WO2015081014A1 - Plugging and abandoning a well using a set-delayed cement composition comprising pumice - Google Patents
Plugging and abandoning a well using a set-delayed cement composition comprising pumice Download PDFInfo
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- WO2015081014A1 WO2015081014A1 PCT/US2014/067112 US2014067112W WO2015081014A1 WO 2015081014 A1 WO2015081014 A1 WO 2015081014A1 US 2014067112 W US2014067112 W US 2014067112W WO 2015081014 A1 WO2015081014 A1 WO 2015081014A1
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- cement composition
- delayed cement
- delayed
- pumice
- dispersant
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- 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
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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
- C04B28/02—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
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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
- C04B40/00—Processes, in general, for influencing or modifying the properties of mortars, concrete or artificial stone compositions, e.g. their setting or hardening ability
- C04B40/0028—Aspects relating to the mixing step of the mortar preparation
- C04B40/0039—Premixtures of ingredients
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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
- C04B40/00—Processes, in general, for influencing or modifying the properties of mortars, concrete or artificial stone compositions, e.g. their setting or hardening ability
- C04B40/06—Inhibiting the setting, e.g. mortars of the deferred action type containing water in breakable containers ; Inhibiting the action of active ingredients
- C04B40/0658—Retarder inhibited mortars activated by the addition of accelerators or retarder-neutralising agents
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- 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
- C09K8/426—Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells for plugging
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- 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
- C09K8/467—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 containing additives for specific purposes
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- E—FIXED CONSTRUCTIONS
- E21—EARTH DRILLING; MINING
- E21B—EARTH DRILLING, e.g. DEEP DRILLING; OBTAINING OIL, GAS, WATER, SOLUBLE OR MELTABLE MATERIALS OR A SLURRY OF MINERALS FROM WELLS
- E21B33/00—Sealing or packing boreholes or wells
- E21B33/10—Sealing or packing boreholes or wells in the borehole
- E21B33/13—Methods or devices for cementing, for plugging holes, crevices, or the like
Definitions
- Embodiments relate to subterranean cementing operations and, in certain embodiments, to set-delayed cement compositions and methods of using set-delayed cement compositions in subterranean formations.
- cement compositions may be used in a variety of subterranean operations.
- a pipe string e.g., casing, liners, expandable tubulars, etc.
- the process of cementing the pipe string in place is commonly referred to as "primary cementing.”
- primary cementing In a typical primary cementing method, a cement composition may be pumped into an annulus between the walls of the wellbore and the exterior surface of the pipe string disposed therein.
- the cement composition may set in the annular space, thereby forming an annular sheath of hardened, substantially impermeable cement (i.e., a cement sheath) that may support and position the pipe string in the wellbore and may bond the exterior surface of the pipe string to the subterranean formation.
- a cement sheath the cement sheath surrounding the pipe string functions to prevent the migration of fluids in the annulus, as well as protecting the pipe string from corrosion.
- Cement compositions also may be used in remedial cementing methods, for example, to seal cracks or holes in pipe strings or cement sheaths, to seal highly permeable formation zones or fractures, to place a cement plug, and the like.
- a broad variety of cement compositions have been used in subterranean cementing operations.
- set-delayed cement compositions have been used.
- Set-delayed cement compositions are characterized by remaining in a pumpable fluid state for about one day or longer (e.g., about 7 days, about 2 weeks, about 2 years or more) at room temperature (e.g., about 80° F) in quiescent storage.
- the set-delayed cement compositions should be capable of being activated whereby reasonable compressive strengths are developed.
- a cement set activator may be added to a set-delayed cement composition whereby the composition sets into a hardened mass.
- the set-delayed cement composition may be suitable for use in wellbore applications, for example, where it is desired to prepare the cement composition in advance.
- This may allow, for example, the cement composition to be stored prior to its use.
- this may allow, for example, the cement composition to be prepared at a convenient location and then transported to the job site. Accordingly, capital expenditures may be reduced due to a reduction in the need for on-site bulk storage and mixing equipment. This may be particularly useful for offshore cementing operations where space onboard the vessels may be limited.
- a plug is formed in a wellbore to seal off the wellbore for abandonment.
- a plugging composition may be placed in the wellbore at a desired depth.
- the plugging composition should set in the wellbore, forming a hardened mass (e.g., a plug) that seals off selected intervals of the wellbore.
- the plug should prevent and/or reduce zonal communication and migration of fluids that may contaminate water-containing formations. It may desirable in certain instances to form one or more plugs in the wellbore adjacent to hydrocarbon-producing formations and water-containing formations.
- set-delayed cement compositions have been developed heretofore, challenges exist with their successful use in subterranean cementing operations.
- set-delayed cement compositions prepared with Portland cement may have undesired gelation issues which can limit their use and effectiveness in cementing operations.
- Other set-delayed compositions that have been developed, for example, those comprising hydrated lime and quartz, may be effective in some operations but may have limited use at lower temperatures as they may not develop sufficient compressive strength when used in subterranean formations having lower bottom hole static temperatures.
- FIG. I illustrates a system for the preparation and delivery of a set-delayed cement composition into a wellbore in accordance with certain embodiments.
- FIG. 2A illustrates a liquid storage vessel that may be used in the delivery of a set-delayed cement composition into a wellbore in accordance with certain embodiments.
- FIG. 2B illustrates a self-contained delivery system that may be used in the delivery of a set-delayed cement composition into a wellbore in accordance with certain embodiments.
- FIG. 3 illustrates an example embodiment of surface equipment that may be used in the placement of a set-delayed cement composition in accordance with certain embodiments.
- FIG. 4 illustrates an embodiment for the placement of a set-delayed cement composition across a set of open perforations and/or a casing leak in accordance with certain embodiments.
- FIG. 5 illustrates an embodiment for the placement of a set-delayed cement composition within an openhole section in accordance with certain embodiments.
- FIG. 6 illustrates an embodiment for the placement of a set-delayed cement composition across the top of a fish and/or casing stub in accordance with certain embodiments.
- FIG. 7 illustrates an embodiment for the placement of a set-delayed cement composition utilizing a wireline deployed dump bailer in accordance with certain embodiments.
- FIG. 8 illustrates an example of surface equipment that may be used in embodiments comprising a wireline dump bailer for placement of a set-delayed cement composition in accordance with certain embodiments.
- Embodiments relate to subterranean cementing operations and, in certain embodiments, to set-delayed cement compositions and methods of using set-delayed cement compositions in subterranean formations.
- set-delayed cement compositions are described for use in plug and abandon operations.
- Embodiments of the set-delayed cement compositions may generally comprise water, pumice, hydrated lime, and a set retarder.
- the set-delayed cement compositions may further comprise a dispersant and/or a viscosifier.
- Embodiments of the set- delayed cement compositions may be foamed.
- embodiments of the set- delayed cement compositions may be capable of remaining in a pumpable fluid state for an extended period of time.
- the set-delayed cement compositions may remain in a pumpable fluid state for about 1 day, about 2 weeks, about 2 years, or longer.
- the set-delayed cement compositions may develop reasonable compressive strengths after activation at relatively low temperatures.
- the set-delayed cement compositions may be suitable for a number of subterranean cementing operations, they may be particularly suitable for use in subterranean formations having relatively low bottom hole static temperatures, e.g., temperatures less than about 200°F or ranging from about 100°F to about 200°F. In alternative embodiments, the set-delayed cement compositions may be used in subterranean formations having bottom hole static temperatures up to 450°F or higher.
- the water used in embodiments of the set-delayed cement compositions may be from any source provided that it does not contain an excess of compounds that may undesirably affect other components in the set-delayed cement compositions.
- a set-delayed cement composition may comprise fresh water or salt water.
- Salt water generally may include one or more dissolved salts therein and may be saturated or unsaturated as desired for a particular application. Seawater or brines may be suitable for use in embodiments.
- the water may be present in an amount sufficient to form a pumpable slurry. In certain embodiments, the water may be present in the set-delayed cement composition in an amount in the range of from about 33% to about 200% by weight of the pumice.
- the water may be present in the set-delayed cement compositions in an amount in the range of from about 35% to about 70% by weight of the pumice.
- the water may be present in the set-delayed cement compositions in an amount in the range of from about 35% to about 70% by weight of the pumice.
- Embodiments of the set-delayed cement compositions may comprise pumice.
- pumice is a volcanic rock that can exhibit cementitious properties in that it may set and harden in the presence of hydrated lime and water.
- the pumice may also be ground.
- the pumice may have any particle size distribution as desired for a particular application.
- the pumice may have a mean particle size in a range of from about 1 micron to about 200 microns. The mean particle size corresponds to d50 values as measured by particle size analyzers such as those manufactured by Malvern Instruments, Worcestershire, United Kingdom.
- the pumice may have a mean particle size in a range of from about 1 micron to about 200 microns, from about 5 microns to about 100 microns, or from about 10 microns to about 25 microns. In one particular embodiment, the pumice may have a mean particle size of less than about 15 microns.
- An example of a suitable pumice is available from Hess Pumice Products, Inc., Malad, Idaho, as DS-325 lightweight aggregate, having a particle size of less than about 15 microns. It should be appreciated that particle sizes too small may have mixability problems while particle sizes too large may not be effectively suspended in the compositions.
- One of ordinary skill in the art, with the benefit of this disclosure, should be able to select a particle size for the pumice suitable for a chosen application.
- Embodiments of the set-delayed cement compositions may comprise hydrated lime.
- the term "hydrated lime” will be understood to mean calcium hydroxide.
- the hydrated lime may be provided as quicklime (calcium oxide) which hydrates when mixed with water to form the hydrated lime.
- the hydrated lime may be included in embodiments of the set-delayed cement compositions, for example, to form a hydraulic composition with the pumice.
- the hydrated lime may be included in a pumice- to-hydrated-lime weight ratio of about 10: 1 to about 1 : 1 or 3: 1 to about 5: 1.
- the hydrated lime may be included in the set-delayed cement compositions in an amount in the range of from about 10% to about 100% by weight of the pumice, for example. In some embodiments, the hydrated lime may be present in an amount ranging between any of and/or including any of about 10%, about 20%, about 40%, about 60%, about 80%, or about 100% by weight of the pumice.
- the cementitious components present in the set-delayed cement composition may consist essentially of the pumice and the hydrated lime. For example, the cementitious components may primarily comprise the pumice and the hydrated lime without any additional components (e.g., Portland cement, fly ash, slag cement) that hydraulically set in the presence of water.
- additional components e.g., Portland cement, fly ash, slag cement
- Embodiments of the set-delayed cement compositions may comprise a set retarder.
- the set retarder may comprise phosphonic acids, such as amino tris(methylene phosphonic acid), ethylenediamine tetra(methylene phosphonic acid), diethylenetriamine penta(methylene phosphonic acid), etc.; lignosulfonates, such as sodium lignosulfonate, calcium lignosulfonate, etc.; salts such as stannous sulfate, lead acetate, monobasic calcium phosphate, organic acids, such as citric acid, tartaric acid, etc.; cellulose derivatives such as hydroxyl ethyl cellulose (HEC) and carboxymethyl hydroxyethyl cellulose (CMHEC); synthetic co- or ter-polymers comprising sulfonate and carboxylic acid groups such as sulfonate
- phosphonic acids such as amino tris(methylene phosphonic acid), ethylenediamine tetra
- Suitable set retarders include, among others, phosphonic acid derivatives.
- One example of a suitable set retarder is Micro Matrix ® cement retarder, available from Halliburton Energy Services, Inc.
- the set retarder may be present in the set-delayed cement compositions in an amount sufficient to delay the setting for a desired time. In some embodiments, the set retarder may be present in the set-delayed cement compositions in an amount in the range of from about 0.01 % to about 10% by weight of the pumice.
- the set retarder may be present in an amount ranging between any of and/or including any of about 0.01 %, about 0.1 %, about 1 %, about 2%, about 4%, about 6%, about 8%, or about 10% by weight of the pumice.
- the appropriate amount of the set retarder will recognize the appropriate amount of the set retarder to include for a chosen application.
- embodiments of the set-delayed cement compositions may optionally comprise a dispersant.
- suitable dispersants include, without limitation, sulfonated-formaldehyde-based dispersants (e.g., sulfonated acetone formaldehyde condensate), examples of which may include Daxad ® 19 dispersant available from Geo Specialty Chemicals, Ambler, Pennsylvania.
- Other suitable dispersants may be polycarboxylated ether dispersants such as Liquiment ® 558 I F and Liquiment ® 514L dispersants available from BASF Corporation Houston, Texas; or EthacrylTM G dispersant available from Coatex, Genay, France.
- a suitable commercially available dispersant is CFRTM-3 dispersant, available from Halliburton Energy Services, Inc, Houston, Texas.
- the Liquiment ® 514L dispersant may comprise 36% by weight of the polycarboxylated ether in water. While a variety of dispersants may be used in accordance with embodiments, polycarboxylated ether dispersants may be particularly suitable for use in some embodiments. Without being limited by theory, it is believed that polycarboxylated ether dispersants may synergistically interact with other components of the set-delayed cement composition.
- the polycarboxylated ether dispersants may react with certain set retarders (e.g., phosphonic acid derivatives) resulting in formation of a gel that suspends the pumice and hydrated lime in the composition for an extended period of time.
- certain set retarders e.g., phosphonic acid derivatives
- the dispersant may be included in the set-delayed cement compositions in an amount in the range of from about 0.01% to about 5% by weight of the pumice. In specific embodiments, the dispersant may be present in an amount ranging between any of and/or including any of about 0.01 %, about 0.1 %, about 0.5%, about 1 %, about 2%, about 3%, about 4%, or about 5% by weight of the pumice.
- One of ordinary skill in the art, with the benefit of this disclosure, will recognize the appropriate amount of the dispersant to include for a chosen application.
- a viscosifier may be included in the set-delayed cement compositions.
- the viscosifier may be included to optimize fluid rheology and to stabilize the suspension.
- examples of viscosifiers include swellable clays such as bentonite or biopolymers such as cellulose derivatives (e.g., hydroxyethyl cellulose, carboxymethyl cellulose, carboxymethyl hydroxyethyl cellulose).
- An example of a commercially available viscosifier is SA-1015TM available from Halliburton Energy Services, Inc., Houston, TX.
- the viscosifier may be included in the set-delayed cement compositions in an amount in the range of from about 0.01 % to about 0.5% by weight of the pumice. In specific embodiments, the viscosifier may be present in an amount ranging between any of and/or including any of about 0.01 %, about 0.05%, about 0.1 %, about 0.2%, about 0.3%, about 0.4%, or about 0.5% by weight of the pumice.
- One of ordinary skill in the art, with the benefit of this disclosure, will recognize the appropriate amount of viscosifier to include for a chosen application.
- additives suitable for use in subterranean cementing operations also may be included in embodiments of the set-delayed cement compositions.
- additives include, but are not limited to: weighting agents, lightweight additives, gas- generating additives, mechanical-property-enhancing additives, lost-circulation materials, filtration-control additives, fluid-loss-control additives, defoaming agents, foaming agents, thixotropic additives, and combinations thereof.
- suitable weighting agents include, for example, materials having a specific gravity of 3 or greater, such as barite.
- one or more of these additives may be added to the set-delayed cement compositions after storing but prior to the placement of a set-delayed cement composition into a subterranean formation.
- embodiments of the set- delayed cement compositions generally should have a density suitable for a particular application.
- the set-delayed cement compositions may have a density in the range of from about 4 pounds per gallon ("lb/gal") to about 20 lb/gal.
- the set-delayed cement compositions may have a density in the range of from about 8 lb/gal to about 17 lb/gal.
- Embodiments of the set-delayed cement compositions may be foamed or unfoamed or may comprise other means to reduce their densities, such as hollow microspheres, low-density elastic beads, or other density-reducing additives known in the art.
- the density may be reduced after storing the composition, but prior to placement in a subterranean formation.
- the set-delayed cement compositions may have a delayed set in that they remain in a pumpable fluid state for one day or longer (e.g., about 1 day, about 2 weeks, about 2 years or more) at room temperature (e.g., about 80° F) in quiescent storage.
- the set-delayed cement compositions may remain in a pumpable fluid state for a period of time from about 1 day to about 7 days or more.
- the set-delayed cement compositions may remain in a pumpable fluid state for about 1 day, about 7 days, about 10 days, about 20 days, about 30 days, about 40 days, about 50 days, about 60 days, or longer.
- a fluid is considered to be in a pumpable fluid state where the fluid has a consistency of less than 70 Bearden units of consistency ("Be"), as measured on a pressurized consistometer in accordance with the procedure for determining cement thickening times set forth in API RP Practice 10B-2, Recommended Practice for Testing Well Cements, First Edition, July 2005.
- Be Bearden units of consistency
- cement set activator or “activator”, as used herein, refers to an additive that activates a set-delayed or heavily retarded cement composition and may also accelerate the setting of the set-delayed, heavily retarded, or other cement composition.
- embodiments of the set-delayed cement compositions may be activated to form a hardened mass in a time period in the range of from about 1 hour to about 12 hours.
- embodiments of the set-delayed cement compositions may set to form a hardened mass in a time period ranging between any of and/or including any of about 1 hour, about 2 hours, about 4 hours, about 6 hours, about 8 hours, about 10 hours, or about 12 hours.
- the set-delayed cement compositions may set to have a desirable compressive strength after activation.
- Compressive strength is generally the capacity of a material or structure to withstand axially directed pushing forces.
- the compressive strength may be measured at a specified time after the set-delayed cement composition has been activated and the resultant composition is maintained under specified temperature and pressure conditions.
- Compressive strength can be measured by either destructive or non- destructive methods.
- the destructive method physically tests the strength of treatment fluid samples at various points in time by crushing the samples in a compression-testing machine.
- the compressive strength is calculated from the failure load divided by the cross-sectional area resisting the load and is reported in units of pound-force per square inch (psi).
- Nondestructive methods may employ a UCATM ultrasonic cement analyzer, available from Fann Instrument Company, Houston, TX.
- Compressive strength values may be determined in accordance with API RP 10B-2, Recommended Practice for Testing Well Cements, First Edition, July 2005.
- the set-delayed cement compositions may develop a 24- hour compressive strength in the range of from about 50 psi to about 5000 psi, alternatively, from about 100 psi to about 4500 psi, or alternatively from about 500 psi to about 4000 psi.
- the set-delayed cement compositions may develop a compressive strength in 24 hours of at least about 50 psi, at least about 100 psi, at least about 500 psi, or more.
- the compressive strength values may be determined using destructive or non-destructive methods at a temperature ranging from 100°F to 200°F.
- the set-delayed cement compositions may have desirable thickening times after activation.
- Thickening time typically refers to the time a fluid, such as a set-delayed cement composition, remains in a fluid state capable of being pumped.
- a number of different laboratory techniques may be used to measure thickening time.
- a pressurized consistometer operated in accordance with the procedure set forth in the aforementioned API RP Practice 10B-2, may be used to measure whether a fluid is in a pumpable fluid state.
- the thickening time may be the time for the treatment fluid to reach 70 Be and may be reported as the time to reach 70 Be.
- the cement compositions may have a thickening time of greater than about 1 hour, alternatively, greater than about 2 hours, alternatively greater than about 5 hours at 3,000 psi and temperatures in a range of from about 50°F to about 400°F, alternatively, in a range of from about 80°F to about 250°F, and alternatively at a temperature of about 140°F.
- Embodiments may include the addition of a cement set activator to the set- delayed cement compositions.
- suitable cement set activators include, but are not limited to: zeolites, amines such as triethanolamine, diethanolamine; silicates such as sodium silicate; zinc formate; calcium acetate; Groups IA and IIA hydroxides such as sodium hydroxide, magnesium hydroxide, and calcium hydroxide; monovalent salts such as sodium chloride; divalent salts such as calcium chloride; nanosilica (i.e., silica having a particle size of less than or equal to about 100 nanometers); polyphosphates; and combinations thereof.
- a combination of the polyphosphate and a monovalent salt may be used for activation.
- the monovalent salt may be any salt that dissociates to form a monovalent cation, such as sodium and potassium salts.
- suitable monovalent salts include potassium sulfate, and sodium sulfate.
- a variety of different polyphosphates may be used in combination with the monovalent salt for activation of the set-delayed cement compositions, including polymeric metaphosphate salts, phosphate salts, and combinations thereof.
- polymeric metaphosphate salts that may be used include sodium hexametaphosphate, sodium trimetaphosphate, sodium tetrametaphosphate, sodium pentametaphosphate, sodium heptametaphosphate, sodium octametaphosphate, and combinations thereof.
- a specific example of a suitable cement set activator comprises a combination of sodium sulfate and sodium hexametaphosphate.
- the activator may be provided and added to the set-delayed cement composition as a liquid additive, for example, a liquid additive comprising a monovalent salt, a polyphosphate, and optionally a dispersant.
- Some embodiments may include a cement set activator comprising a combination of a monovalent salt and a polyphosphate.
- the monovalent salt and the polyphosphate may be combined prior to addition to the set-delayed cement composition or may be separately added to the set-delayed cement composition.
- the monovalent salt may be any salt that dissociates to form a monovalent cation, such as sodium and potassium salts. Specific examples of suitable monovalent salts include potassium sulfate and sodium sulfate.
- a variety of different polyphosphates may be used in combination with the monovalent salt for activation of the set-delayed cement compositions, including polymeric metaphosphate salts, phosphate salts, and combinations thereof, for example.
- polymeric metaphosphate salts that may be used include sodium hexametaphosphate, sodium trimetaphosphate, sodium tetrametaphosphate, sodium pentametaphosphate, sodium heptametaphosphate, sodium octametaphosphate, and combinations thereof.
- a specific example of a suitable cement set activator comprises a combination of sodium sulfate and sodium hexametaphosphate.
- sodium hexametaphosphate is also known in the art to be a strong retarder of Portland cements. Because of the unique chemistry of polyphosphates, polyphosphates may be used as a cement set activator for embodiments of the set-delayed cement compositions disclosed herein.
- the ratio of the monovalent salt to the polyphosphate may range, for example, from about 5: 1 to about 1 :25 or from about 1 :1 to about 1 : 10.
- Embodiments of the cement set activator may comprise the monovalent salt and the polyphosphate salt in a ratio (monovalent salt to polyphosphate) ranging between any of and/or including any of about 5: 1 , 2: 1 , about 1 :1 , about 1 :2, about 1 :5, about 1 :10, about 1 :20, or about 1 :25.
- the combination of the monovalent salt and the polyphosphate may be mixed with a dispersant and water to form a liquid additive for activation of a set-delayed cement composition.
- suitable dispersants include, without limitation, the previously described dispersants, such as sulfonated-formaldehyde- based dispersants and polycarboxylated ether dispersants.
- a commercial dispersant is CFR-3TM dispersant, available from Halliburton Energy Services, Inc.
- a suitable polycarboxylated ether dispersant is Liquiment ® 514L or 5581 F dispersants, available from BASF Corporation, Houston, Texas.
- the liquid additive may function as a cement set activator.
- a cement set activator may also accelerate the setting of the set-delayed or heavily retarded cement.
- the use of a liquid additive to accelerate a set-delayed or heavily retarded cement is dependent upon the compositional makeup of the liquid additive as well as the compositional makeup of the set-delayed or heavily retarded cement. With the benefit of this disclosure, one of ordinary skill in the art should be able to formulate a liquid additive to activate and/or accelerate a set-delayed or heavily retarded cement composition.
- the cement set activator may be added to embodiments of the set-delayed cement composition in an amount sufficient to induce the set-delayed cement composition to set into a hardened mass.
- the cement set activator may be added to the set-delayed cement composition in an amount in the range of about 0.1 % to about 20% by weight of the pumice.
- the cement set activator may be present in an amount ranging between any of and/or including any of about 0.1 %, about 1 %, about 5%, about 10%, about 15%, or about 20% by weight of the pumice.
- One of ordinary skill in the art, with the benefit of this disclosure, will recognize the appropriate amount of cement set activator to include for a chosen application.
- a set-delayed cement composition may be used in a variety of subterranean operations, including primary and remedial cementing.
- a set-delayed cement composition may be provided that comprises water, pumice, hydrated lime, a set retarder, and optionally a dispersant.
- the set-delayed cement composition may be introduced into a subterranean formation and allowed to set therein.
- introducing the set-delayed cement composition into a subterranean formation includes introduction into any portion of the subterranean formation, including, without limitation, into a wellbore drilled into the subterranean formation, into a near wellbore region surrounding the wellbore, or into both.
- Embodiments may further include activation of the set-delayed cement composition.
- the activation of the set-delayed cement composition may comprise, for example, the addition of a cement set activator to the set-delayed cement composition.
- a set-delayed cement composition may be provided that comprises water, pumice, hydrated lime, a set retarder, and optionally a dispersant.
- the set- delayed cement composition may be stored, for example, in a vessel or other suitable container.
- the set-delayed cement composition may be permitted to remain in storage for a desired time period.
- the set-delayed cement composition may remain in storage for a time period of about 1 day or longer.
- the set-delayed cement composition may remain in storage for a time period of about 1 day, about 2 days, about 5 days, about 7 days, about 10 days, about 20 days, about 30 days, about 40 days, about 50 days, about 60 days, or longer.
- the set-delayed cement composition may remain in storage for a time period in a range of from about 1 day to about 7 days or longer. Thereafter, the set-delayed cement composition may be activated, for example, by addition of a cement set activator, introduced into a subterranean formation, and allowed to set therein.
- embodiments of the set- delayed cement composition may be introduced into an annular space between a conduit located in a wellbore and the walls of a wellbore (and/or a larger conduit in the wellbore), wherein the wellbore penetrates the subterranean formation.
- the set-delayed cement composition may be allowed to set in the annular space to form an annular sheath of hardened cement.
- the set-delayed cement composition may form a barrier that prevents the migration of fluids in the wellbore.
- the set-delayed cement composition may also, for example, support the conduit in the wellbore.
- a set-delayed cement composition may be used, for example, in squeeze-cementing operations or in the placement of cement plugs.
- the set-delayed composition may be placed in a wellbore to plug an opening (e.g., a void or crack) in the formation, in a gravel pack, in the conduit, in the cement sheath, and/or between the cement sheath and the conduit (e.g., a microannulus).
- embodiments of the set-delayed cement compositions may be used as plugging compositions for forming a seal in plug-and-abandon operations.
- Embodiments of the set-delayed cement plugging compositions may be used onshore or offshore.
- Set -delayed cement plugging compositions may be preferred over traditional plugging compositions in certain applications (e.g., offshore applications) because a set-delayed cement plugging composition may require less equipment and personnel to use, which may be particularly advantageous in operations where space is limited.
- An example of a method for plugging and abandoning a well comprises placing a plugging composition in a selected plug location in a wellbore and allowing the plugging composition to set to form a plug.
- the plug location may be selected so that the wellbore can be sealed off for abandonment.
- the plug location may be selected so that a selected interval of the wellbore may be sealed.
- the selected location may be adjacent to a hydrocarbon-containing formation or a water-containing formation.
- the plugging and abandoning operation may include the formation of two or more plugs in the wellbore.
- a method may further include the placement of a second plugging composition in another selected plug location in the wellbore.
- the plugging technique may comprise any such pump that is sufficient for a given application.
- certain applications may comprise wireline operated dump bailers.
- Embodiments comprise the formation of a cement plug in a wellbore with low permeability.
- Low permeability is defined as a plug with a permeability of less than about 0.1 millidarcy.
- a cement plug with low permeability prevents the migration of fluids and gas.
- An embodiment comprises A method of plugging a wellbore, comprising: providing a set-delayed cement composition comprising pumice, hydrated lime, a cement set retarder, and water; activating the set-delayed cement composition to produce an activated set- delayed cement composition; introducing the activated set-delayed cement composition into the wellbore; and allowing the activated set-delayed cement composition to form a plug in the wellbore that has a permeability of less than 0.1 millidarcy.
- the set-delayed cement composition may comprise one or more of the additional additives described herein.
- An embodiment comprises a method of plugging a wellbore, comprising: providing a cement composition comprising water, pumice, hydrated lime, a dispersant, a viscosifier, a weighting agent, and a cement set retarder; storing the cement composition for a period of about 1 day or longer; activating the cement composition to produce an activated cement composition; introducing the activated cement composition into the wellbore; and allowing the cement composition to form a plug in the wellbore that has a permeability of less than 0.1 millidarcy.
- the cement composition may comprise one or more of the additional additives described herein.
- An embodiment comprises a set-delayed cementing system for plugging a wellbore comprising: a set-delayed cement composition comprising: water, pumice, hydrated lime, and a cement set retarder; a cement set activator for activating the set-delayed cement composition, mixing equipment for mixing the set-delayed cement composition and the cement set activator to produce an activated set-delayed cement composition, and equipment for delivering the activated set-delayed cement composition to a wellbore.
- the set-delayed cement composition may further comprise one or more of the additional additives described herein.
- FIG. 1 illustrates a system 2 for the preparation of a set-delayed cement composition and subsequent delivery of the composition to a wellbore in accordance with certain embodiments.
- the set-delayed cement composition may be mixed in mixing equipment 4, such as a jet mixer, re-circulating mixer, or a batch mixer, for example, and then pumped via pumping equipment 6 to the wellbore.
- the mixing equipment 4 and the pumping equipment 6 may be disposed on one or more cement trucks as will be apparent to those of ordinary skill in the art.
- a jet mixer may be used, for example, to continuously mix the lime/settable material with the water as it is being pumped to the wellbore.
- a re-circulating mixer and/or a batch mixer may be used to mix the set-delayed cement composition, and the activator may be added to the mixer as a powder prior to pumping the cement composition downhole.
- the set-delayed cement composition may be prepared onshore and delivered to the well site in fit-for-purpose delivery tanks.
- the mixing equipment may be the same as described in the description of FIG. 1 above.
- the delivery system for some embodiments may include a liquid storage vessel 10 with a detached circulating pump 12, additive skid 14, and additive tank 16.
- the detached circulating pump 12 may be used to re-circulate the set-delayed cement composition in the liquid storage vessel 10.
- the additive skid 14 (which may include a pump, for example) may be used to deliver additives from additive tank 16 to the set-delayed cement composition in the liquid storage vessel 10.
- the delivery system for some embodiments may include a self-contained delivery system 18 which comprises a storage tank 20, circulating pump 22, liquid additive system 24, and additive tank 26.
- the circulating pump 22 may be used to re-circulate the set-delayed cement composition in the storage tank 20.
- the liquid additive system 24 (which may include a pump, for example) may be used to deliver additives from additive tank 26 to the set-delayed cement composition in the storage tank 20.
- FIG. 3 illustrates surface equipment 28, which may be used in the placement of a set-delayed cement composition in accordance with certain embodiments. It should be noted that while FIG.
- the surface equipment 28 may include a cementing unit 30, which may include one or more cement trucks.
- the cementing unit 30 may include mixing equipment 4 and pumping equipment 6 (e.g., FIG. 1 ) as will be apparent to those of ordinary skill in the art.
- the cementing unit 30 may pump a set-delayed cement composition 32 through a feed pipe 34 and to a tubing connection 36 which conveys the set- delayed cement composition 32 downhole.
- the set-delayed cement composition 32 may be placed across the perforations and/or casing leak 38 in accordance with example embodiments.
- a cement retainer or squeeze packer 40 may be ran to a depth above the open perforations and/or casing leak 38 and set on either wireline or tubing 42.
- wellbore 44 is shown extending generally vertically into the subterranean formation 46, the principles described herein are also applicable to wellbores that extend at an angle through the subterranean formation 46, such as horizontal and slanted wellbores.
- the wellbore 44 comprises walls 48.
- a casing 50 has been inserted into the wellbore 44.
- the casing 50 may be cemented to the walls 48 of the wellbore 44 by cement sheath 52.
- the set-delayed cement composition 32 may be pumped down the interior of the tubing 42.
- the set-delayed cement composition 32 may be allowed to flow down the interior of the tubing 42 through the cement retainer or squeeze packer 40 at the bottom of the tubing 42 and down across and into the open perforations and/or casing leak 38.
- the set-delayed cement composition 32 may be allowed to set inside the casing 50, for example, to form a plug that seals the open perforations and/or casing leak 38 in the wellbore 44.
- other techniques may also be utilized for introduction of the set-delayed cement composition 32.
- open ended tubing and/or drill pipe may be used to place the set-delayed cement composition 32 across the open perforations and/or casing leak 38.
- FIG. 5 illustrates an additional embodiment comprising the placement of the set-delayed cement composition 32 within an openhole section 54 to isolate the formation 46 below.
- FIG. 5 shows the set-delayed cement composition 32 inside the openhole section 54, but the set-delayed cement composition 32 may at times enter into the casing 50 above.
- the set-delayed cement composition 32 may be pumped through the drillpipe and/or tubing 42 and a cement retainer or squeeze packer 40.
- the drillpipe and/or tubing 42 may be open ended.
- FIG. 6 illustrates an embodiment comprising the placement of a cement plug across the top of well equipment, such as a fish and/or casing stub 56.
- the set-delayed cement composition 32 may be spotted through an open ended drillpipe or tubing 42.
- the bottom of the set-delayed cement composition 32 may be placed at a predetermined distance into the casing 50 and back up into the openhole section 54 above the casing stub 56.
- FIG. 7 illustrates an embodiment comprising the setting of a cementing plug utilizing a wireline 58 deployed dump bailer 60.
- the set-delayed cement composition 32 may be placed above either a fish or bridge plug 62.
- the set-delayed cement composition 32 may be pre-mixed and placed inside the dump bailer 60.
- the dump bailer 60 may then be ran to the necessary depth via wireline 58 and either dumped via a remotely operated valve located at the bottom of the dump bailer 60 or a class of ceramic disk may be broken by bumping it against the bottom of the hole.
- the dump bailer 60 may be pulled back to the surface and additional runs may be performed if necessary.
- FIG. 8 illustrates an embodiment of a standard surface rig up for a dump bailer 60 operation.
- a wireline truck 64 or skid may be utilized to lower the dump bailer 60 through the tubing connection 36 via either electric wireline 58 or slickline.
- the set-delayed cement composition may be placed utilizing coiled tubing as the means of conveyance instead of sectioned tubing.
- This means of conveyance can be utilized to perform any of the job types as described above.
- the exemplary set-delayed cement compositions disclosed herein may directly or indirectly affect one or more components or pieces of equipment associated with the preparation, delivery, recapture, recycling, reuse, and/or disposal of the disclosed set-delayed cement compositions.
- the disclosed set-delayed cement compositions may directly or indirectly affect one or more mixers, related mixing equipment, mud pits, storage facilities or units, composition separators, heat exchangers, sensors, gauges, pumps, compressors, and the like used generate, store, monitor, regulate, and/or recondition the exemplary set-delayed cement compositions.
- the disclosed set-delayed cement compositions may also directly or indirectly affect any transport or delivery equipment used to convey the set-delayed cement compositions to a well site or downhole such as, for example, any transport vessels, conduits, pipelines, trucks, tubulars, and/or pipes used to compositionally move the set-delayed cement compositions from one location to another, any pumps, compressors, or motors (e.g., topside or downhole) used to drive the set-delayed cement compositions into motion, any valves or related joints used to regulate the pressure or flow rate of the set-delayed cement compositions, and any sensors (i.e., pressure and temperature), gauges, and/or combinations thereof, and the like.
- any transport or delivery equipment used to convey the set-delayed cement compositions to a well site or downhole
- any transport vessels, conduits, pipelines, trucks, tubulars, and/or pipes used to compositionally move the set-delayed cement compositions from one location to another
- any pumps, compressors, or motors
- the disclosed set-delayed cement compositions may also directly or indirectly affect the various downhole equipment and tools that may come into contact with the set-delayed cement compositions such as, but not limited to, wellbore casing, wellbore liner, completion string, insert strings, drill string, coiled tubing, slickline, wireline, drill pipe, drill collars, mud motors, downhole motors and/or pumps, cement pumps, surface- mounted motors and/or pumps, centralizers, turbolizers, scratchers, floats (e.g., shoes, collars, valves, etc.), logging tools and related telemetry equipment, actuators (e.g., electromechanical devices, hydromechanical devices, etc.), sliding sleeves, production sleeves, plugs, screens, filters, flow control devices (e.g., inflow control devices, autonomous inflow control devices, outflow control devices, etc.), couplings (e.g., electro-hydraulic wet connect, dry connect, inductive coupler, etc.), control lines (e.g., electrical
- the composition had a density of 13.6 pounds per gallon.
- the weighting agent was Micromax ® FF weight additive available from Halliburton Energy Services, Inc., Houston, TX.
- the cement retarder was Micro Matrix ® Cement Retarder available from Halliburton Energy Services, Inc., Houston, TX.
- the dispersant was Liquiment 5581 F dispersant available from BASF, Florham Park, New Jersey.
- the viscosifier was SA-1015TM suspending agent available from Halliburton Energy Services, Inc., Houston, TX. After preparation, the rheological properties of the sample was measured using a Model 35A Fann Viscometer and a No.
- Table 3 tabulates the apparent viscosity of the composition at 100 rpm versus the composition age. The results are presented below.
- the data shows a gradual decrease in viscosity from day 2 through day 14, after which time the viscosity of the composition begins to stabilize around an average of 625 cP through day 31.
- This decline in apparent viscosity in the early going and subsequent stabilization may be advantageous for storing, mixing, and pumping the set-delayed cement composition and presents a distinctive feature in that it avoids the need for post-prep treatments such as additional dispersant or water to mitigate increasing viscosity.
- the destructive 24-hour compressive strength of the sample was measured after the addition of a 2% active liquid additive cement set activator comprising sodium sulfate, sodium hexametaphosphate, a polycarboxylated ether dispersant, and water.
- the destructive compressive strength was measured by allowing the samples to cure in a 2" by 4" plastic cylinder that was placed in a water bath at 134° F to form set cylinders. Immediately after removal from the water bath, destructive compressive strengths were determined using a mechanical press in accordance with API RP 1 OB-2, Recommended Practice for Testing Well Cements. The results of this test are set forth below in Table 4. The reported compressive strengths are an average for two cylinders of each sample.
- the destructive 24-hour compressive strength of the sample was further measured at the 21 -day mark after further curing the sample for 1 day, 3 days, or 7 days.
- the sample was activated either with the addition of a 2% active liquid additive cement set activator comprising sodium sulfate, sodium hexametaphosphate, a polycarboxylated ether dispersant, and water; or a 10% CaCh solution.
- the destructive compressive strength was measured by allowing the samples to cure in a 2" by 4" plastic cylinder that was placed in a water bath at 134° F (140° F for the 7 day sample) to form set cylinders.
- Table 6 below provides two other formulations of set-delayed cement plugging compositions and their corresponding 30-day compressive strengths (psi) and 5-day permeability (md) measurements.
- Composition A had a density of 13.5 pounds per gallon.
- Composition B had a density of 16.3 pounds per gallon.
- the cement retarder was Micro Matrix ® Cement Retarder available from Halliburton Energy Services, Inc., Houston, TX.
- the dispersant was Liquiment 5581 F dispersant available from BASF, Florham Park, New Jersey.
- the viscosifier was V-Mar ® 3 concrete rheology-modifying admixture available from W. R. Grace & Co., Cambridge, MA.
- the weighting agent was Micromax ® FF weight additive available from Halliburton Energy Services, Inc., Houston, TX.
- compositions and methods are described in terms of “comprising,” “containing,” or “including” various components or steps, the compositions and methods can also “consist essentially of or “consist of the various components and steps.
- indefinite articles “a” or “an,” as used in the claims, are defined herein to mean one or more than one of the element that it introduces.
- ranges from any lower limit may be combined with any upper limit to recite a range not explicitly recited, as well as, ranges from any lower limit may be combined with any other lower limit to recite a range not explicitly recited, in the same way, ranges from any upper limit may be combined with any other upper limit to recite a range not explicitly recited.
- any numerical range with a lower limit and an upper limit is disclosed, any number and any included range falling within the range are specifically disclosed.
- every range of values (of the form, "from about a to about b,” or, equivalently, “from approximately a to b,” or, equivalently, “from approximately a-b") disclosed herein is to be understood to set forth every number and range encompassed within the broader range of values even if not explicitly recited.
- every point or individual value may serve as its own lower or upper limit combined with any other point or individual value or any other lower or upper limit, to recite a range not explicitly recited.
Abstract
Description
Claims
Priority Applications (6)
Application Number | Priority Date | Filing Date | Title |
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MX2016005292A MX2016005292A (en) | 2013-11-26 | 2014-11-24 | Plugging and abandoning a well using a set-delayed cement composition comprising pumice. |
SG11201602947TA SG11201602947TA (en) | 2013-11-26 | 2014-11-24 | Plugging and abandoning a well using a set-delayed cement composition comprising pumice |
AU2014354935A AU2014354935B2 (en) | 2013-11-26 | 2014-11-24 | Plugging and abandoning a well using a set-delayed cement composition comprising pumice |
CA2928206A CA2928206C (en) | 2013-11-26 | 2014-11-24 | Plugging and abandoning a well using a set-delayed cement composition comprising pumice |
GB1605339.9A GB2537493B (en) | 2013-11-26 | 2014-11-24 | Plugging and abandoning a well using a set-delayed cement composition comprising pumice |
NO20160535A NO20160535A1 (en) | 2013-11-26 | 2016-04-05 | Plugging and abandoning a well using a set-delayed cement composition comprising pumice |
Applications Claiming Priority (2)
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US14/090,573 US9212534B2 (en) | 2012-03-09 | 2013-11-26 | Plugging and abandoning a well using a set-delayed cement composition comprising pumice |
US14/090,573 | 2013-11-26 |
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WO2015081014A1 true WO2015081014A1 (en) | 2015-06-04 |
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PCT/US2014/067112 WO2015081014A1 (en) | 2013-11-26 | 2014-11-24 | Plugging and abandoning a well using a set-delayed cement composition comprising pumice |
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AR (1) | AR098478A1 (en) |
AU (1) | AU2014354935B2 (en) |
CA (1) | CA2928206C (en) |
GB (1) | GB2537493B (en) |
MX (2) | MX2016005292A (en) |
NO (1) | NO20160535A1 (en) |
SG (1) | SG11201602947TA (en) |
WO (1) | WO2015081014A1 (en) |
Citations (5)
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US4676832A (en) * | 1984-10-26 | 1987-06-30 | Halliburton Company | Set delayed cement compositions and methods of using the same |
US20020162657A1 (en) * | 2001-05-04 | 2002-11-07 | Weatherford/Lamb | Method and apparatus for plugging a wellbore |
US20070289744A1 (en) * | 2006-06-20 | 2007-12-20 | Holcim (Us) Inc. | Cementitious compositions for oil well cementing applications |
US20080169100A1 (en) * | 2007-01-11 | 2008-07-17 | Halliburton Energy Services, Inc. | Methods of servicing a wellbore with compositions comprising quaternary material and sorel cements |
US20130233550A1 (en) * | 2012-03-09 | 2013-09-12 | Halliburton Energy Services, Inc. | Set-Delayed Cement Compositions Comprising Pumice and Associated Methods |
Family Cites Families (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US7743828B2 (en) * | 2005-09-09 | 2010-06-29 | Halliburton Energy Services, Inc. | Methods of cementing in subterranean formations using cement kiln cement kiln dust in compositions having reduced Portland cement content |
US8276666B2 (en) * | 2007-08-08 | 2012-10-02 | Halliburton Energy Services Inc. | Sealant compositions and methods of use |
-
2014
- 2014-11-19 AR ARP140104353A patent/AR098478A1/en active IP Right Grant
- 2014-11-24 MX MX2016005292A patent/MX2016005292A/en unknown
- 2014-11-24 SG SG11201602947TA patent/SG11201602947TA/en unknown
- 2014-11-24 CA CA2928206A patent/CA2928206C/en active Active
- 2014-11-24 GB GB1605339.9A patent/GB2537493B/en active Active
- 2014-11-24 AU AU2014354935A patent/AU2014354935B2/en active Active
- 2014-11-24 WO PCT/US2014/067112 patent/WO2015081014A1/en active Application Filing
-
2016
- 2016-04-05 NO NO20160535A patent/NO20160535A1/en unknown
- 2016-04-22 MX MX2021007696A patent/MX2021007696A/en unknown
Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4676832A (en) * | 1984-10-26 | 1987-06-30 | Halliburton Company | Set delayed cement compositions and methods of using the same |
US20020162657A1 (en) * | 2001-05-04 | 2002-11-07 | Weatherford/Lamb | Method and apparatus for plugging a wellbore |
US20070289744A1 (en) * | 2006-06-20 | 2007-12-20 | Holcim (Us) Inc. | Cementitious compositions for oil well cementing applications |
US20080169100A1 (en) * | 2007-01-11 | 2008-07-17 | Halliburton Energy Services, Inc. | Methods of servicing a wellbore with compositions comprising quaternary material and sorel cements |
US20130233550A1 (en) * | 2012-03-09 | 2013-09-12 | Halliburton Energy Services, Inc. | Set-Delayed Cement Compositions Comprising Pumice and Associated Methods |
Also Published As
Publication number | Publication date |
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GB201605339D0 (en) | 2016-05-11 |
NO20160535A1 (en) | 2016-04-05 |
GB2537493A (en) | 2016-10-19 |
MX2016005292A (en) | 2017-01-05 |
SG11201602947TA (en) | 2016-05-30 |
CA2928206C (en) | 2018-01-16 |
CA2928206A1 (en) | 2015-06-04 |
AU2014354935B2 (en) | 2017-01-12 |
GB2537493B (en) | 2018-08-08 |
AU2014354935A1 (en) | 2016-04-21 |
AR098478A1 (en) | 2016-06-01 |
MX2021007696A (en) | 2021-08-05 |
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