WO2017109583A2 - Compositions de ciment, de mortier et de béton à base de phosphate de magnésium à temps d'utilisation accru - Google Patents

Compositions de ciment, de mortier et de béton à base de phosphate de magnésium à temps d'utilisation accru Download PDF

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Publication number
WO2017109583A2
WO2017109583A2 PCT/IB2016/002007 IB2016002007W WO2017109583A2 WO 2017109583 A2 WO2017109583 A2 WO 2017109583A2 IB 2016002007 W IB2016002007 W IB 2016002007W WO 2017109583 A2 WO2017109583 A2 WO 2017109583A2
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WO
WIPO (PCT)
Prior art keywords
composition according
cement composition
phosphate
present
weight
Prior art date
Application number
PCT/IB2016/002007
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English (en)
Other versions
WO2017109583A3 (fr
Inventor
Ramkumar Natarajan
Satheesh Kumar Kartheesan Thiyagarajan
Original Assignee
Eko Tech4Trans Pvt. Ltd.
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.)
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Publication date
Application filed by Eko Tech4Trans Pvt. Ltd. filed Critical Eko Tech4Trans Pvt. Ltd.
Publication of WO2017109583A2 publication Critical patent/WO2017109583A2/fr
Publication of WO2017109583A3 publication Critical patent/WO2017109583A3/fr

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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
    • C04B28/34—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 cold phosphate binders
    • 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 is directed to a fast setting cement, more specifically a phosphate-based cement using a source of low purity metal oxide, a phosphate component, a retarder, sufficient water and, optionally, calcium oxide containing material having substantially high amount of amorphous glass content.
  • US patent No. 6, 136,088 discloses a high early strength binder based on phosphate cement utilizing a maximum binder level of 58%, which avoids the evolution of ammonia gas in its preparation by reacting mono ammonium phosphate with potassium carbonate and a process for preparing a cementitious binder useful in a quick setting mortar, whose utility includes a repair material for cementitious structures.
  • the binding system is based on the formation of potassium struvite, by reacting a source of high purity magnesium oxide with potassium phosphate and water. Although still quick setting, the set time of this binder is slower than the set time of struvite.
  • 7,001 ,860 discloses an inexpensive construction material, adapted for use in warm weather climates where Styrofoam or other synthetic organic resin foams are used as construction materials and require a coating of a hard, dense material for a surface finish and a method to coat Styrofoam structures with a material which cures or sets at room temperature and is easy to apply in the field.
  • US patent No. 7,204,880 discloses a cement formula utilizing the metal oxide along with mono potassium phosphate and mono ammonium phosphate but uses a very small amount of it because of the use of high purity metal oxide. If the percentage of mono ammonium phosphate is increased the final cement sets faster making it impractical for large area applications.
  • the present invention relates to the method of producing a structural material with an improved workability to be used in the infrastructure development.
  • the failure was attributed to the purity of magnesium oxide used. It was unexpectedly and surprisingly found that by lowering the purity of metal oxides by adding other compounds like silicate or aluminate, the loading of metal oxides can be increased and the loading of phosphates can be decreased thereby reducing the cost of the final binder and extend the working time of the cement so that it can be used for many other applications other than road repair.
  • the phosphate cement comprising a source of low purity metal oxides can also overcome the working time issue by using low purity metal oxides in combination with retarders such as an alkali metal stannate or an alkali metal fluoride or an alkali metal sulphate.
  • the water resistance is improved by the use of amorphous calcium oxide containing material.
  • the use of a high amount of low cost high solubility phosphate provides for a cost effective cement composition.
  • the mechanical properties of the cement are improved by the use of calcium oxide containing fillers having amorphous glass content.
  • the novel cement with good strength coupled with improved flowability and increased working time and mechanical properties is produced by mixing the right proportions of metal oxide or a source of low purity metal oxide, an industrial waste containing a source of silica which can include fly ash, steel slag, ground granulated blast furnace slag (GGBFS), and a phosphate component, and a retarder with a sufficient amount of water.
  • a source of silica which can include fly ash, steel slag, ground granulated blast furnace slag (GGBFS), and a phosphate component
  • GGBFS ground granulated blast furnace slag
  • a retarder with a sufficient amount of water.
  • the resulting cement does not involve clinkering.
  • a preferred embodiment of the present invention is directed to overcoming the problem of poor water resistance, increased cost and lack of working time of traditional phosphate cements which has been the main hindrance to the widespread use of such cements.
  • the setting time of the final cement depends upon the amount of metal cations released from the metal oxide to be able to react with phosphate anions when water is added to the dry cement components. If the amount of metal cations released is higher in a given period of time then the cements sets faster. If the release of the cations can be controlled, the setting can be controlled.
  • One of the ways to do it is by increasing the calcination temperature of metal oxides or the having other compounds along with the metal oxides which will lower the amount of metal oxide getting released. Examples of such compounds are silicates and aluminates, which can be represented as MgSi0 3 and MgAl 2 0 4 .
  • the non stoichiometric metal oxide silicates can be represented as MgO x Si02 (1-x) and the metal oxide aluminate can be represented as MgO x Al 2 0 3( i. x) .
  • Reactivity of magnesium oxide depends on its morphology and its chemical composition. Highly crystalline oxide is also the least soluble in the phosphate solution (the crystals are called periclase) and it is achieved by increasing the temperature of calcination. Due to the low solubility of these crystals, the mixing and application time of the resulting cement is expected to be longer than that without this crystal morphology.
  • this lower purity (thus, less reactive) magnesium oxide or magnesium silicate it may be then possible to reduce the content of the phosphate by increasing the content of this magnesium oxide. By reducing the content of the phosphate in the total binder the cost of the cement is consequently reduced as the former is a high cost component in the binder.
  • the binder here is referred as the combination of metal oxide or metal silicate, metal aluminate and the phosphate component.
  • the cement forming reaction between 100% magnesium oxide and mono potassium phosphate can be expressed as: MgO + KH 2 P0 4 + 5H 2 0 -» Mg P0 4 .6H 2 0 ( 1 )
  • the molecular weight ratio of metal oxide: phosphate would ideally have to be 40 grams: 136 grams (1 : 3.2). This ratio not only makes the price of the binder high but also results in a quick setting composition. In an effort to reduce the price of the binder, a slight increase (of as little as 10%) in the high purity metal oxide weight releases more cations in the mix which renders the cement fast setting, hence unsuitable for certain practical applications.
  • the cement forming reaction when using a low purity metal oxide with silicate may be written as:
  • Magnesium potassium phosphate the final product formed due to the chemical reaction between magnesium oxide and mono potassium phosphate has a solubility product constant of 24X10 " " and gets converted into Mg 3 (P04) 2 when immersed in water for a prolonged period of time accompanied by a drop in the mechanical properties making it unusable in areas where prolonged water immersion is expected. It was found after an extensive period of testing with various fillers along with binder (magnesium silicate + phosphate component) that by having a suitable magnesium oxide/silicate : phosphate component ratio, the water resistance of these phosphate cements is greatly increased.
  • a preferred embodiment of the present invention comprises a source of low purity metal oxide ( ⁇ 85% purity) or similar material such as magnesium silicate or magnesium aluminate.
  • This source of low purity metal oxide is preferably present in the range of 20-55% by weight of the total composition.
  • This source of low purity metal oxide is more preferably present in the range of 25-45%).
  • This source of low purity metal oxide is even more preferably present in the range of 30-40%.
  • the preferred form of metal oxide is magnesium oxide.
  • the phosphate component is selected from the group consisting of: a low solubility acid phosphate; a high solubility acid phosphate, and combinations thereof.
  • the low solubility acid phosphate (such as mono potassium phosphate) is preferably present in an amount ranging from 1 to 45% by weight of the total composition; and when present, the high solubility acid phosphate (such as mono ammonium phosphate) is preferably present in an amount ranging from 1 to 20% by weight of the total composition, more preferably from 1 to 15% and even more preferably from 1 to 5%.
  • the total content of phosphate component will range of 20-55% by weight of the total composition. More preferably, the phosphate component is present in the range of 25-45%. Even more preferably, the phosphate component is present in the range of 30-40%.
  • material containing calcium oxide in the range of 1 -50% and having high amorphous glass content includes materials selected from the group consisting of: fly ash, ground granulated blast furnace slag and steel slag. More preferred is fly ash. When present, such material is preferably present in an amount ranging from 15 to 45% by weight of the total composition. More preferably, this material is present from 15 to 25 % by weight of the total composition.
  • the ratio of MgO: phosphate component should range between 0.6: 1 to 1 .5: 1.
  • fibers are added to the cement composition in order to increase the flexural strength of the resulting cement.
  • the fibers are selected from the group consisting of: glass fibers (preferably 3mm long); polypropylene fibers; and basalt fibers. Most preferred are glass fibers.
  • Pigments such as titanium dioxide can be added to impart a white tone to the cement. Typically, the presence of pigments ranges from 1 to 5% but can be reasonably adjusted to more or less than this range in order to obtain the desired color or tone while substantially maintaining the physical characteristics required of the cement.
  • retarders are generally used.
  • retarders are selected from the group consisting of: alkali metal fluoride; alkali metal stannate; borax and combinations thereof. More preferably, an alkali metal fluoride such as sodium fluoride is used. In another preferred embodiment, an alkali metal stannate such as sodium stannate is used.
  • the alkali metal fluoride such as sodium fluoride is preferably present in an amount ranging from 0.1 to 10 % by weight of the total composition, more preferably from 1 to 5%.
  • the alkali metal stannate such as sodium stannate is preferably present in an amount ranging from 0.1 to 10 % and more preferably from 1 to 5% by weight of the total composition.
  • borax is preferably present in an amount ranging from 0.1 to 10 % and more preferably from 1 to 5% by weight of the total composition.
  • the amount of water used in the cement composition should generally be half the amount of binder.
  • the person of ordinary skill in the art will know that the amount of water can be varied within a reasonable range to optimize the cement performance (setting time and strength) without departing from the scope of the present invention.
  • the working time of the cement according to a preferred embodiment of the present invention will be ten minutes or more.
  • the cements according to the present invention can be used to make concretes by the addition of various types of aggregates commonly used in the field. These include fine granular sand such as quartz sand (of 3mm size) as well as rock aggregates (such as 20mm stones).
  • cements according to the present invention can be used to make mortars by the addition of various types of fine granular material such as sand commonly used in the field.
  • fine granular material such as sand commonly used in the field.
  • the purposes disclosed herein are understood to be examples of the breadth of use the present invention can be applied and should not be construed to be limited to such.
  • the initial setting time was of 3 minutes and the final setting time was 5 minutes.
  • the cement hardness was monitored and recorded over a range of time of up to 4 weeks. The results of the hardness testing for Example 6 are listed below:
  • the initial setting time was of 20 minutes and the final setting time was 30 minutes.
  • the cement hardness was monitored and recorded over a range of time of up to 4 weeks. The results of the hardness testing for Example 7 are listed below:
  • the preparation process involved the mixing of all the powder components including sand followed by the addition of water and the wet mixture was then mixed with a mixer.

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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)

Abstract

Cette invention concerne une composition de ciment à base de phosphate, comprenant : une source d'oxyde métallique de faible pureté, un composant de phosphate, éventuellement, un retardateur, une quantité suffisante d'eau et, éventuellement, un matériau contenant de l'oxyde de calcium présentant une teneur en verre amorphe sensiblement élevée. L'invention concerne en outre des procédés de fabrication de ladite composition.
PCT/IB2016/002007 2015-12-21 2016-12-14 Compositions de ciment, de mortier et de béton à base de phosphate de magnésium à temps d'utilisation accru WO2017109583A2 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
CA2915539 2015-12-21
CA2915539A CA2915539A1 (fr) 2015-12-21 2015-12-21 Ciment a base de phosphate de magnesium, mortier et compositions de beton offrant une periode de travail prolongee

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WO2017109583A2 true WO2017109583A2 (fr) 2017-06-29
WO2017109583A3 WO2017109583A3 (fr) 2017-08-03

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113443849A (zh) * 2021-07-28 2021-09-28 喜跃发国际环保新材料股份有限公司 一种磷酸镁水泥用缓凝剂及其使用方法
CN115448687A (zh) * 2022-10-18 2022-12-09 中铁第四勘察设计院集团有限公司 一种磷酸铵镁水泥基复合材料及其制备方法和应用

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108975751B (zh) * 2018-09-27 2021-04-09 辽宁科大中驰镁建材科技有限公司 一种混凝土用外加剂、制备及应用

Family Cites Families (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4758278A (en) * 1986-11-28 1988-07-19 E. I. Du Pont De Nemours And Company Magnesium oxide powder for workable, rapid-setting phosphate-containing cement compositions
US20020009622A1 (en) * 1999-08-03 2002-01-24 Goodson David M. Sprayable phosphate cementitious coatings and a method and apparatus for the production thereof
JP4562929B2 (ja) * 2001-02-14 2010-10-13 独立行政法人農業・食品産業技術総合研究機構 セメント組成物
CA2462546A1 (fr) * 2004-03-30 2005-09-30 Michael J. Mabey Materiaux composites a base de « mousse minerale » legere et methodes pour les produire et les utiliser
US7204880B1 (en) * 2004-05-21 2007-04-17 Turner Terry A Rapid setting cement
US9815738B2 (en) * 2012-10-09 2017-11-14 Premier Magnesia, Llc Magnesium phosphate cement

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113443849A (zh) * 2021-07-28 2021-09-28 喜跃发国际环保新材料股份有限公司 一种磷酸镁水泥用缓凝剂及其使用方法
CN113443849B (zh) * 2021-07-28 2022-12-02 喜跃发国际环保新材料股份有限公司 一种磷酸镁水泥用缓凝剂及其使用方法
CN115448687A (zh) * 2022-10-18 2022-12-09 中铁第四勘察设计院集团有限公司 一种磷酸铵镁水泥基复合材料及其制备方法和应用
CN115448687B (zh) * 2022-10-18 2023-08-04 中铁第四勘察设计院集团有限公司 一种磷酸铵镁水泥基复合材料及其制备方法和应用

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WO2017109583A3 (fr) 2017-08-03
CA2915539A1 (fr) 2017-06-21

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