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Presentation___ 01/11/2000 GRECIAN MAGNESITE S.A. - Presentation at Industrial Minerals Annual Forum - Minerals in Architectural Markets, November 2000 MAGNESIA CEMENTS: OVER A HUNDRED YEARS OLD BUT STILL NOVEL Paper presented by: M. HALARIS, Dr.

  1. Presentation___ 01/11/2000 GRECIAN MAGNESITE S.A. - Presentation at Industrial Minerals Annual Forum - Minerals in Architectural Markets, November 2000 MAGNESIA CEMENTS: OVER A HUNDRED YEARS OLD BUT STILL NOVEL Paper presented by: M. HALARIS, Dr. TH. ZAMPETAKIS MAGNESITE /MAGNESIA BACKGROUND Magnesite, magnesia and magnesium compounds are terms used to designate a variety of industrial raw materials which are related by their common main constituent, magnesium, but still very much diversified by their different properties as well as different uses. The term � magnesia � in particular refers to the various types of magnesium oxides, which are available in the market. Deadburned magnesia, caustic calcined magnesia and electrofused magnesia are all three magnesium oxides possessing different physical properties and thus addressing to diverse applications. Magnesia originates from two main sources: Natural and synthetic. The basic concept and technology of the two production processes are quite different, while the resulting end products are similar, presenting however differences in terms of their respective degree of purity. Figure 1 presents schematically the production process of magnesite / magnesia / magnesium compounds from natural sources. Magnesite / magnesia is used in several industrial sectors. It is worth mentioning that contrarily to deadburned magnesia (dbm) which is mainly used as a high duty refractory raw material, caustic calcined magnesia (ccm) addresses to a much wider spectrum of applications, including certain specialized niche markets. Figure 2 summarizes the main magnesite / magnesia fields of application. μμ

  2. Figure 1: Production process from natural sources Figure 2: Magnesite / Magnesia Applications CAUSTIC CALCINED MAGNESIA · Construction · Industrial flooring · Insulating panels Environmental applications: · Flue gas treatment Various Industrial applications: · Industrial effluent treatment · Pulp and paper industry · Sewage treatment · Abrasives (grinding and polishing wheels) · Water purification · Electrofused magnesia · Acid rain · Steel industry (fluxes, insulating powder, · Waste incinerators electrical steel) · Glass industry Agricultural applications: · Tanning industry · Animal Feed · Fuel & lubricant additives · Fertilizers, Soil conditioner · Sugar μμ

  3. · Chemicals, pharmaceuticals, cosmetics · Fillers (plastics, rubber, paints, adhesives) DEADBURNED MAGNESIA · Refractories · Magnesium metal · Welding fluxes · Heating elements · Mineral insulated cables MAGNESITE RAW · Ceramics · Fertilizers · Welding fluxes · Magnesium metal · Fluxes for the steel industry · Fillers For the sake of completeness of this short prologue on magnesite / magnesia fundamentals the following global figures on production and consumption are presented to the best of our knowledge in order to show the significance of this important industrial minerals sector. Magnesite / Magnesia Global Figures · World natural magnesite reserves: 10.000.000.000 mt · World natural magnesite production: 18.000.000 mt/annum · World magnesia production /consumption 9.500.000 mt/annum out of which... sources over 80%, dbm: over 80% From natural: sources less than 20%, ccm: less than 20% From synthetic: μμ

  4. MAGNESIA CEMENTS In 1867 a French engineer named Stanislas Sorel discovered that when active magnesium oxide is added to a solution of magnesium chloride an exothermic reaction takes place and forms magnesium oxychloride, which appears like an extremely strong and hard block. Investigating further the properties of magnesium oxychloride he realized that, apart from its extraordinary endurance in mechanical strength, it also had an excellent bonding capacity, enabling the binding of various organic and inorganic aggregates. The first aggregate used was wood shavings (sawdust) and the initial commercial application of this invention was in the construction of flooring, which became known as Sorel cement floor. The first floors were laid during the 1890 � s for use in residential and industrial constructions under the name of � xylolith � (wood stone) or � parquet sans joints � (jointless floor). Further technical developments followed over the years in terms of the aggregates and additives, as well as the solutions of magnesium salts used, enlarging the spectrum of application of the magnesia cement. Magnesium oxychloride (MOC) Magnesium oxysulphate (MOS) Magnesium phosphate (MAP) are well known magnesia cements which are mainly used in architectural applications, such as: · Construction of industrial floors · Construction of thermal and acoustical insulating panels and _other prefabricated building boards · Grinding and polishing stone μμ

  5. · Fire proofing and special light construction elements · Plus some lesser applications such as production of special stuccos and manufacture of articrafts. MAGNESIUM OXYCHLORIDE CEMENT Chemistry This cement is manufactured by mixing magnesia with magnesium chloride solutions in well-defined proportions to produce the magnesium oxychloride, which is the bonding phase. The investigation of the system MgO-MgCl2-H2O by some authors1-5 highlights the complexity of the Sorel cement chemistry because of the large number of parameters affecting the nature and the quality of the reaction products between magnesium oxide and magnesium chloride solution. The main bonding phases found in hardened Sorel cement are 5Mg(OH)2?MgCl2?8H2O (form-5: Diag.1) and 3Mg(OH)2?MgCl2?8H2O (form-3: Diag.2). This is in agreement with previous research work3, stating that form-3 and form-5 are the only stable phases in the system MgO-MgCl2-H2O (fig.3). Figure 3: The system MgO-MgCl2-H2O The first, because of its crystallization in well-formed needle like crystals (fig.4) has superior mechanical properties and is formed using a molar ratio of MgO:MgCl2:H2O = 5:1:13 according to the global reaction (1). The theoretical formation of form-3 corresponds to a molar ratio of MgO:MgCl2:H2O = 3:1:11 according to the global reaction (2). 5Mg0+MgCl2+13H2O � 2Mg3(OH)5Cl?4H2O (1) 3Mg0+MgCl2+11H2O � 2Mg2(OH)3Cl?4H2O (2) Figure 4: Crystal structure of the MOC (form-5) μμ

  6. A parallel or competitive reaction is the hydration of magnesium oxide due to the presence of excess water according to the chemical equation (3). MgO + H2O � Mg (OH)2 (3) The presence of Mg (OH)2 indicates a low quality magnesium oxychloride and in some cases the form-5 phase is transformed at later stages to the form-3 with mechanical strength decrease. Some authors6,7 attribute the late appearance of the form-3 phase to the reaction between the Mg (OH)2 obtained from reaction (3) and the unreacted MgCl2 present in the mortar under some conditions. In our experiments we observed this transformation of phases in some caustic magnesias produced from microcrystalline type magnesite (diag.3). Over a period of time, atmospheric carbon dioxide is possible to react with magnesium oxychloride to form a surface layer of Mg (OH)ClCO3?3H2O able to limit the Sorel cement � s water sensibility (diag.4). Sorrell and Urwongse state in their investigations3 that «samples with composition near 3.1.8 (form-3) showed a marked tendency to form the chlorocarbonate Mg (OH)2?MgCl2?2MgCO3?6H2O». Through our own research work on the subject we concluded that the appearance of chlorocarbonate is not correlated with the existence of the form-3 phase and its formation could be possible from both magnesium oxychloride phases (form-3 and form-5) according to the following global chemical equations: 3Mg(OH)2?MgCl2?8H2O + 2CO2 � Mg(OH)2?MgCl2?2MgCO3?6H2O+4H2O (4) 5Mg(OH)2?MgCl2?8H2O + 2CO2 � Mg(OH)2?MgCl2?2MgCO3?6H2O+4H2O+Mg(OH)2 (5) Dry atmospheric conditions eliminate the water produced and favor the chlorocarbonate formation, reaction (5) generates the very white Mg(OH)2, which could appear as white shadows on the Sorel cement � s surface. Cole and Demediuk8 also reported that both forms change after long periods of time to the above mentioned basic magnesium chlorocarbonate. The influence of this phase formation on mechanical and other Sorel cement properties has not been investigated yet. Raw Materials Both magnesia � s physical properties and magnesium chloride solution characteristics in association with various components proportions are the main parameters to obtain magnesium oxychloride cement with suitable properties. Important raw materials characteristics affecting Sorel cement properties are the following: Caustic calcined magnesia Caustic calcined magnesia from natural magnesite is the normal magnesia type used for Sorel cement products. Grecian CCM, because of its unique properties such as whiteness, microcrystallinity, high Mg0 availability and capability to produce mortars with adjustable setting properties, has a leading position on this market. The most important magnesia � s characteristics affecting its performance in this application are: Microstructure: It is well known that this magnesia � s characteristic depends on the raw magnesite used for its production. There are two types of natural magnesite, the macro μμ

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