 2010 193
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Nuclear Science 2010 Nuclear Produc
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ORGANISATION FOR ECONOMIC CO-OPERAT
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TABLE OF CONTENTS Table of contents
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TABLE OF CONTENTS Y. Gong, E. Chalk
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EXECUTIVE SUMMARY Executive summary
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EXECUTIVE SUMMARY steam turbine, in
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EXECUTIVE SUMMARY sulphur depositio
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EXECUTIVE SUMMARY affords saving 35
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EXECUTIVE SUMMARY safety assessment
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EXECUTIVE SUMMARY The question was
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CHANGING THE WORLD WITH HYDROGEN AN
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NUCLEAR HYDROGEN PRODUCTION PROGRAM
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NUCLEAR HYDROGEN PRODUCTION PROGRAM
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FRENCH RESEARCH STRATEGY TO USE NUC
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PRESENT STATUS OF HTGR AND HYDROGEN
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STATUS OF THE KOREAN NUCLEAR HYDROG
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THE CONCEPT OF NUCLEAR HYDROGEN PRO
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CANADIAN NUCLEAR HYDROGEN R&D PROGR
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APPLICATION OF NUCLEAR-PRODUCED HYD
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STATUS OF THE INL HIGH-TEMPERATURE
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HIGH-TEMPERATURE STEAM ELECTROLYSIS
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MATERIALS DEVELOPMENT FOR SOEC Mate
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A METALLIC SEAL FOR HIGH-TEMPERATUR
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DEGRADATION MECHANISMS IN SOLID OXI
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Page 170 and 171: CEA ASSESSMENT OF THE SULPHUR-IODIN
Page 181: STATUS OF THE INERI SULPHUR-IODINE
Page 184 and 185: INFLUENCE OF HTR CORE INLET AND OUT
Page 196 and 197: EXPERIMENTAL STUDY OF THE VAPOUR-LI
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Page 216 and 217: INTEGRATED LABORATORY SCALE DEMONST
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STUDY OF THE HYDROLYSIS REACTION OF
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DEVELOPMENT OF CuCl-HCl ELECTROLYSI
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EXERGY ANALYSIS OF THE Cu-Cl CYCLE
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CaBr 2 HYDROLYSIS FOR HBr PRODUCTIO
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SESSION V: ECONOMICS AND MARKET ANA
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DEVELOPMENT OF THE HYDROGEN ECONOMI
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NUCLEAR H 2 PRODUCTION - A UTILITY
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ALKALINE AND HIGH-TEMPERATURE ELECT
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THE PRODUCT OF HYDROGEN BY NUCLEAR
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SUSTAINABLE ELECTRICITY SUPPLY IN T
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PROHYTEC, THE FRENCH INDUSTRIAL PLA
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NHI ECONOMIC ANALYSIS OF CANDIDATE
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MARKET VIABILITY OF NUCLEAR HYDROGE
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POSSIBILITY OF ACTIVE CARBON RECYCL
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NUCLEAR SAFETY AND REGULATORY CONSI
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TRANSIENT MODELLING OF S-I CYCLE TH
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PROPOSED CHEMICAL PLANT INITIATED A
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CONCEPTUAL DESIGN OF THE HTTR-IS NU
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USE OF PSA FOR DESIGN OF EMERGENCY
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HEAT PUMP CYCLE BY HYDROGEN-ABSORBI
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HEAT EXCHANGER TEMPERATURE RESPONSE
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ALTERNATE VHTR/HTE INTERFACE FOR MI
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POSTER SESSION CONTRIBUTIONS Poster
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ACTIVITIES OF NUCLEAR RESEARCH INST
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ACTIVITIES OF NUCLEAR RESEARCH INST
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A URANIUM THERMOCHEMICAL CYCLE FOR
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A URANIUM THERMOCHEMICAL CYCLE FOR
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MEETING ORGANISATION Annex 1: Meeti
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LIST OF PARTICIPANTS REYTIER, Magal
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LIST OF PARTICIPANTS BROWN, Nichola
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LIST OF PARTICIPANTS SINK, Carl US
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