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Process for Preparing Reactive Magnesium Oxide

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Process for Preparing Reactive Magnesium Oxide (19) & (11) EP 1 254 083 B1 (12) EUROPEAN PATENT SPECIFICATION (45) Date of publication and mention (51) Int Cl.: of the grant of the patent: C04B 9/12 (2006.01) C04B 28/10 (2006.01) 03.08.2011 Bulletin 2011/31 (86) International application number: (21) Application number: 01946835.4 PCT/AU2001/000077 (22) Date of filing: 29.01.2001 (87) International publication number: WO 2001/055049 (02.08.2001 Gazette 2001/31) (54) PROCESS FOR PREPARING REACTIVE MAGNESIUM OXIDE CEMENTS VERFAHREN ZUR HERSTELLUNG VON REAKTIVEN MAGNESIUMOXIDZEMENTEN PROCEDE DE PREPARATION DE CIMENTS D’OXYDE DE MAGNESIUM REACTIF (84) Designated Contracting States: (56) References cited: AT BE CH CY DE DK ES FI FR GB GR IE IT LI LU EP-A2- 0 352 096 AU-A- 5 571 573 MC NL PT SE TR FR-A- 890 325 GB-A- 871 428 US-A- 2 880 101 US-A- 4 572 862 (30) Priority: 27.01.2000 AU PQ527100 01.05.2000 AU PQ718100 • DATABASE WPI Derwent Publications Ltd., London, GB; Class L02, AN 1978-01248A, (43) Date of publication of application: XP003007992 & JP 52 138 522 A (ASAHI 06.11.2002 Bulletin 2002/45 CHEMICAL IND KK) 18 November 1977 • DATABASE WPI Derwent Publications Ltd., (73) Proprietor: TECECO PTY LTD London, GB; Class L02, AN 1980-31587C, Glenorchy, Tasmania 7010 (AU) XP003007993 & JP 55 037 469 A (MATSUSHITA ELEC WORKS) 15 March 1980 (72) Inventor: HARRISON, Aubry, John, Weston • DATABASE WPI Derwent Publications Ltd., Glenorchy, Tasmania 7010 (AU) London, GB; Class L02, AN 1984-156243, XP003007994 & JP 59 083 970 A (MITSUI (74) Representative: Andrae, Steffen et al MOKUZAI KOGY) 15 May 1984 Andrae Flach Haug • DATABASE WPI Derwent Publications Ltd., Balanstrasse 55 London, GB; Class P43, AN 1984-186182, 81541 München (DE) XP003007995 & JP 59 105 882 A (NIPPON CEMENT KK) 19 June 1984 • DATABASE WPI Week 199519, Derwent Publications Ltd., London, GB; Class A94, AN 1995-144563,XP003007996 & JP 7 069 706 A (ADO CERAMICS KENKYUSHO YG) 14 March 1995 • DATABASE WPI Week 199836, Derwent Publications Ltd., London, GB; Class L02, AN 1998-426033, XP003007997 & RU 2 102 349 C1 (NIZHEGOROD ARCHITECTURE BUILDING) 20 January 1998 Note: Within nine months of the publication of the mention of the grant of the European patent in the European Patent Bulletin, any person may give notice to the European Patent Office of opposition to that patent, in accordance with the Implementing Regulations. Notice of opposition shall not be deemed to have been filed until the opposition fee has been paid. (Art. 99(1) European Patent Convention). EP 1 254 083 B1 Printed by Jouve, 75001 PARIS (FR) EP 1 254 083 B1 Description Technical Field of the Invention 5 [0001] This invention relates to a process for preparing a hydraulic amount composition containing magnesium oxide (magnesia). A process for making cement is described in FR-A 890325. Background to the Invention 10 [0002] A number of cements based on magnesia have previously been made. If a salt such as magnesium chloride or sulphate is added to reactive magnesia and the mixture is allowed to react and hydrate magnesium oxychlorides and magnesium oxysulphates are formed that can be very strong but are not sufficiently weatherproof and are corrosive. Although there are many patents describing improvements to overcome these deficiencies such as the use of phosphates or soluble silicates, they are not generally economic. 15 [0003] Magnesium oxychlorides were first discovered and prepared by Sorel in 1867. Magnesium oxysulphates were discovered by Olmer and Delyon in 1934. Magnesium oxychlorides and oxysulphates are commonly referred to as Sorel cements. [0004] A number of compounds are formed when magnesia reacts with magnesium chloride to form oxychlorides. The main bonding phases so far found in hardened cement pastes are Mg(OH)2, (Mg(OH)2)3 .MgCl2 .8H2O and (Mg 20 (OH)2)5.MgCl2.8H2O. (Mg(OH)2)5.MgCl2.8H2O has superior mechanical properties and is formed using a molar ratio of MgO:MgCl2:H2O = 5:1:13 MgCl2 + 5MgO + 13H2O = (Mg(OH)2)5.MgCl2.8H2O 25 [0005] If magnesium sulphate is used instead four oxysulphate phases are considered to form at temperatures between 30 and 120°C; Ng(OH)2)5.MgSO4.3H2O,(Mg(OH)2)3.MgSO4.8H2O. Mg(OH)2.MgSO4.5H2O, and Mg(OH)2.2MgSO4. 3H2O. Only (Mg(OH)2)3.MgSO4.8H2O is stable below 35°C. 3MgO + MgSO4 +11H2O = (Mg(OH)2)3.MgSO4.8H2O 30 [0006] Zinc, calcium, copper and other elements also form similar compounds. Magnesium oxychlorides achieve higher compressive strengths than magnesium oxysulphates. The main problem with Sorel cements is that both mag- nesium oxychlorides and magnesium oxysulphates tend to break down in water and particularly in acids. Corrosion of steel reinforcing also occurs. 35 [0007] The use of soluble silicates such as sodium silicate has been described as a means of improving the water resistance of Sorel type cements. These cements are of little practical use however because of the high cost of soluble silicates. [0008] Magnesia reacts with soluble phosphates to precipitate almost totally insoluble magnesium phosphate. 40 MgO + H2O = Mg(OH)2 3Mg(OH)2 + 2H3PO4 = Mg3((PO)4)2 + 6H2O [0009] The use of phosphates has also been advocated as a means of improving the water resistance of Sorel type 45 cements. Such cements, although described in the literature, are expensive due to the shortage of economic deposits of phosphate and as a result widespread use is limited. [0010] A range of magnesium phosphate cements has been used including magnesium ammonium phosphate which is thought to be formed by an acid-base reaction between magnesia and di hydrogen ammonium phosphate. This results in an initial gel formation followed by the crystallisation into an insoluble phosphate, mainly magnesium ammonium 50 phosphate hexahydrate, [NH4MgPO4.6H2O]. The magnesium oxide used in this system is produced by calcining at higher temperatures and is referred to in the industry as being "dead burned" and is not as reactive as magnesia made at lower temperatures. A set retarder, typically either borax or boric acid is also used to give a workable set time. MgO + NH4H2PO4 + 5H2O = NH4MgPO4.6H2O 55 [0011] High-lime magnesiochrome cement finds use in refractories. The cement is based upon magnesia plus calcium chromate - chromite, a complex mineral produced by the combination of lime with chrome oxide (Cr 2O3) in an oxidising environment Hydration is normally performed with a 30% aqueous solution of magnesium chloride hexahydrate (MgCl 2. 2 EP 1 254 083 B1 6H2O) solution at 8 per cent by weight of the cement. The products are complex. As well as hydrates they also consist of carbonates, which are formed by the effects of carbonation. Typical products formed can include brucite [Mg(OH)2], various magnesium oxychlorides [(Mg (OH)2)X.MgCl2.YH2O] calcium chromate dihydrate (CaCrO 4.2H2O), calcium mon- ochromite (CaCr2O4) portlandite [Ca(OH)2], secondary magnesium carbonate (MgCO3), secondary calcium carbonate 5 (CaCO3) and mixed calcium magnesium carbonates [(Ca,Mg)CO3]. [0012] Other known cementitions magnesia compounds include hydroxychlorides and sulphates such as Mg (OH)2).MgCl2.8H2O, hydroxy carbonates [Mg5(OH)2(CO)4.4H2O] and hydroxy chloro carbonates [e.g. Mg2OHClCO3. 3H2O] as well as hydro magnesite and magnesite. [0013] Brucite [Mg(OH)2] alone has not found much commercial use as a cement previously mainly because the 10 setting rate is too slow. Summary of the Invention [0014] The invention provides a process for preparing a hydraulic cement composition including blending of reactive 15 magnesium oxide with one or more hydraulic cements wherein the reactive magnesium oxide is blended at a level of at least 5% by weight of the hydraulic cementitious components excluding pozzolan and the reactive magnesium oxide has been prepared by being calcined separately from other hydraulic cementitious components at a temperature of less than 750°C and ground to a particle size with greater than 95% of the particles of less than 120 microns before blending wherein said reactive magnesium oxide in the composition hydrates to form brucite as a binder in the hydraulic cement 20 matrix. [0015] The hydraulic cements can include any hydraulic cement including Portland type cements, calcium aluminate cements, alinite cements, belinite cements, belite cements, hydrogarnet cements and ferrari cements as well as other magnesium cements such as Sorel cements. Pozzolans (including wastes) and fillers are not regarded as hydraulic cementitious components in this specification. Sorel cements include water in their composition and are therefore con- 25 sidered as hydraulic cements. [0016] Preferably the prepared composition further includes at least 10% of a pozzolan. [0017] Preferably the prepared hydraulic cement composition includes ground Portland cement clinker type minerals. Detailed Description of the Invention 30 [0018] The present invention provides a process for preparing cement compositions containing substantial proportions of reactive magnesia that hydrates to form brucite which is a useful cementitious component. The prepared compositions generally but not always contain a high proportion of pozzolans, many of which are wastes such as fly ash. [0019] The process includes the blending of reactive magnesia with hydraulic cements, preferably Portland cements 35 but also other cements including other magnesium cements and/or the use of various accelerators as a means of improvingthe setting and hardening times and early strength. Both blending with other cements and the use of accelerators as formulation strategies can be used independently, or sometimes combined to advantage rendering brucite useful as a binder in a cement matrix. [0020] When other commercially useful cements are blended with reactive Magnesia in the formulations prepared 40 according to this invention ultimate strength is also improved. The magnesia in turn provides a virtually insoluble matrix of high pH in which most other cements are stable and affords a degree of protection in normally aggressive solutions such as sulphates.
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