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Good Quality-Final Version of Thesis-Yingxia Qu Experimental Study of the Melting and Reduction Behaviour of Ore Used in the HIsarna Process PhD thesis Yingxia Qu This research described in this thesis was performed in the department of Materials Science and Engineering of Delft University of Technology in the Netherlands. This research was carrier out under project number M41.5.09327 in the framework of the Research Program of the Materials Innovation Institute M2i in the Netherlands (www.m2i.nl). Experimental Study of the Melting and Reduction Behaviour of Ore Used in the HIsarna Process Proefschrift ter verkrijging van de graad van doctor aan de Technische Universiteit Delft; op gezag van de Rector Magnificus prof. ir. K.C.A.M. Luyben; voorzitter van het College van Promoties in het openbaar te verdedigen op 3 september 2013 om 10:00 uur door Yingxia Qu Master of Engineering in Ferrous Metallurgy Northeastern University, Shenyang, China geboren te Liaoning, China Dit proefschrift is goedgekeurd door de promotor: Prof. dr. R. Boom Copromotor: Dr. Y. Yang Samenstelling promotiecommissie: Rector Magnificus, voorzitter Prof. dr. R. Boom, Technische Universiteit Delft, promotor Dr. Y. Yang, Technische Universiteit Delft, copromotor Prof. dr. P. Taskinen, Aalto University, Finland Prof. dr. ir. J. Sietsma, Technische Universiteit Delft Prof. dr. J. H.W. de Wit, Technische Universiteit Delft Dr. C. Zeilstra, Tata Steel, Netherlands Prof. dr. S. Seetharaman, Warwick University, United Kingdom Prof. dr. I. Richardson, Technische Universiteit Delft (Reserve) Keywords: smelting reduction, smelting cyclone, iron-making, fine iron ore, thermal decomposition, individual particle, iron ore reduction, ISBN: 978-90-6562-330-0 Copyright ©2013, by Yingxia Qu [email protected] All rights reserved. No part of the material protected by this copyright notice may be reproduced or utilized in any form or by any means, electronic or mechanical, including photocopying, recording or by any information storage and retrieval system, without permission from the author. Printed in the Netherlands To my family… Contents Contents Contents .................................................................................................................. i Chapter 1 Introduction .......................................................................................... 1 1.1 Background to the present study .......................................................................1 1.2 Current status of the ironmaking and steelmaking processes............................2 1.2.1 Blast furnace ironmaking process ........................................................... 4 1.2.1.1 Conventional blast furnace.......................................................... 4 1.2.1.2 Top gas recycling blast furnace (TGRBF) with CO 2 capture and storage (CCS) ......................................................................................... 6 1.2.2 Non-blast furnace ironmaking technology ............................................... 7 1.3 Basic reactions and thermodynamics of the gas solid iron oxide reduction..... 18 1.3.1 The sequence of reduction of iron oxides with gases............................ 19 1.3.2 Equilibrium between iron oxides and reducing gases ........................... 19 1.4 Kinetics of reduction of iron oxides with gases ................................................ 22 1.4.1 Rate law ................................................................................................ 22 1.4.2 Reaction rate of iron ore reduction ........................................................ 24 1.5 Determination of rate controlling steps of iron ore reduction............................ 28 1.5.1 Model–fitting methods ........................................................................... 29 1.5.2 Model–free methods.............................................................................. 33 1.5.2.1 Standard method....................................................................... 33 1.5.2.2 Friedman’s method.................................................................... 33 1.6 Objectives and layout of the thesis .................................................................. 34 References............................................................................................................. 36 Chapter 2 Experimental Apparatus and Analysis Methods ............................. 39 2.1 Introduction ...................................................................................................... 39 2.2 High temperature drop tube furnace ................................................................ 41 2.2.1 The furnace ........................................................................................... 44 2.2.2 The syringe pump feeder....................................................................... 44 2.2.3 Injection probe....................................................................................... 45 2.2.4 Sampling probe ..................................................................................... 50 2.2.5 Sample collector.................................................................................... 51 2.2.6 Pre-tests before the experiment ............................................................ 51 2.2.6.1 Syringe pump particle feeder .................................................... 51 2.2.6.2 Temperature profile and cooling effect in the reactor ................ 52 2.3 TGA – DSC ...................................................................................................... 55 2.4 Electrically heated horizontal furnace .............................................................. 56 2.5 Analysis methods ............................................................................................. 57 References............................................................................................................. 59 i Contents Chapter 3 Experimental Study on the Thermal Decomposition Behaviour of Iron Ore Particles ................................................................................................. 61 3.1 Introduction ...................................................................................................... 61 3.2 Theoretical evaluation...................................................................................... 63 3.3 Experimental .................................................................................................... 66 3.3.1 Experimental strategy............................................................................ 66 3.3.2 Materials................................................................................................ 67 3.3.3 Experimental conditions ........................................................................ 68 3.3.3.1 Thermal decomposition of iron ore in the TGA-DSC ................. 68 3.3.3.2 Thermal decomposition of iron ore in the horizontal furnace..... 68 3.3.3.3 Thermal decomposition of iron ore in the HDTF........................ 69 3.4. Results and discussion ................................................................................... 72 3.4.1 Experimental results with TGA-DSC...................................................... 72 3.4.1.1 Thermal decomposition of hematite ore .................................... 72 3.4.1.2 Thermal decomposition of hematite .......................................... 77 3.4.2 Experimental results in the horizontal furnace....................................... 80 3.4.2.1 Effect of holding time................................................................. 80 3.4.2.2 Effect of temperature................................................................. 81 3.4.3 Experimental results in the HDTF.......................................................... 83 3.4.3.1 Effect of temperature and gas ................................................... 84 3.4.3.2 Effect of residence time............................................................. 86 3.4.3.3 Effect of particle size ................................................................. 88 3.4.4 Reproducibility tests .............................................................................. 89 3.4.5 Summary of the main results................................................................. 91 3.5 Conclusions ..................................................................................................... 92 References............................................................................................................. 94 Chapter 4 Reduction Behaviour of Individual Iron Ore Particles in the High Temperature Drop Tube Furnace ....................................................................... 95 4.1 Introduction ...................................................................................................... 95 4.2 Experimental procedures ................................................................................. 95 4.3 Experimental conditions................................................................................... 96 4.4 Experimental objective and strategy ................................................................ 99 4.5 Experimental results of the iron ore reduction................................................ 100 4.5.1 Reduction degree of hematite ore ....................................................... 100 4.5.1.1 Reproducibility testing ............................................................. 100 4.5.1.2 Effect of PCR and H 2 content of the reducing gas..................
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