US20030041785A1 - Reactive magnesium oxide cements - Google Patents

Reactive magnesium oxide cements Download PDF

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US20030041785A1
US20030041785A1 US10/181,442 US18144202A US2003041785A1 US 20030041785 A1 US20030041785 A1 US 20030041785A1 US 18144202 A US18144202 A US 18144202A US 2003041785 A1 US2003041785 A1 US 2003041785A1
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hydraulic cement
cements
cement composition
magnesia
magnesium
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Aubrey Harrison
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TecEco Pty Ltd
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Priority claimed from AUPQ5271A external-priority patent/AUPQ527100A0/en
Priority claimed from AUPQ7181A external-priority patent/AUPQ718100A0/en
Application filed by Individual filed Critical Individual
Assigned to TECECO PTY LTD reassignment TECECO PTY LTD ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: HARRISON, AUBRY JOHN WESTON
Publication of US20030041785A1 publication Critical patent/US20030041785A1/en
Priority to US11/016,722 priority Critical patent/US7347896B2/en
Abandoned legal-status Critical Current

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    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
    • C04B28/30—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing magnesium cements or similar cements
    • C04B28/32—Magnesium oxychloride cements, e.g. Sorel cement
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
    • C04B28/02—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing hydraulic cements other than calcium sulfates
    • C04B28/04—Portland cements
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
    • C04B28/02—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing hydraulic cements other than calcium sulfates
    • C04B28/06—Aluminous cements
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
    • C04B28/02—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing hydraulic cements other than calcium sulfates
    • C04B28/10—Lime cements or magnesium oxide cements
    • C04B28/105—Magnesium oxide or magnesium carbonate cements
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
    • C04B2111/20—Resistance against chemical, physical or biological attack
    • C04B2111/23—Acid resistance, e.g. against acid air or rain
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
    • C04B2111/20—Resistance against chemical, physical or biological attack
    • C04B2111/24—Sea water resistance
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W30/00—Technologies for solid waste management
    • Y02W30/50—Reuse, recycling or recovery technologies
    • Y02W30/91—Use of waste materials as fillers for mortars or concrete

Definitions

  • This invention relates to magnesium cements and in particular to cements containing magnesium oxide (magnesia).
  • Magnesium oxychlorides were first discovered and prepared by Sorel in 1867. Magnesium oxysulfates were discovered by Olmer and Delyon in 1934. Magnesium oxychlorides and oxysulfates are commonly referred to as Sorel cements.
  • a number of compounds are formed when magnesia reacts with magnesium chloride to form oxychlorides.
  • magnesium sulfate is used instead four oxysulfate phases are considered to form at temperatures between 30 and 120° C.; (Mg(OH) 2 )5T.MgSO 4 .3H 2 O,(Mg(OH) 2 )3.MgSO 4 .8H 2 O, Mg(OH) 2 .MgSO 4 .5H 2 O, and Mg(OH) 2 .2MgSO 4 .3H 2 O. Only (Mg(OH) 2 )3.MgSO 4 .8H 2 O is stable below 35° C.
  • Zinc, calcium, copper and other elements also form similar compounds.
  • Magnesium oxychlorides achieve higher compressive strengths than magnesium oxysulfates.
  • the main problem with Sorel cements is that both magnesium oxychlorides and magnesium oxysulfates tend to break down in water and particularly in acids. Corrosion of steel reinforcing also occurs.
  • 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 crystallisation into an insoluble phosphate, mainly magnesium ammonium phosphate hexahydrate, [NH 4 MgPO 4 .6H 2 O].
  • 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.
  • 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 2 O 3 ) in an oxidising environment. Hydration is normally performed with a 30% aqueous solution of magnesium chloride hexahydrate (MgCl 2 .6H 2 O) solution at 8 per cent by weight of the cement.
  • MgCl 2 .6H 2 O magnesium chloride hexahydrate
  • 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.MgCl 2 .YH 2 O.] calcium chromate dihydrate (CaCrO 4 .2H 2 O), calcium monochromite (CaCr 2 O 4 ) portlandite [Ca(OH) 2 ], secondary magnesium carbonate (MgCO 3 ), secondary calcium carbonate (CaCO 3 ) and mixed calcium magnesium carbonates [(Ca,Mg)CO 3 ].
  • cementitious magnesia compounds include hydroxychlorides and sulfates such as Mg(OH) 2 .MgCl 2 .8H 2 O, hydroxy carbonates [Mg 5 (OH) 2 (CO 3 ) 4 .4H 2 O] and hydroxy chloro carbonates [e.g. Mg 2 OHClCO 3 .3H 2 O] as well as hydro magnesite and magnesite. Hydroxy chloro carbonates and sulfates are also formed as a result of atmospheric carbonation of magnesium oxy chloride and magnesium oxy sulphate, and these often ultimately revert to magnesite and hydromagnesite.
  • hydroxychlorides and sulfates such as Mg(OH) 2 .MgCl 2 .8H 2 O, hydroxy carbonates [Mg 5 (OH) 2 (CO 3 ) 4 .4H 2 O] and hydroxy chloro carbonates [e.g. Mg 2 OHClCO 3 .3H 2 O] as well as
  • Most hydraulic cements are calcium based and apart from calcium aluminate and some slag cements, generally contain ground Portland type clinkers and are classified as Portland type cements by standards developed in most countries to ensure their quality. In Europe a large number of countries have been involved in the development of what is referred to as the European Prestandard for Common Cements (ENV 197-1:1992) which covers a wide range of formulations including Portland cements, Portland—slag cements (including slag from steel making), Portland silica fume cements, Portland pozzolana or flyash cements, Portland burnt shale cements, Portland limestone cements, Portland composite cements, blast furnace cements, pozzolanic cements and various composite cements.
  • ENV 197-1:1992 European Prestandard for Common Cements
  • ASTM American Society for Testing and Materials
  • Applicable standards are C 150-95 (Standard specification for Portland cement), C219-94 (Standard terminology relating to hydraulic cement) and C595M-95 (Standard specification for blended hydraulic cements).
  • Other hydraulic cements include geopolymers which are based on poly(silico-oxo-aluminate) or (—Si—O—Al—O—)n (with n being the degree of polymerization).
  • Geopolymers are formed from the geosynthesis of poly(silisic) acid (SiO 2 )n and potassium alumina-silicate, in aqueous alkali medium (KOH, NaOH), Ca(OH)2, Mg(OH)2 etc.) As water is required to synthesise the precursors that polymerise in the reaction, the cement is considered to be hydraulic in terms of the definition cited.
  • the invention provides in one form a cement composition that includes reactive magnesium oxide at a level of at least 5% w/w of hydraulic cementitious components in the composition excluding pozzolans wherein the magnesium oxide is prepared by low temperature calcination and fine grinding and wherein the hydraulic cementitious components exclude magnesium oxychlorides and magnesium oxysulfates.
  • the cementitious components may include any hydraulic cement defined in ASTM C219-94 as “a cement that sets and hardens by chemical interaction with water and that is capable of doing so under water.” This definition includes a wide range of cements including but not limited to Portland and blended Portland type cements listed by the various standards, slag cements, calcium aluminate type cements, alite cements, belite cements, ferrari cements lime cements and geopolymers. as well as sulfates other than the excluded magnesium salts.
  • the ratio of reactive magnesia to ground Portland clinker is in the range 1:3 to 2.5:1.
  • composition further includes at least 10% of a pozzolan w/w.
  • composition further includes at least 80% of a pozzolan w/w.
  • the pozzolan is fly ash.
  • the hydraulic cement composition includes ground Portland cement clinker type minerals.
  • the present invention provides cement compositions containing substantial proportions of reactive magnesia that hydrates to form brucite which is a useful cementitious component. They generally but not always contain a high proportion of pozzolans, many of which are wastes such as fly ash.
  • compositions include the blending of reactive magnesia with hydraulic cements, preferably Portland cements but also other cements including other magnesium cements and/or the use of various accelerators as a means of improving the 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.
  • pozzolans is not necessary as a strong cement is produced by merely blending Portland cement clinker minerals and reactive magnesia. However, they are useful as they have, most often only when activated, but sometimes depending on their composition without activation, cementitious properties. They also serve to mask the slower setting times of the magnesia component, preventing structural defects and if they are also wastes, they reduce costs.
  • accelerators are both an additional and alternative technique to improve early setting and hardening times of cements. If accelerators such as ferrous sulfate are used whether with blends of reactive magnesia and pozzolans alone (an alternative technique) or also with other cementitious components (an additional technique) they are added in small proportion only (less than 20% of the MgO proportion).
  • a particular embodiment of the strategy of blending magnesia with Portland clinker minerals was made with the following proportions that achieved high strengths in the order of 12-20 mpa after pre curing for 48 hours followed by steaming at 55° C. for 48 hours and then further curing for a period of three weeks.
  • the composition was made by mixing as dry powders 600 g (94% by weight) fly ash from the Gladstone power station in Australia, 30 g (4.67% by weight) reactive magnesia ground to 95% passing 45 micron and 100% passing 125 micron (branded as XLM and from Causmag in Australia) and 12 g (1.87% by weight) ground Portland cement clinker ground to 100% less than 125 micron from Australian Cement in Railton Kenya. Water was added to make a stiff paste and this was then vibrated into moulds. After approximately six weeks the sample reached a strength approaching 20 mpa and was resistant to sulfates and other solutions aggressive to Portland cement.
  • Portland cements containing magnesium oxide are currently termed “unsound” and the use of limestones containing magnesium for making Portland cements is avoided. The reason why is because when magnesite or dolomite, present as an “impurity” contained in limestone, is slaked at high temperatures during the manufacture of Portland cement, a highly unreactive oxide termed “dead burned magnesia” is produced and added hydrates long after other cementitious components.
  • Magnesite (MgCO 3 ) begins decomposing to the oxide at a substantially lower temperatures and pressure than limestone (CaCO 3 ) This is true of mixtures of limestone and magnesite as well as for the distinguishable mineral dolomite which contains both magnesium and calcium as carbonates.
  • Atomic No. Enthalpy Entropy T(PCO 2 Reaction of metal ⁇ H 0 (kcal) ⁇ G 0 (kcal) 1 atm)
  • MgCO 3 MgO + CO 2 12 28 16 540° C.
  • CaCO 3 GaO + CO 2 20 42 31 900° C.
  • Portland cement is typically made between 1450° C. and 1500° C. At these temperatures any magnesium carbonate content becomes unreactive due to the formation of larger more defined crystals with less surface area and lower porosity than at lower temperatures.
  • Magnesia produced in this manner referred to as ‘dead burned’, is unreactive and hydrates very slowly—usually long after the other components in a cement such as Portland cement have hydrated. As a result stresses are introduced resulting in what is often termed unsound cement. Because of this magnesium oxides have been condemned for many years in Portland cement. Unreactive magnesia is also unsuitable for use in the present invention.
  • magnesia and other cements and in particular Portland type cements are matched.
  • magnesia component must be separately calcined at lower temperatures and in conditions that are suitable for the manufacture of reactive magnesia, ground to a fine size depending on the reactivity required and only then blended with other cementitious components, pozzolans or both.
  • Suitable magnesia should be calcined at low temperatures (less than 750° C.) and ground to greater than 95% passing 120 micron. Generally the lower the temperature of calcination and finer the grind, the more reactive the magnesia is and the faster it hydrates. Magnesia calcined as 650° C. passing 45 micron or less is better.
  • a suitable test for reactivity is the citric acid test and low temperature calcined magnesia ground to 95% passing 45 micron tests at about 10 seconds using this method which uses 0.5 g sodium benzoate, 28 g citric acid monhydrate and 0.1 g phenolphthaleim dissolved in water and diluted to 1 litre.
  • the test method is to first weigh a 2.00 g sample of magnesia on a watch glass. Then Pipette 100 ml of the prepared solution in to a dry 250 ml tall form beaker. Add the 2.00 g powder sample previously weighed and stir (preferably with a magnetic stirrer) immediately. Record the time in seconds for the stirred solution to turn pink.
  • the reactivity and hydration rates of hydraulic cements, and in particular Portland clinker products, magnesia and lime are affected by the temperature and conditions of calcining as well as the particle porosity, texture and size and the porosity, texture and size of interspersed components such as pozzolans including fly ash and can therefore be engineered to match mainly by varying slaking temperatures and grind sizes.
  • volume changes are approximately neutral to prevent structural defects occurring during setting and volume changes are related to reactivity.
  • composition of the present invention It is desirable with the composition of the present invention to maintain a moist environment particularly after the first few hours curing and it has been determined that approximately neutral volume changes result if this is the case, resulting in little or no stresses that have to be accommodated.
  • brucite is formed which is highly insoluble (Ksp 1.8 ⁇ 10 ⁇ 11 , equivalent to 0.18 g/litre) and it blocks off access to water for farther hydration.
  • Pozzolans including natural pozzolans and artificial pozzolans such as fly ash and other wastes also react with alkalis including reactive magnesia and the free lime component included in Portland cement clinker products and formed as a result of the hydration of calcium silicates to produce more calcium silicate hydrates that further bond the components of the cement together.
  • the free lime in the cements contemplated by this invention containing pozzolans is replaced by brucite which has a similar reduction and oxidation potential but much lower solubility.
  • Inter particle surface interaction also results in chemical as well as physical bonding between fine grains of pozzolan and other cementitious components and between the pozzolan grains themselves. This is mainly due to hydration reactions but also surface hydrolysis and geopolymeric reactions particularly if an alkali such as provided by the more soluble portlandite phase (Portlandite or calcium carbonate has a Ksp of 5.5 ⁇ 10 ⁇ 6 or solubility of 1.37 g/litre) of Portland cement is present or separately added.
  • an alkali such as provided by the more soluble portlandite phase (Portlandite or calcium carbonate has a Ksp of 5.5 ⁇ 10 ⁇ 6 or solubility of 1.37 g/litre) of Portland cement is present or separately added.
  • the grains of pozzolan also provide nucleation sites for the hydration of other components of the cement.
  • pozzolan which has been defined includes materials containing silicon and aluminium that react with or are activated by an alkali, and in the presence of water form stable silicon and aluminium compounds.
  • Wastes which are pozzolans and which contribute to strength given the longer term or shorter periods if accelerated by accelerators also described or by heating preferably in a moist environment are wastes produced by the agriculture and mining industry in increasing amounts such as reactive fly ash, flue wastes, slags including iron ore slag, and other wastes from the metal production industry as well as silica fine, ground brick, and sewerage sludge ash.
  • Passive wastes take no chemical part in the formation of a cement and include, sawdust, unburnt rice husks, some mine tailings, mineral extraction wastes etc. and virtually all may be used as fillers. A high proportion can be added without loss in strength and add to abrasion resistance (and in many cases workability). If fine enough they act as micro aggregates and often result in greater strength.
  • fly ash is economically the most important and has been found to make a slightly better cement when combined with magnesia than ground vitrified iron ore slag and the reasons for this could be that the heat treatment has been more appropriate and the silicon alumina ratio is closer to ideal proportions.
  • red mud contains soluble sodium compounds, particularly sodium carbonate, sodium sulfate is produced and could be effectively recovered.
  • the carbonates remain as siderite, or alternatively combine with the magnesium forming magnesite and hydromagnesite.
  • Bauxite may also be used as a source of alumina depending on the alumina content of the primary waste and is available in large quantities at low cost.
  • Bauxite consists mainly of gibbsite (Al 2 O 3 .3H 2 O), boehmite (Al 2 O 3 .H 2 O), and diaspore. Diaspore has the same composition as boehmite but is denser and harder.
  • Sewerage sludge ash besides being a source of reactive silica and alumina and therefore a pozzolan, is a rich source of soluble phosphates.
  • the phosphates react readily with magnesia forming mostly stable insoluble phosphates which have good binding properties.
  • the residue from burning organic wastes such as rice husks is also reactive and may contain ideal quantities of silica and alumina.
  • Reactive magnesia added during the final stages of manufacture of other cements such as calcium aluminate cements, slag cements, and geopolymeric cements etc. can also be an advantage.
  • Alkaline chemicals that accelerate the setting of Portland cement include chemicals such as alkali and alkali earth hydroxides, carbonates, formates, aluminates and silicates.
  • alkaline accelerants work with the composition of the present invention. If Portland cement is included in the blend they aid the formation not only of calcium aluminates but also of calcium silicates by mobilising silica and alumina, both of which are much more soluble in an alkaline environment.
  • Another group of accelerants are acids and in particular soluble salts of acids and generally both the cation and anion contribute to the overall affect facilitating the dissolution of magnesia and lime. Although early setting is accelerated long term strength is generally reduced.
  • anions that cause significant acceleration with Portland cements are halides, nitrates, nitrites, formates, thiosulfates and thiocyanates. Their activity also appears to depend on the associated cation and research has shown that with Portland cement divalent and trivalent cations such as calcium, magnesium, barium and aluminium appear to be more affective than monovalent ions such as sodium, potassium and ammonium.
  • acidic accelerants not mentioned by the above authors include sulfates such as ferrous sulfate and calcium or aluminium sulfate.
  • accelerators that are salts of acids such as ferrous sulfate.
  • initial setting may be accelerated, but the addition of too much does not contribute to longer term hardening and can be deleterious.
  • Iron salts including sulfates and chlorides and in particular ferrous sulfate are the most recommended accelerants because of cost and environmental benefits as many of them are wastes.
  • reactive magnesia can be blended with a range of hydraulic and chemical cements and iron salts can also be used in many such blends including the commercially more important blends with ground Portland clinker minerals discussed.
  • the quantity added should be kept as low as possible to achieve the required initial set. Iron salts do not appear to contribute to final strength, and if too much is added this may even be reduced.
  • Ferrous sulfate is recommended in most instances because it is less aggressive than ferric sulfate or ferrous or ferric chloride for instance and also cheaper.
  • a small percentage (0.5-20% of the MgO content) of ferrous sulfate is effective in accelerating the initial setting of cements made using a proportion of added reactive magnesium oxide and in particular with blends of such cements with pozzolans including pozzolanic wastes such as fly ash. The amount added depends on a number of factors including the reactivity of the magnesia and other components of the cement.
  • a major advantage of using iron salts and in particular ferrous sulfate as accelerants is the low cost of the salts.
  • Ferrous sulfate is also not anywhere near as hygroscopic as either magnesium sulfate or magnesium chloride used in the manufacture of Sorel cements and in a dry atmosphere it can be ground to a fine size enabling the economical production of “all in the bag” mixes.
  • the amount and type of iron salt added is determined by trial and error as the reactions in the case of pure magnesia depend on the reactivity of the magnesia, particle size etc. and if pozzolans including wastes such as fly ash are also added, are heavily masked. Other blended wastes may also have a masking affect and more or less quantity or more or less aggressive iron salts may need to be used depending on the nature of the waste, be it fly ash, sewerage ash, rice husks etc all of which vary in reactivity. As the reaction of magnesia with iron salts is exothermic, and can get too warm if too much iron salt is added, care needs to be taken. Whether or not steam or autoclaving is also used needs to be considered as reaction rates roughly double with every 10 deg. rise in temperature, whereas increases in pressure do not have quite such a marked affect.
  • ferrous sulphate as an accelerator rather than accelerators such as sodium or potassium sulfates is that iron compounds are generally less soluble than some of the sodium or potassium compounds that form in reactions with unknown components of various wastes and pozzolans with which they may react. The possibility of efflorescence is thus reduced.
  • a simple experiment illustrates the affect of the addition of small amounts of ferrous sulfate to a cement made with magnesia and fly ash.
  • Several samples were compared for strength over a period. Each sample was made with 50% fly ash and the balance was reactive (citric acid test 22 seconds) magnesia ground to 95% less than 45 micron and 100% loss than 125 micron with ferrous sulfate at ratios given in the table.
  • the graph below shows strength on the vertical axis determined on an apparatus for measuring comparative compressive and shear strength on an arbitrary linear scale. (The scale is arbitrary in that it has not been equated to standard test units. The results produced by the apparatus are however very consistent and thus can be used for comparison purposes.)
  • the horizontal axis is time.
  • the cementitious minerals forming in the above example include brucite, ferro brucite, amakinite, iron oxysulfate, magnesium (iron) oxysulfate (see below) haematite and magnetite and near the surface, where access to CO2 is possible, hydromagnesite and magnesite and a magnesium hydroxy sulpho carbonate. Ultimately silicates and aluminates, and their hydrates form very slowly.
  • Brucite is the main cementing phase and the structure consists of layers of hydroxyls with magnesium in between. Fe ++ also substitutes for Mg ++ in brucite and may increase the strength. A fine dispersion of magnetite (Fe 3 O 4 ) also often occurs in the structure, possibly also adding to strength.
  • a pozzolan such as fly ash or an alternative source of reactive silica and alumina is added to cements containing reactive magnesia the pozzolan reacts in a number of ways previously discussed including reacting with any free lime producing more calcium silicate hydrates if free lime is present such as caused by the addition of Portland clinker as well as surface hydrolysis and geopolymeric reactions occurring.
  • Soluble silicates and aluminates can also be added to advantage encouraging the formation of silicate and aluminate minerals but cost will generally rule out the use of these materials.
  • compositions of the present invention are that they able to accommodate a wide variety of extraneous cations and anions. Many of these extraneous cations and anions are thought to find their way into the open layered structure of brucite, where if the are toxic, they are rendered inert as long as the brucite does not dissolve.
  • compositions of the present invention are generally not attacked by soft waters. Surface protection by carbonates ensues with most acid rains.
  • the high reactive magnesia cement compositions described are also very resistant to sea and ground water attack and this is thought to be because brucite, the main component, is virtually insoluble at the pH of sea water (8.2) and in most ground waters and does not suffer ion replacement or decomposition in the same manner as the calcium silicate hydrate found in Portland cement as portlandite is replaced or leached out.
  • Tests have confirmed resistance to agents such as glaubers salts, epsom salts, sodium chloride, ammonium nitrate and week organic acids.
  • Neosyn EA is a sodium salt of naphthalene sulphonic acid polymer with formaldehyde. These appear to work in a manner similar to Portland cement affecting surface charge however in most situations they do not seem to be needed.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Curing Cements, Concrete, And Artificial Stone (AREA)
  • Soil Conditioners And Soil-Stabilizing Materials (AREA)
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  • Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
US10/181,442 2000-01-27 2001-01-29 Reactive magnesium oxide cements Abandoned US20030041785A1 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
US11/016,722 US7347896B2 (en) 2000-01-27 2004-12-21 Reactive magnesium oxide cements

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
AUPQ5271 2000-01-27
AUPQ5271A AUPQ527100A0 (en) 2000-01-27 2000-01-27 A strategy for producing magnesium based eco-cements
AUPQ7181A AUPQ718100A0 (en) 2000-05-01 2000-05-01 Sustainable eco-cement technologies for the new millenium
AUPQ7181 2000-05-01

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