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WO2016003289A1 - Matériau cimentaire géopolymère à base de norite - Google Patents

Matériau cimentaire géopolymère à base de norite Download PDF

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Publication number
WO2016003289A1
WO2016003289A1 PCT/NO2015/050115 NO2015050115W WO2016003289A1 WO 2016003289 A1 WO2016003289 A1 WO 2016003289A1 NO 2015050115 W NO2015050115 W NO 2015050115W WO 2016003289 A1 WO2016003289 A1 WO 2016003289A1
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WIPO (PCT)
Prior art keywords
norite
range
cementitious
alkali
solution
Prior art date
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Ceased
Application number
PCT/NO2015/050115
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English (en)
Inventor
Mahmoud KHALIFEH
Helge HODNE
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Individual
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Individual
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Publication of WO2016003289A1 publication Critical patent/WO2016003289A1/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
    • 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
    • C04B14/00—Use of inorganic materials as fillers, e.g. pigments, for mortars, concrete or artificial stone; Treatment of inorganic materials specially adapted to enhance their filling properties in mortars, concrete or artificial stone
    • C04B14/02—Granular materials, e.g. microballoons
    • C04B14/04—Silica-rich materials; Silicates
    • C04B14/14—Minerals of vulcanic origin
    • 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
    • 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
    • C04B2111/00215—Mortar or concrete mixtures defined by their oxide composition
    • 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

Definitions

  • the invention is concerning a cementitious norite-based geopolymeric material and a method of providing a curable slurry of a cementitious norite-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 over 175 years ago, it has become the most common construction ingredient produced practically in many countries. Portland cement is also the most common material used in petroleum industry for zonal isolation.
  • cement has some advantages such as; low fluid loss, adjustable slurry parameters, pumpability, and builds rather enough compressive strength at moderated temperatures.
  • sealant for zonal isolation which motivate petroleum industry to attempt potential alternatives to cement.
  • cement experiences degradation at corrosive environments, it has low tensile strength, shrinks and develops low compressive strength at high temperatures ( ⁇ above 150° C).
  • cement is not ductile and thus it does not withstand tectonic stresses. Potential gas influx is also a concern with respect to Portland cement permeability.
  • 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 new class of inorganic materials, which are used as alternative to cement and replacing binder in concrete.
  • geopolymers are alumino-silicate materials, which react in alkaline solution. The reaction shows a complex process as respects universally it could be said that in 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.
  • geopolymers are characterized by a number of physical characteristics including thermal stability, high surface smoothness, hard surface, long-term durability and high adhesive property to natural stone and steel.
  • thermal stability high surface smoothness
  • hard surface hard surface
  • long-term durability high adhesive property to natural stone and steel.
  • only few published studies exist on the corrosion of metal bars in geopolymer concrete (Davidovits, 2011. Xu, 2002).
  • the geopolymerization development depends on many parameters including chemical and mineralogical composition, particle size and surface area, curing 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.
  • geopolymers based on the used source e.g., kaolinite- based, metakaolin-based, fly ash-based, phosphate-based, etc.
  • the present invention introduces a new geopolymeric material, which can be called as norite-based geopolymer and prepared for oilfield cementing applications.
  • Norite is mixed with an alkali activator to prepare a geopolymeric slurry.
  • Alkali activator is prepared by mixing various concentrations of alkali solution and alkali silicate solution .
  • Norite-based geopolymer sets at 25 - 200 °C under ambient pressure and high pressures.
  • the main objective is to get a high enough compressive strength of the set material and to find the effect of different additives on the rheological and physical property of the slurry and final product after setting .
  • Ultrasonic Cement Analyzer UCA
  • UCS Uniaxial Compressive Strength
  • sets of sensitivity analysis tests have been performed to find the influence of alkali concentration, liquid/solid ratio, curing temperature and pressure on the chemo-physical property of the developed norite-based geopolymer.
  • Norite is an intrusive igneous rock and predominantly composed of orthopyroxene and plagioclase.
  • Orthopyroxene is an inosilicate and therefore has interlocking chains of silicate tetrahedra.
  • Norite contains ilmenite and in the Streckeisen system is in the same group with gabbro and anorthosite (H. Pichler, C. Schmitt-Riegraf: "Rock- forming minerals in thin section", second edition, 1997. Translated to English by L. Hoke, 1997. Published by Chapman & Hall). Similar to gabbro and anorthosite, norite is very rich in plagioclase compared to K-feldspar and quartz.
  • the present invention introduces a new geopolymeric material, which can be called as norite-based geopolymer and prepared for oilfield cementing applications like sealing an annulus between casings, sealing an annulus between a liner and a formation, zonal isolation, temporary and permanent plugging, and squeeze operations.
  • the invention relates more particularly to a cementitious norite-based geopolymeric material, wherein a mixture of fine-grained norite and an alkaline medium concentration including an alkali solution and an alkali silicate solution is forming a curable slurry.
  • the norite particle size may be maximum 75 ⁇ .
  • the alkali solution may comprise NaOH in the range of 6M-10M, more preferably in the range of 7M-9M.
  • the alkali solution may comprise KOH in the range of 4M-8M more preferably in the range of 5M-7M.
  • the liquid/solid ratio of the mixture may be in the range of 0.35-0.50 by weight, more preferably in the range of 0.40-0.45 by weight.
  • the molar ratio of Na 2 0/Si0 2 or K 2 0/Si0 2 respectively may be in the range of 0-2.0.
  • the norite may be calcined.
  • the invention relates more particularly to a method of providing a curable slurry of a cementitious norite-based geopolymeric material, wherein the method comprises the steps of:
  • the method may comprise the further step of:
  • the method may comprise the further step of:
  • norite was used for forming geopolymer binder and geopolymer cement.
  • Norite which is a waste stream in production of titanium dioxide, was supplied by Kronos Titan AS, Fredrikstad, Norway. The norite particle size was less than 1 mm.
  • Chemical analysis and traced minerals of norite are tabulated in Tables 1 and 2 as given by Kronos Titan AS.
  • the laboratory at Kronos Titan AS reports the pH for norite to be 6.5 (Kronos Titan AS, 2004).
  • the NaOH and KOH pellets were caustic soda with 99% purity and were made in Germany under the brand name of Merck.
  • the slurry density is necessary to be measured in order to select the appropriate empirical correlation for strength measurement.
  • a pycnometer was used for density measurement. Densities were measured at room temperature and atmospheric pressure.
  • UCS Uniaxial Compressive Strength
  • Toni Kunststoff-H mechanical tester was deployed .
  • the apparatus applies a TestXpert v7.11 testing software to calculate the compressive strength.
  • the compressive strength of the specimens were measured according to ASTM CI 09.
  • an Ultrasonic Cement Analyzer was used.
  • the UCA provides a continuous non-destructive method of determining compressive strength as a function of time by measuring the transient times of an acoustic signal. Transient times are converted to compressive strength by means of some empirical correlations. The convenient correlation could be identified by using the specific gravity of the slurry.
  • HP/HT high-pressure/high- temperature
  • Every well is unique and needs its particular slurry design.
  • Slurry should be designed based on the well parameters such as: well depth, circulating temperature, well pressure, well diameter and fracture gradient.
  • Table 3 shows measured compressive strengths of some of norite-based geopolymers. Curing pressure and temperature was selected based on a real oilfield data, which are 1200 psi and 88 °C.
  • Fig. 4 reveals the estimated compressive strength for produced grinded norite-based geopolymers with different concentration of NaOH.
  • Test no. 1 was accomplished for non-grinded and the second one for grinded norite. Both of specimens were mixed with the 8 M NaOH in separate containers. Liquid/solid ratio of 0.4 by weight was kept constant for both specimens. Specimens were cured at ambient conditions for 7 days. The obtained specimen from test no. 1 was non-consolidated while the other one was consolidated, see figures 3a and 3b.
  • Fig. 4 shows the obtained results for grinded norite-based geopolymers for various concentrations of NaOH.
  • Fig. 5 reveals the obtained results of the strength build-up for both experiments.
  • Fig. 3a Effect of particle size on reactivity of grinded norite

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Organic Chemistry (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Materials Engineering (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Structural Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Geology (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Environmental & Geological Engineering (AREA)
  • Civil Engineering (AREA)
  • Curing Cements, Concrete, And Artificial Stone (AREA)
  • Devices For Post-Treatments, Processing, Supply, Discharge, And Other Processes (AREA)

Abstract

L'invention concerne un matériau cimentaire géopolymère à base de norite, un mélange de norite à grains fins et d'une concentration de milieu alcalin comprenant une solution alcaline et une solution de silicate alcalin formant une suspension épaisse durcissable. L'invention concerne également un procédé de formation d'une suspension épaisse durcissable d'un matériau cimentaire géopolymère à base de norite, le procédé comprenant les étapes consistant à : utiliser une norite à grains fins ; et ajouter une concentration d'une solution alcaline et d'une solution de silicate alcalin en un rapport liquide-solide dans la plage de 0,35 à 0,50.
PCT/NO2015/050115 2014-06-30 2015-06-25 Matériau cimentaire géopolymère à base de norite Ceased WO2016003289A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
NO20140831 2014-06-30
NO20140831A NO342076B1 (no) 2014-06-30 2014-06-30 Sementerende, norittbasert geopolymermateriale og fremgangsmåte for å tilveiebringe en pumpbar, herdbar velling av et sementerende, norittbasert geopolymermateriale

Publications (1)

Publication Number Publication Date
WO2016003289A1 true WO2016003289A1 (fr) 2016-01-07

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NO (1) NO342076B1 (fr)
WO (1) WO2016003289A1 (fr)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2017199198A1 (fr) * 2016-05-20 2017-11-23 The Catholic University Of America Composition géopolymère pompable pour applications d'étanchéification de puits
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
WO2021110571A1 (fr) * 2019-12-06 2021-06-10 The University Of Stavanger Procédé de minéralisation de co2 dans des polymères inorganiques (géopolymères)

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20050160946A1 (en) * 2003-01-31 2005-07-28 Comrie Douglas C. Cementitious materials including stainless steel slag and geopolymers
WO2008017413A1 (fr) * 2006-08-07 2008-02-14 Services Petroliers Schlumberger Formulation géopolymérique pompable et application pour le stockage de dioxyde de carbone
WO2009103480A1 (fr) * 2008-02-19 2009-08-27 Services Petroliers Schlumberger Formulation géopolymère pompable pour application à un champ pétrolifère
WO2011072784A1 (fr) * 2009-12-17 2011-06-23 Services Petroliers Schlumberger Géopolymères aptes au pompage comprenant un auxiliaire de mélange et un agent de dispersion
WO2013176545A1 (fr) * 2012-05-23 2013-11-28 Pqa B.V. Composition géopolymère comprenant des additifs

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20050160946A1 (en) * 2003-01-31 2005-07-28 Comrie Douglas C. Cementitious materials including stainless steel slag and geopolymers
WO2008017413A1 (fr) * 2006-08-07 2008-02-14 Services Petroliers Schlumberger Formulation géopolymérique pompable et application pour le stockage de dioxyde de carbone
WO2009103480A1 (fr) * 2008-02-19 2009-08-27 Services Petroliers Schlumberger Formulation géopolymère pompable pour application à un champ pétrolifère
WO2011072784A1 (fr) * 2009-12-17 2011-06-23 Services Petroliers Schlumberger Géopolymères aptes au pompage comprenant un auxiliaire de mélange et un agent de dispersion
WO2013176545A1 (fr) * 2012-05-23 2013-11-28 Pqa B.V. Composition géopolymère comprenant des additifs

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
KOLBERG, L.E.: "Geopolymerization of Norite", MASTER THESIS, FACULTY OF SCIENCE AND TECHNOLOGY, University of Stavanger, XP055250516 *

Cited By (3)

* 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
WO2017199198A1 (fr) * 2016-05-20 2017-11-23 The Catholic University Of America Composition géopolymère pompable pour applications d'étanchéification de puits
WO2021110571A1 (fr) * 2019-12-06 2021-06-10 The University Of Stavanger Procédé de minéralisation de co2 dans des polymères inorganiques (géopolymères)

Also Published As

Publication number Publication date
NO20140831A1 (no) 2015-12-31
NO342076B1 (no) 2018-03-19

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