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WO2016032341A1 - Matériau géopolymère cimentaire à base d'aplite - Google Patents

Matériau géopolymère cimentaire à base d'aplite Download PDF

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Publication number
WO2016032341A1
WO2016032341A1 PCT/NO2015/050146 NO2015050146W WO2016032341A1 WO 2016032341 A1 WO2016032341 A1 WO 2016032341A1 NO 2015050146 W NO2015050146 W NO 2015050146W WO 2016032341 A1 WO2016032341 A1 WO 2016032341A1
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WIPO (PCT)
Prior art keywords
aplite
alkali
cementitious
range
solution
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PCT/NO2015/050146
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English (en)
Inventor
Mahmoud KHALIFEH
Helge HODNE
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Individual
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Filing date
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Publication of WO2016032341A1 publication Critical patent/WO2016032341A1/fr
Anticipated expiration legal-status Critical
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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
    • C04B28/006—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 mineral polymers, e.g. geopolymers of the Davidovits type
    • C04B28/008—Mineral polymers other than those of the Davidovits type, e.g. from a reaction mixture containing waterglass
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
    • C09K8/42—Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells
    • C09K8/46—Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells containing inorganic binders, e.g. Portland 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
    • C04B12/00—Cements not provided for in groups C04B7/00 - C04B11/00
    • C04B12/005—Geopolymer cements, e.g. reaction products of aluminosilicates with alkali metal hydroxides or silicates
    • 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
    • C04B28/006—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 mineral polymers, e.g. geopolymers of the Davidovits type
    • 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
    • C04B2111/00034—Physico-chemical characteristics of the mixtures
    • C04B2111/00146—Sprayable or pumpable mixtures
    • 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
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P40/00—Technologies relating to the processing of minerals
    • Y02P40/10—Production of cement, e.g. improving or optimising the production methods; Cement grinding
    • 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 invention concerns a cementitious aplite-based geopolymeric material.
  • cements two different types may be distinguished : “hydraulic” cements such as Portland cements, and “geopolymer” cements.
  • Portland cement Since the development of Portland cement, it has become the most common construction ingredient. Portland cement is also widespread material used in petroleum industry for sealing the annular space between casing and for zonal isolation. However, there are some drawbacks regarding chemo-physical properties of hardened Portland cement and emission of greenhouse gases in its manufacturing process.
  • Alkali-activated binders are receiving increasing attention as alternative to Portland cement due to their high enough strength, durability and low environmental impact. Unlike Portland cement, the source of alkali-activated binders can be waste-stream materials used with very limited further processing. Alkali-activated binders are developed by mixing an alkaline activator, which could be an alkaline solution or a mix of alkaline solution with alkaline silicate solution, with a source of aluminosilicate material such as fly ash, kaolin, metakaolin, blast furnace slag, etc. Concisely, the hydroxyl group (OH " ) penetrates to the original structure of aluminosilicate material and depol- ymerize the silicates.
  • an alkaline activator could be an alkaline solution or a mix of alkaline solution with alkaline silicate solution
  • a source of aluminosilicate material such as fly ash, kaolin, metakaolin, blast furnace slag, etc. Conc
  • Oligomers are of rea rrangement of gel formation polycondensation networking solidification. Broadly, de- polymerization, transportation or orientation and polycondensation are three main mechanisms in development of alkali-activated binders.
  • the product of reaction is an inorganic material, which has been coined "geopolymer".
  • Taftan pozzolan had four crystalline mineral phases; quartz, hornblende, anor- thite and biotite.
  • quartz, hornblende, anor- thite and biotite were not reactive. Based on their result, the final setting times of all their systems were relatively long due to high liquid/solid ratio of 0.44.
  • the invention has for its object to remedy or to reduce at least one of the drawbacks of the prior art, or at least provide a useful alternative to prior art.
  • the object is achieved through features, which are specified in the description below and in the claims that follow.
  • Geopolymers are one of the materials which chemo-physical characteristics and abundance have attracted much attention, recently. Geopolymeric cements result from a mineral polycondensation reaction in an alkaline medium. If geopolymers (reactive alumino-silicate materials) are mixed with appropriate additives under suitable temperature and pressure, they set and the final product can withstand high pressures, temperatures and corrosive environments for long-term.
  • Geopolymers are a are used as alternative to cement and replacing binder in concrete.
  • n is a degree of polycondensation
  • z is the atomic ratio of
  • Si/AI which may be 1, 2, 3 or higher.
  • geopolymers are alumino-silicate materials, which react in alkaline solution. The reaction shows a complex process but it could be said that in an alkaline medium the bonds of Si-O-Si are broken and Al atoms penetrate into the original Si-O-Si structure; alumino-silicate gels are mostly formed in the process. Cations must be present in the framework cavities to balance the negative charges of ions (J. Davidovits: "Geopolymer chemistry & applications", 3 rd edition, July 2011, p. 3-5, 228-230, 365-371, 375-386. F.
  • the geopolymerization development depends on many pa rameters including chemical and mineralogical composition, particle size and surface area, cu ring temperature and pressure, alkali cation type, Si/AI ratio of the used substances, activator/solid ratio, and types of additives (E. I. Diaz, E. N. Allouche, S. Eklund : "Factors affecting the suitability of fly ash as source material for geopolymers” Elsevier, Fuel, Vol. 89, 2010, p. 992-996. D. L. Y. Kong, J. G. Sanjayan, K. Sagoe-Crentsil; "Factors affecting the performance of metakaolin geopolymers exposed to elevated temperatures.” Journal of Material Science, Vol.
  • geopolymers based on the used source e.g., kaolinite- based, metakaolin-based, fly ash-based, phosphate-based, etc.
  • Aplite is an intrusive rock in which quartz, alkali feldspar, microcline and albite are the dominant components. Oligoclase, muscovite, apatite and zircon are principally minerals of aplites. Biotite and all ferromagnesian minerals rarely appear in aplites. Aplite members are usually Na-rich. Aplites contain Si0 2 and Al 2 0 3 and whereby are similar to pozzolans, and they seem to have the potential to be utilized in development of an aplite-based geopolymer cement.
  • the present invention introduces a new geopolymeric material, which can be called as an aplite-based geopolymer and prepared for oilfield cementing applications like sealing annuli between casings, sealing an annulus between a liner and a formation, zonal isolation, temporary and permanent plugging, and squeeze operations.
  • Aplite is mixed with additives and an alkali activator to prepare a geopolymeric slurry.
  • the additives are Blast Furnace Slag (BFS) and Microsilica.
  • BFS Blast Furnace Slag
  • the alkali activator is prepared by mixing various concentrations of alkali solution and alkali silicate solution.
  • the main objective is to create a cementitious material, which gets high enough compressive strength in order to withstand some degree of tectonic stresses.
  • the product should be impermeable, non-shrinking, withstand corrosive environments and bonds with rocks and casings.
  • UCS Uniaxial Compressive Strength
  • the invention relates more particularly to a cementitious aplite-based geopolymeric material, characterised in that a mixture of fine-grained aplite and an alkaline medium concentration including an alkali solution and an alkali silicate solution is forming a curable slurry.
  • the aplite particle size might be maximum 75 ⁇ .
  • the alkali solution may comprise NaOH in the range of 6M-10M.
  • the alkali solution may comprise NaOH in the range of 7M-9M.
  • the alkali solution may comprise KOH in the range of 4M-8M.
  • the alkali solution may comprise KOH in the range of 5M-7M.
  • the liquid/solid ratio of the mixture may be in the range of 0.40-0.50 by weight. Alternatively, the liquid/solid ratio of the mixture may be in the range of 0.42-0.47 by weight.
  • the invention relates more particularly to a method of providing a curable slurry of a cementitious aplite-based geopolymeric material, characterised in that the method comprises the steps of:
  • the method may comprise the further steps of:
  • Table 1 tabulates the chemical composition of grinded aplite which was supplied by HELI Utvikling AS, Namskogan, Norway.
  • Fig. 1 depicts the particle size distribution analysis of the used aplite.
  • Elkem microsilica grade 955 was supplied by Elkem AS, Oslo, Norway.
  • BFS Blast Furnace Slag
  • SSAB Merox AB Oxelosund, Sweden under the brand name of Merit 5000.
  • Sodium hydroxide (NaOH) and potassium hydroxide (KOH) came as pellets with 99% purity delivered by Merck KGaA, Darmstadt, Germany.
  • Sodium silicate solution Na 2 Si0 3
  • the chemical composition of the Na 2 Si0 3 was: 28.5% Si0 2 , 8.5% Na 2 0 and 63% H 2 0.
  • Potassium silicate solution (K 2 Si0 3 ) used was supplied by Univar AS, Oslo, Norway. Potassium silicate solution reported to have 38% of K 2 Si0 3 and 62% H 2 0. Distilled water was used throughout the experiments. Table 1
  • Sodium hydroxide solutions were prepared with three different concentrations of 6, 8, and 10 M of NaOH. Potassium hydroxide solutions were prepared with concentrations of 4 and 6 M.
  • Activators were prepared with different proportions as Table 2 summarizes alkali solution/alkali silicate ratios. It is recommended to prepare the activator one day before to get the components uniformly mixed. Liquid-solid mixing should be respected in order to get the most efficient product. Prime, micro silica should be added to the activator and mixed for 2 minutes. Then aplite was added and mixed for 2 minutes. Latter BFS was added and mixed . Liquid and solid phases were mixed by using a Hamilton Beach blender. Slurries were cast into cylindrical plastic moulds of dimensions of 5.2 cm in diameter and 10 cm in length. Table 3 outlines the different recipes, which have shown the prime results. Specimens were cured at ambient pres- sure and temperature for 7 and 28 days within a plastic box, which was filled with tap water. Note that specimens could be cured out of the plastic box.
  • a Zeiss Supra 35VP model scanning electron microscope (SEM) analyzer was used to reveal the microstructure of the aplite-based geopolymers.
  • Particle Size Distributions (PSD) of aplite was estimated by Sympatec HELOS laser diffraction particle size analyzer and experiment was performed at Tel-Tek national research institute in Norway. Sauter Mean Diameter (SMD) and Volume Mean Diameter (VMD) were reported 3.20 and 19.68 ⁇ , respectively. Aplite's density estimated to be 1.18 (g/cc).
  • X-ray powder diffraction (XRD) analysis of the aplite and the produced geopolymers were performed using synchrotron radiation with wavelength of 0.6888A.
  • the XRD measurements were performed with a PILATUS2M -based diffracto meter at European Synchrotron Radiation Facility (ESRF).
  • the angular range was 0-46, 2theta.
  • the obtained result shows the aplite and aplite-based geopolymers are crystalline.
  • aplite-based geopolymers Due to low CaO content (20%) the aplite-based geopolymers can withstand carbon dioxide attacks.
  • the aplite-based geopolymer does not produce greenhouse gases, it can be called an environmental friendly cementitious material.
  • Sodium hydroxide concentration can vary between 6 and 10 M and even higher.
  • Potassium hydroxide concentration can vary between 4 and 8 M.
  • Alkali solution to alkali silicate solution ratio can vary between 0.3 and 1.
  • Fig. 1 Particle Size Distribution (PSD) analysis of the used aplite
  • Fig. 2a Estimated compressive strength of the aplite-based geopolymer with an alkali solution comprising NaOH after 7 and 28 days
  • Fig. 2b Estimated compressive strength of the aplite-based geopolymer with an alkali solution comprising KOH after 7 and 28 days.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Organic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Structural Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Geology (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Environmental & Geological Engineering (AREA)
  • Curing Cements, Concrete, And Artificial Stone (AREA)

Abstract

L'invention porte sur un matériau géopolymère cimentaire à base d'aplite, un mélange d'aplite à grains fins et d'une concentration de milieu alcalin comprenant une solution alcaline et une solution de silicate de métal alcalin formant une suspension épaisse durcissable. L'invention porte également sur un procédé de production d'une suspension épaisse durcissable d'un matériau géopolymère cimentaire à base d'aplite, le procédé comprenant les étapes consistant à : utiliser une aplite à grains fins ; et ajouter une concentration d'une solution alcaline et d'une solution de silicate de métal alcalin en un rapport liquide/solide dans la plage de 0,40 à 0,50.
PCT/NO2015/050146 2014-08-29 2015-08-27 Matériau géopolymère cimentaire à base d'aplite Ceased WO2016032341A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
NO20141050A NO342894B1 (no) 2014-08-29 2014-08-29 Sementerende, aplittbasert geopolymermateriale og fremgangsmåte for å tilveiebringe en pumpbar, herdbar velling av et sementerende, aplittbasert geopolymermateriale
NO20141050 2014-08-29

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US9957434B2 (en) 2015-11-18 2018-05-01 Board Of Regents, The University Of Texas System Cementitious compositions comprising a non-aqueous fluid and an alkali-activated material
WO2022140155A1 (fr) * 2020-12-21 2022-06-30 Terra Co2 Technology Holdings, Inc. Réactifs cimentaires, leurs procédés de fabrication et leurs utilisations
US11485681B2 (en) 2019-06-27 2022-11-01 Terra Co2 Technology Holdings, Inc. Cementitious reagents, methods of manufacturing and uses thereof
US11591262B2 (en) 2019-06-27 2023-02-28 Terra Co2 Technology Holdings, Inc. Cementitious reagents, methods of manufacturing and uses thereof

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2006114623A2 (fr) * 2005-04-26 2006-11-02 Statoilhydro Asa Procede de construction et de traitement de puits
WO2009103480A1 (fr) * 2008-02-19 2009-08-27 Services Petroliers Schlumberger Formulation géopolymère pompable pour application à un champ pétrolifère
US20120152153A1 (en) * 2010-12-17 2012-06-21 The Catholic University Of America Geopolymer composite for ultra high performance concrete

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DK2338949T3 (da) * 2009-12-17 2012-11-05 Schlumberger Technology Bv Pumpbare geopolymerer omfattende et blandehjælpemiddel og et dispergeringsmiddel
NL2008863C2 (en) * 2012-05-23 2013-11-26 Pqa B V Geopolymer composition comprising additives.

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2006114623A2 (fr) * 2005-04-26 2006-11-02 Statoilhydro Asa Procede de construction et de traitement de puits
WO2009103480A1 (fr) * 2008-02-19 2009-08-27 Services Petroliers Schlumberger Formulation géopolymère pompable pour application à un champ pétrolifère
US20120152153A1 (en) * 2010-12-17 2012-06-21 The Catholic University Of America Geopolymer composite for ultra high performance concrete

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
SIMONSEN, E.: "STRENGTH DEVELOPMENT OF APLITE-BASED GEOPOLYMER CEMENTS", MASTER THESIS, 13 November 2013 (2013-11-13) *

Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US9957434B2 (en) 2015-11-18 2018-05-01 Board Of Regents, The University Of Texas System Cementitious compositions comprising a non-aqueous fluid and an alkali-activated material
US11485681B2 (en) 2019-06-27 2022-11-01 Terra Co2 Technology Holdings, Inc. Cementitious reagents, methods of manufacturing and uses thereof
US11542196B2 (en) 2019-06-27 2023-01-03 Terra Co2 Technology Holdings, Inc. Cementitious reagents, methods of manufacturing and uses thereof
US11548819B2 (en) 2019-06-27 2023-01-10 Terra Co2 Technology Holdings, Inc. Cementitious reagents, methods of manufacturing and uses thereof
US11560333B2 (en) 2019-06-27 2023-01-24 Terra Co2 Technology Holdings, Inc. Cementitious reagents, methods of manufacturing and uses thereof
US11591263B2 (en) 2019-06-27 2023-02-28 Terra Co2 Technology Holdings, Inc. Cementitious reagents, methods of manufacturing and uses thereof
US11591262B2 (en) 2019-06-27 2023-02-28 Terra Co2 Technology Holdings, Inc. Cementitious reagents, methods of manufacturing and uses thereof
US11597679B2 (en) 2019-06-27 2023-03-07 Terra Co2 Technology Holdings, Inc. Cementitious reagents, methods of manufacturing and uses thereof
US11649189B2 (en) 2019-06-27 2023-05-16 Terra Co2 Technology Holdings, Inc. Cementitious reagents, methods of manufacturing and uses thereof
US12234185B2 (en) 2019-06-27 2025-02-25 Terra Co2 Technology Holdings, Inc. Cementitious reagents, methods of manufacturing and uses thereof
WO2022140155A1 (fr) * 2020-12-21 2022-06-30 Terra Co2 Technology Holdings, Inc. Réactifs cimentaires, leurs procédés de fabrication et leurs utilisations

Also Published As

Publication number Publication date
NO20141050A1 (no) 2016-03-01
NO342894B1 (no) 2018-08-27

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