WO2009136169A1 - Composition de ciment contenant de la magnésie - Google Patents

Composition de ciment contenant de la magnésie Download PDF

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Publication number
WO2009136169A1
WO2009136169A1 PCT/GB2009/001152 GB2009001152W WO2009136169A1 WO 2009136169 A1 WO2009136169 A1 WO 2009136169A1 GB 2009001152 W GB2009001152 W GB 2009001152W WO 2009136169 A1 WO2009136169 A1 WO 2009136169A1
Authority
WO
WIPO (PCT)
Prior art keywords
akermanite
gehlenite
mgsi
present
sio
Prior art date
Application number
PCT/GB2009/001152
Other languages
English (en)
Inventor
Gary Hunt
Original Assignee
Cenin Limited
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Cenin Limited filed Critical Cenin Limited
Publication of WO2009136169A1 publication Critical patent/WO2009136169A1/fr

Links

Classifications

    • 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
    • C04B28/08—Slag 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
    • C04B28/04—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
    • C04B28/08—Slag cements
    • C04B28/082—Steelmaking slags; Converter slags
    • 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
    • C04B7/00—Hydraulic cements
    • C04B7/14—Cements containing slag
    • C04B7/147—Metallurgical slag
    • C04B7/153—Mixtures thereof with other inorganic cementitious materials or other activators
    • C04B7/17—Mixtures thereof with other inorganic cementitious materials or other activators with calcium oxide containing activators
    • 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
    • C04B7/00—Hydraulic cements
    • C04B7/14—Cements containing slag
    • C04B7/147—Metallurgical slag
    • C04B7/153—Mixtures thereof with other inorganic cementitious materials or other activators
    • C04B7/17—Mixtures thereof with other inorganic cementitious materials or other activators with calcium oxide containing activators
    • C04B7/19—Portland cements
    • 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

  • the present invention relates to a method of controlling the strength development and/or setting times of cement, mortar and concrete and/or concrete products produced by such a method.
  • cement we mean hydrated cementitious material
  • mortar we mean a hydrated mixture of cementitious material and sand
  • concrete we mean a hydrated mixture of cementitious material, sand and a coarser aggregate.
  • Portland cement as a cementitious material, is well established and widely used in industry. Portland cement provides a strong and durable component in concrete/mortar.
  • PC The main constituents of PC include Portland cement clinker (a hydraulic material which consists of two-thirds by weight calcium silicates ((CaO) 3 SiO 2 (CaO) 2 SiO 2 ), the remainder being calcium aluminates (CaO 3 Al 2 O 3 ) and calcium ferro-aluminate (CaO 4 Al 2 O 3 Fe 2 O 3 (and other oxides), and minor additional constituents. Minor constituents of up to 5 % can be added and the cement is still classed as PC. After the addition of materials such as Ground Granulated Blast Furnace Slag (GGBS), Pulverised Fuel Ash (PFA) etc, the resultant cement is classed as a composite cement.
  • GGBS Ground Granulated Blast Furnace Slag
  • PFA Pulverised Fuel Ash
  • PC has the disadvantage that its production is a high energy intensive process that creates significant environmental damage due to the high level of carbon dioxide produced. Furthermore, PC has a further disadvantage of being the most expensive component of concrete and mortar. Industrial wastes and raw materials are, in general considered to be an increasingly serious environmental problem. At present, many of these raw materials are dumped to landfill. Some of these industrial waste and by-products contain elements that are common to those found in cements and cement replacements.
  • GGBS a significant constituent of composite cements, as mentioned above, is an example of a raw material which is recycled rather than being dumped to landfill.
  • WBFS Weathered Blast Furnace Slag
  • MgO magnesium oxide
  • the present invention seeks to address the problems of the prior art.
  • a first aspect of the present invention comprises a method of controlling the strength development of cement, mortar or concrete comprising varying the amount of Ca 2 MgSi 2 O 7 (akermanite) and Ca 2 Al 2 SiO 7 (gehlenite) present in dependence upon the desired strength characteristics of the cement, mortar or concrete.
  • a further aspect of the present invention is a method of controlling the setting time of cement, mortar or concrete comprising varying the amount of Ca 2 MgSi 2 O 7 (akermanite) and Ca 2 Al 2 SiO 7 (gehlenite) present in dependence upon the desired setting time.
  • Akermanite and gehlenite are preferably present in the cementitious material prior to hydration. However, akermanite and/or gehlenite may also be formed during the hydration process if sufficient free lime and free magnesium oxide present or released from the hydrating materials. In addition, Silica must be present to allow akermanite and/or gehlenite to form during the hydration process.
  • the combined amount of Ca 2 MgSi 2 O 7 (akermanite) and Ca 2 Al 2 SiO 7 (gehlenite) present in the concrete is up to around 20% by weight.
  • Ca 2 MgSi 2 O 7 (akermanite) and Ca 2 Al 2 SiO 7 (gehlenite) are present in the concrete in an amount of up to around 15% by weight.
  • Ca 2 MgSi 2 O 7 (akermanite) and Ca 2 Al 2 SiO 7 (gehlenite) are present in the concrete an amount in range of around 8 to 12 % by weight. It will be appreciated that it is the combined amounts of akermanite and gehlenite that are being referred to.
  • the Ca 2 MgSi 2 O 7 (akermanite) and Ca 2 Al 2 SiO 7 (gehlenite) are derived at least in part from WBFS.
  • WBFS When WBFS is present in the cementitious material, WBFS undergoes a chemical reaction on hydration in the presence of free lime and calcium silicates to produce and increased total amount of Ca 2 MgSi 2 O 7
  • Finding a commercial use for WBFS is particularly advantageous as it is available in abundance, and provides a useful way to recycle the waste by-product of another industrial process.
  • Ca 2 MgSi 2 O 7 (akermanite) and Ca 2 Al 2 SiO 7 (gehlenite) are from the melilite group of compounds and is typically found in dolomite and limestone rocks, and is also found in iron and steel slags such as, but not limited to, WBFS.
  • Ca 2 MgSi 2 O 7 (akermanite) and Ca 2 Al 2 SiO 7 (gehlenite) are not present in GGBS.
  • the calcium and silica phases are well known and commonplace in composite PC cements and other composite cements.
  • the total combined level of Ca 2 MgSi 2 O 7 (akermanite) and Ca 2 Al 2 SiO 7 (gehlenite) may be varied in dependence upon the amount of WBFS present in the cementitious composition at the time of hydration.
  • the method further comprises providing a source of MgO.
  • a source of MgO By adding additional MgO to the cementitious composition prior to hydration, more Ca 2 MgSi 2 O 7 (akermanite) and Ca 2 Al 2 SiO 7 (gehlenite) are produced during the hydration step in the presence of free lime and calcium silicate.
  • MgO is present in the concrete in an amount in the range of around 3 to 7 % by weight.
  • the MgO is derived at least in part from WBFS, which typically contains MgO in an amount of around 8 to 12% by weight.
  • WBFS typically contains MgO in an amount of around 8 to 12% by weight.
  • the amount of MgO could be greater depending on the source of slag as the composition can vary between countries and steel and iron plants.
  • the MgO which combines with the calcium and silica phases of the WBFS is derived at least in part from paper ash.
  • paper ash Many types of paper ash contain akermanite and free lime, and the inclusion of such paper ash as a component in the cementitious composition prior to hydration assists in the formation of Ca 2 MgSi 2 O 7 (akermanite) and Ca 2 Al 2 SiO 7 (gehlenite) post hydration.
  • the hydration of the cementitious composition is carried out substantially in the absence of granulated slag.
  • the method of the present invention may further comprise providing a source of free CaO.
  • the method of the present invention may further comprise providing a source of free calcium silicates.
  • a further aspect of the present invention provides a cement, mortar or concrete composition
  • a cement, mortar or concrete composition comprising Ca 2 MgSi 2 O 7 (akermanite) and Ca 2 Al 2 SiO 7 (gehlenite).
  • concrete containing the Ca 2 MgSi 2 O 7 (akermanite) and Ca 2 Al 2 SiO 7 (gehlenite) is produced using a method in accordance with a first aspect of the present invention.
  • Ca 2 MgSi 2 O 7 (akermanite) and Ca 2 Al 2 SiO 7 (gehlenite) are present in the cement, mortar or concrete in a combined total amount of up to 15 %.
  • Ca 2 MgSi 2 O 7 (akermanite) and Ca 2 Al 2 SiO 7 (gehlenite) are present in a combined total amount in the range of around 8 to 12
  • a further aspect of the present invention provides a mortar composition
  • a mortar composition comprising
  • Ca 2 MgSi 2 O 7 (akermanite) and Ca 2 Al 2 SiO 7 (gehlenite).
  • mortar containing the Ca 2 MgSi 2 O 7 (akermanite) and Ca 2 Al 2 SiO 7 (gehlenite) is produced using a method in accordance with a first aspect of the present invention. It is preferred that the Ca 2 MgSi 2 O 7 (akermanite) and Ca 2 Al 2 SiO 7 (gehlenite) are present in the mortar in a combined total amount of up to 15 %. However, more preferably Ca 2 MgSi 2 O 7 (akermanite) and Ca 2 Al 2 SiO 7 (gehlenite) are present in the concrete in a combined total amount in the range of around 8 to 12 %.
  • a further aspect of the present invention provides a cementitious composition comprising WBFS and optionally an additional source of MgO.
  • MgO may be added directly, or MgO may be provided by including paper ash or any other suitable source of MgO in the cementitious composition.
  • a further aspect of the present invention provides a cementitious composition comprising a hydrated blend of paper ash and weathered blast furnace slag.
  • Figure 1 is a graph illustrating mortar strength development over 28 days with 12 % by total weight of akermanite and gehlenite present;
  • Figure 2 is a graph illustrating mortar strength development over 28 days with 15 % by total weight of akermanite and gehlenite present;
  • Figure 3 is a graph illustrating mortar strength development over 84 days in the presence of various amounts of MgO
  • Figure 4 is a graph illustrating mortar strength development over 84 days in the presence of different grades of MgO
  • Figure 5 is a graph illustrating the composition changes of Portland cement over a 24 hour period.
  • Figures 6 - 10 are graphs of composition changes in cement pastes:
  • Figure 6 is a graph illustrating the composition changes of a standard cement composition for a composite blend formed from Portland cement and GGBS;
  • Figure 7 is a graph illustrating the composition changes of a standard cement composition for RMl, a composite blend formed from Portland cement and Cenin;
  • Figure 8 is a graph illustrating the composition changes of a standard cement composition for RM3, a composite blend formed from Portland cement and Cenin
  • Figure 9 is a graph illustrating the composition changes of a standard cement composition for BLl (Blend 1), a composite blend formed from Portland cement and Cenin Grade 2 with a ratio of 70% paper ash: 30% WBFS;
  • Figure 10 is a graph illustrating the composition changes of a standard cement composition for BL2 (Blend 2), a composite blend formed from Portland cement and Cenin Grade 2 with a ratio of 30% paper ash: 70% WBFS;
  • Figure 11 is a graph illustrating the heat of hydration for PC (C3), GGBS (C7), BIl (Blend 1) and B12 (Blend 2);
  • Figure 12 is a graph illustrating the initial setting times for PC (C3), GGBS (Cl), BIl (Blend 1) and B12 (Blend 2);
  • Figure 13 is a table and graphs illustrating the composition changes of the blend '30% SDP and 70% C3' over time;
  • Figure 14 is a table and graphs illustrating the composition changes of the blend '30% WCP and 70% C3' over time;
  • Figure 15 is a table and graphs illustrating the composition changes of the blend '30% PFA and 70% C3 ' over time.
  • Figure 16 is a table and graphs illustrating the composition changes of the blend '30% C7 and 70% C3' over time.
  • Waste paper-ash comes from combined heat and power (CHP) systems and so is already dry prior to being milled. WBFS is heated to remove surface moisture prior to the milling process.
  • CHP combined heat and power
  • WBFS and waste paper-ash are then milled to less than 75 ⁇ m (and preferably less than 40 ⁇ m).
  • the milling of each component is typically carried out separately. However, it is envisaged that the two components could be combined prior to milling and the two components milled together to increase the efficiency of the milling process.
  • the two components are then in a condition to be blended with any selected additional components to be included in the cementitious material prior to hydration, such components to include magnesium, calcium and silica oxides or materials containing them.
  • the additional components may also be added prior to milling.
  • the main components that form during the hydration process are listed below. These compounds are mainly formed during the first 24 hours after initiation of hydration, with further changes in the property of the cement observable over time.
  • the C3S is present in a high percentage and the Calcite is present in a low percentage. However, this rapidly changes as the C3S is changed to Calcite.
  • Paper ash is a waste product from the paper industry and comprises burned sludge optionally with wood and/or plastics.
  • RMl, RM6 & RM13 are different sources of paper ash.
  • RMl is a mixture of paper and wood with a free lime content of around 7%.
  • RM6 is a mixture of paper ash and plastics with both free lime and high chloride present.
  • RM13 is paper sludge and has a free lime content of around 30%. Chloride is present in all materials with RM 6 having a particularly high chloride content.
  • Blend 1 is a composite blend of Portland cement and Cenin Grade 2 with a 70%:30% ratio of paper ash:weathered slag.
  • Blend 2 is a composite Portland Cement and Cenin Grade 2 with 30% paper ash:70% WBFS.
  • B12 has akermanite and gehlenite in the blend in a total combined amount of 15 % by weight.
  • the strength development of the mortar was tested over a period of 28 days.
  • the akermanite and gehlenite level is manipulated by changing the ratio between the paper ash and the WBFS. It can also be manipulated by adding free MgO and/or free CaO.
  • Blend R23A was prepared including MgO at various replacement levels i.e. 5%, 10%, 15% and 25%, and the compressive strength of mortar prepared from the blends measure over 84 days from hydration.
  • RM23A is derived from a dolomitic limestone quarry and therefore contains a higher level of MgO than the other samples mentioned previously.
  • the compressive strength of concrete prepared using conventional Portland cement was also measured over 84 days as a control.
  • the compressive strength of the mortar is tested by producing mortar prisms and testing to European standard EN: 196
  • the replacement level of MgO in the blend is increased this appears to be detrimental to the strength development of the mortar.
  • the mortar is mixed with aggregate to produce concrete and the compressive strength of the concrete tested over time, the concrete is observed to be marginally stronger than comparable mortar under experimental conditions.
  • the observed concrete strength can be influenced at least in part by the type and shape of the aggregate used.
  • Various blends (RM23A, RM23B, RM23C, RM23D, RM23E and RM23F) were prepared using various grades of MgO.
  • the MgO in RM23A was prepared from Dolomite and sea water.
  • the MgO in the remaining blends was prepared from limestone and sea water.
  • the various blends used vary in production time and cost as shown below:
  • the compressive strength of mortar produced using each of the blends mentioned above was measured over a period of 84 days.
  • the mortar composition includes 95% PC and 5% MgO.
  • the compounds akermanite and gehlenite can be found in both weathered slag and paper ash (although there is significantly more akermanite and gehlenite present in weathered slag). There is also free lime present in paper ash which is not detected after the hydration process has begun. Therefore, it is likely that the free lime becomes bound with another compound, the most likely candidates being the akermanite and gehlenite.
  • Figure 5 shows the above results in line-graph form.
  • composition changes of a standard cement composition for a composite blend formed from Portland cement and GGBS A composite blend was prepared from Portland cement and C7 (the composite blend having a 75:25% ratio of PGGGBS) and the levels of various components monitored over a period of 24 hours following initiation of hydration. The results are shown below:
  • Figure 6 shows the above results in line-graph form.
  • a composite blend was prepared from Portland cement and RMl (the composite blend having a 75:25% ratio of PQRMl) and the levels of various components monitored over a period of 24 hours following initiation of hydration. The results are shown below:
  • a composite blend was prepared from Portland cement and RM3 (the composite blend having a 75:25% ratio of PC:RM3) and the levels of various components monitored over a period of 24 hours following initiation of hydration. The results are shown below:
  • Figure 8 shows the above results in line-graph form.
  • a composite blend was prepared from Portland cement and BIl (the composite blend having a 75:25% ratio of PC:B1.
  • BU has a 70:30% ratio of paper ash:weathered slag) and the levels of various components monitored over a period of 24 hours following initiation of hydration. The results are shown below: Table 7:
  • Figure 9 shows the above results in line-graph form. It is clear from the graph that the C3 and C2 phases are similar to that of Portland cement except that the calcite is present in a reduced amount and arcanite, akermanite and gehlenite are now present.
  • a composite blend was prepared from Portland cement and B12 (the composite blend having a 75:25% ratio of PC:B12. B12 having a 70:30% ratio of weathered slag:paper ash) and the levels of various components monitored over a period of 24 hours following initiation of hydration. The results are shown below:
  • Figure 10 shows the above results in line-graph form. From the graph it can be seen that the C3 and C2 phases are much close and the level of arcanite is similar to a PC/GGBS composite. However, the combined level of akermanite and gehlenite is higher.
  • Blend 1 (BIl) has the best strength development and therefore Blend 1 has the most desirable composition.
  • Graph 11 shows the heat of hydration that occurs during hydration of C3 (PC), C7 (GGBS), BIl (Blend 1) and B12 (Blend 2).
  • BU - BIl has a 70:30% ratio of paper ash:weathered slag
  • B12 - has a 70:30% ratio of weathered slag:paper ash
  • Graph 12 shows the initial settings times of the samples BIl composite blend, B12 composite blend, C3 composite blend and Cl composite blend and it is clear that the setting times of BU composite blend and B12 composite blend are significantly lower than those of C3 and Cl composite blend.
  • blend 3 (30% PFA and 70% CS) it is shown that arcanite is present in PFA in very limited quantities and decreases over time.
  • blend 4 (30% C7 and 70% C3) some variation can be seen over time in the amount of arcanite present, however, the levels of akermanite and gehlenite do not vary as dramatically as observed with blend 2.

Abstract

La présente invention concerne un procédé de contrôle du développement de la résistance et du temps de durcissement de ciment, de mortier ou de béton qui consiste à faire varier la quantité combinée totale de Ca2MgSi2O7 (akermanite) et de Ca2Al2SiO7 (gehlénite) présente en fonction des caractéristiques de résistance et/ou des temps de durcissement souhaités.
PCT/GB2009/001152 2008-05-07 2009-05-07 Composition de ciment contenant de la magnésie WO2009136169A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
GB0808296A GB0808296D0 (en) 2008-05-07 2008-05-07 Low carbon cement composition
GB0808296.8 2008-05-07

Publications (1)

Publication Number Publication Date
WO2009136169A1 true WO2009136169A1 (fr) 2009-11-12

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WO (1) WO2009136169A1 (fr)

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CN113135754A (zh) * 2021-04-29 2021-07-20 安徽工业大学 一种制备具有压电性能的胶凝复合材料的方法、胶凝复合材料及其应用

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JP6102428B2 (ja) * 2013-03-29 2017-03-29 住友大阪セメント株式会社 水硬性組成物

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113135754A (zh) * 2021-04-29 2021-07-20 安徽工业大学 一种制备具有压电性能的胶凝复合材料的方法、胶凝复合材料及其应用
CN113135754B (zh) * 2021-04-29 2022-06-03 安徽工业大学 一种制备具有压电性能的胶凝复合材料的方法、胶凝复合材料及其应用

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GB0907909D0 (en) 2009-06-24
GB0808296D0 (en) 2008-06-11

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