CA2468940A1 - Resilient cement - Google Patents
Resilient cement Download PDFInfo
- Publication number
- CA2468940A1 CA2468940A1 CA002468940A CA2468940A CA2468940A1 CA 2468940 A1 CA2468940 A1 CA 2468940A1 CA 002468940 A CA002468940 A CA 002468940A CA 2468940 A CA2468940 A CA 2468940A CA 2468940 A1 CA2468940 A1 CA 2468940A1
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- CA
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- Prior art keywords
- latex
- sealing composition
- weight
- range
- present
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Abandoned
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Classifications
-
- 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
- E21B33/14—Methods or devices for cementing, for plugging holes, crevices, or the like for cementing casings into boreholes
-
- 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
- C09K8/44—Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells containing organic binders only
-
- 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
- C09K8/473—Density reducing additives, e.g. for obtaining foamed cement compositions
-
- 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
- C09K8/50—Compositions for plastering borehole walls, i.e. compositions for temporary consolidation of borehole walls
-
- 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
- C09K8/50—Compositions for plastering borehole walls, i.e. compositions for temporary consolidation of borehole walls
- C09K8/504—Compositions based on water or polar solvents
- C09K8/506—Compositions based on water or polar solvents containing organic compounds
- C09K8/508—Compositions based on water or polar solvents containing organic compounds macromolecular compounds
- C09K8/512—Compositions based on water or polar solvents containing organic compounds macromolecular compounds containing cross-linking agents
-
- 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
-
- 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
- E21B43/00—Methods or apparatus for obtaining oil, gas, water, soluble or meltable materials or a slurry of minerals from wells
- E21B43/02—Subsoil filtering
- E21B43/10—Setting of casings, screens, liners or the like in wells
- E21B43/103—Setting of casings, screens, liners or the like in wells of expandable casings, screens, liners, or the like
Abstract
A method and composition is provided for sealing a subterranean zone penetrated by a well bore, wherein the composition basically comprises a mixture of latex, dithio carbamate, zinc oxide, and sulfur.
Description
RESILIENT CEMENT
Background The present embodiment relates generally to a composition for sealing a subterranean zone penetrated by a well bore.
In the drilling and completion of an oil or gas well, a composition is often introduced in the well bore for cementing casing or pipe strings. In this process, known as "primary cementing," a composition is pumped into the annular space between the walls of the well bore and the pipe string. The composition sets in the annular space, supporting and positioning the pipe string, and forming a substantially impermeable barrier which divides the well bore into subterranean zones. After primary cementing, the undesirable migration of fluids between zones is prevented.
Likewise, compositions are often subsequently introduced into a subterranean zone for remedial operations to recover circulation or to plug the well bore. Most remedial operations comprise introducing a composition into the well bore to reestablish a seal between the zones.
Previously, a variety of cement compositions have been used for cementing.
However, cement is undesirable for use with expandable casing. After the expandable casing is placed down hole, a mandrel is run through the casing to expand the casing, and expansions up to twenty five percent are possible. As cement is incompressible, expansion of the casing can lead to crushing of the cement, and consequent loss of effectiveness regarding the zones. Therefore, a composition with comparable strength to cement, but greater elasticity and compressibility is required for cementing expandable casing.
Description A sealing composition according to the present embodiment basically comprises a mixture of latex, dithio caxbamate, zinc oxide, and sulfur, for sealing a subterranean zone penetrated by a well bore. The sulfur containing component vulcanizes the latex to form a solid mass which seals the zone.
Background The present embodiment relates generally to a composition for sealing a subterranean zone penetrated by a well bore.
In the drilling and completion of an oil or gas well, a composition is often introduced in the well bore for cementing casing or pipe strings. In this process, known as "primary cementing," a composition is pumped into the annular space between the walls of the well bore and the pipe string. The composition sets in the annular space, supporting and positioning the pipe string, and forming a substantially impermeable barrier which divides the well bore into subterranean zones. After primary cementing, the undesirable migration of fluids between zones is prevented.
Likewise, compositions are often subsequently introduced into a subterranean zone for remedial operations to recover circulation or to plug the well bore. Most remedial operations comprise introducing a composition into the well bore to reestablish a seal between the zones.
Previously, a variety of cement compositions have been used for cementing.
However, cement is undesirable for use with expandable casing. After the expandable casing is placed down hole, a mandrel is run through the casing to expand the casing, and expansions up to twenty five percent are possible. As cement is incompressible, expansion of the casing can lead to crushing of the cement, and consequent loss of effectiveness regarding the zones. Therefore, a composition with comparable strength to cement, but greater elasticity and compressibility is required for cementing expandable casing.
Description A sealing composition according to the present embodiment basically comprises a mixture of latex, dithio caxbamate, zinc oxide, and sulfur, for sealing a subterranean zone penetrated by a well bore. The sulfur containing component vulcanizes the latex to form a solid mass which seals the zone.
In a first embodiment, the composition comprises a mixture of latex, dithio carbamate, zinc oxide, sulfur and acetylenic alcohol. Preferably, the amount of Latex is maintained at a 41-90 percent ratio by weight of the composition. The dithio carbamate Is preferably present in an amount that is 0.1-2 percent of the latex by weight. The zinc oxide is preferably present in an amount that is 2-5 percent of the latex by weight. The sulfur is preferably present in an amount that is 1-4 percent of the latex by weight.
The composition may further comprise stearic acid. The stearic acid is preferably present in an amount that is 0.1-2 percent of the latex by weight.
The composition may further comprise a weighting agent. The weighting agent is preferably present in an' amount that is 0.1-150 percent of the.latex by weight.
The composition may further comprise acetylenic alcohol for defoaming, such as is available from Halliburton Energy of Duncan, Okta.,.under the trademark "D-AlR3n''s " _ The acetylene alcohol is. preferably present in an amount that is 0.001-0.2 percent of the .
latex by weight.
In a second embodiment, the composition comprises a mixture of latex, dithio carbamate, zinc oxide, sulfur, and a foaming agent, wherein the mixture is foamed.
Preferably, the .amount of.latex is maintained at a 41-90 percent ratio by weight of the composition. The dithio, carbamate is prefereably present in an amount that ~is 0.1-2 percent of the latex by.weight. The zinc oxide is preferably present in an amount that is 2-5 percent of the latex by weight. The sulfur is preferably present in an amount that is 1-4 percent of the latex by weight. The foaming agent is preferably present in an amount that is 2-4 percent by the latex by weight.
The composition may further comprise steanc acid. The stearic acid is preferably present in an amount that is 0:1-2 percent of the latex by weight.
The composition may further comprise a weighting agent. The weighting agent is .preferably present in an amount that is 0.1-150 percent of the latex by weight.
As will be understood by those skilled in the art, the Latex for either embodiment may be any of a variety of well known rubber materials commercially available which contain. unsaturation in the backbone ~ of the polymer. These include natural rubber (cis-1,4-polyisoprene), modified types thereof, synthetic polymers, and blends of the foregoing. The synthetic polymers include styrene/butadiene rubber, cis-1,4-polybutadiene, neoprene rubber, acrylonitrile styrene/butadiene rubber, and cis-1,4-polyisoprenerubber.
For either embodiment, the composition preferably includes a latex comprising a styrene/butadiene copolymer latex emulsion prepared by emulsion polymerization.
The weight ratio of styrene to butadiene in the latex can range from 10:90 to 90:10.
The emulsion is a colloidal dispersion of the copolymer. The colloidal dispersion includes water from about 40-70% by weight of the emulsion. In addition to the dispersed copolymer, the latex often includes small quantities of an emulsifier, polymerization catalysts, chain modifying agents and the like. Also, styrene/butadiene latexes are often commercially produced as terpolymer latexes which include up to about 3% by weight of a third monomer to assist in stabilizing the latex emulsions.
Non-ionic groups which exhibit stearic effects and which contain long ethoxylate or hydrocarbon tails can also be present.
Most preferably for either embodiments, the composition includes a latex with a styrene/butadiene weight ratio of about 25:75, with the styrene/butadiene copolymer suspended in a 50% by weight aqueous emulsion, available from Halliburton Energy Services of Duncan, Okla., under the trademark "LATEX 2000''M ."
The weighting agent for either embodiment may be silica flour, such as is available from Halliburton Energy Services of Duncan, Okla., under the trademark "SSA-1TM ." Alternatively, the weighting agent may be manganese oxide weighting additive, available from Halliburton Energy Services of Duncan, Okla., under the trademark "MICROMAX~ ." Alternatively, the weighting agent may be crystalline silica with an average particle size of 10 microns, available from Halliburton Energy Services of Duncan, Okla., under the trademark "MICROSANDTM ."
Dithio carbamate for either embodiment is available from Halliburton Energy Services of Duncan, under the trademark "FLEXCEM COMPONENT LTM ."
The foaming agent for the second embodiment may be an ethoxylated alcohol ether sulfate surfactant, which is available from Halliburton Energy Services of Duncan, under the trademark "ZONE SEAL 2000 ." The ZONE SEAL 2000 surfactant is the subject of U.S. Patent No. 6,063,738, the entire disclosure of which is incorporated herein as if reproduced in its entirety. Alternatively, the foaming agent may be an amidopropylbetaine surfactant, which is available from Halliburton Energy Services of Duncan, under the trademark "HC-2TM ." The HC-2TM surfactant is discussed in U.S. Patent No. 5,588,489, the entire disclosure ofwhich is incorporated herein as if reproduced in its entirety.
The following examples are illustrative of the methods and compositions discussed above.
To test curing properties of the first embodiment, 450 grams of LATEX
2000 latex, and components in the amounts listed in TABLE 1 were added to form three batches. Each of the batches was mixed in a blaring blender. The batches were poured into receptacles and incubated at the temperatures listed.
Component Batch 1 Batch 2 Batch 3 FLEXCEM
COMPONENT LTM 5.6g 5.6g 4.5g dithio carbamate Zinc Oxide 9g 9g 22.58 Sulfur 9g 9g 13.58 Stearic acid - - 9g 4.5g D-AIR3TM acetylenic 14.68 14.68 3g alcohol SSA-1TM silica flour600g 600g - -Component Batch 1 Batch 2 Batch 3 No Set; Set; Set;
Comments 48hr at 80F 48hr at 150F 5.5hr at 150F
TABLE 1 shows that the second and third batches set.
To test curing properties of the first embodiment with a different weighting agent, 100 grams of LATEX 2000 latex (with the exception of Batch 8), and components in the amounts listed in TABLE 2 (including a C~5 alcohol ethoxylated with 15 moles of ethylene oxide, which is available from Halliburton Energy Services of Duncan, under the trademark "434B ~") were added to form eight batches.
Each of the batches was mixed in a blaring blender. The batches were poured into receptacles and incubated at the temperatures listed.
Batch Batch Batch Batch Batc Batch Batch 8 Component Batch 2 3 4 h 5 6 7 (500 g latex) FLEXCEM
COMPONEN
5.6g 5.6g 0.75g 0.75g 4.5g 4.5g 1.5g 2g T LTM dithio carbamate Zinc Oxide 9g 9g 14g 14g 22.Sg 22.5g 14g 15g Sulfur 9g 9g 9g 9g 13.58 13.5g 9g lOg Stearic acid- - - - 4.5g - - - - - - - -Batch Batch Batch Batch Batc Batch Batch 8 Component Batch 2 3 4 h 6 7 (500 5 g latex) acetylenic 14.6g 14.6g 3g 3g 3g 3g - - Sg alcohol MICROMAx TM manganese 600g 600g 400g 400g 400g 400g 400g 400g oxide ( 1 S .3 lb/gal) ethoxylated - - 45g 45g 45g 45g 45g 26g lOg alcohol Set;
No set;No No set; No set;No No set;
set; set;
Latex 48hr Comments 48hr 24hr 24hr 48hr 24hr 72hr at at at at at at inverted at TABLE 2 shows that the fifth batch set without stearic acid.
To test curing properties of the second embodiment, LATEX 2000TM latex in the amounts listed in TABLES 3A and 3B, were mixed with components in the amounts listed in TABLES 3A and 3B (including a C~5 alcohol ethoxylated with moles of ethylene oxide, which is available from Halliburton Energy Services of Duncan, under the trademark "4340 ~;" a sodium salt of alpha-olefinic sulfonic acid surfactant which is discussed in U.S. Patent No. 5,588,489, the entire disclosure of which is incorporated herein as if reproduced in its entirety, and is available from _7-Halliburton Energy Services of Duncan, under the trademark "AQF-2TM;" an alcohol ether sulfate surfactant which is discussed in U.S. Patent No. 5,588,489, the entire disclosure of which is incorporated herein as if reproduced in its entirety, and is available from Halliburton Energy Services of Duncan, under the trademark "HOWCO SUDS;" and ammonium decasulfate, which is available from Halliburton Energy Services of Duncan, under the trademark "CFASTM") were added to form twelve batches. Each of the batches was mixed in a blaring blender with a sealable metal canister. The batches were poured into receptacles and incubated at the temperatures listed.
Components Batch Batch Batch Batch Batch Batch Batch LATEX
450g 450g 450g 450g 450g 600g 600g TM
latex FLEXCEM
COMPONEN
5.6g 5.6g 5.6g 5.6g 5.6g 6g 6g T LTM dithio carbamate Zinc Oxide 9g 9g 9g 9g 9g 30g 30g Sulfur 9g 9g 9g 9g 9g 18g 18g Stearic acid9g 9g 9g 9g 9g - - -aceiylenic 14.6g 14.68 - - - - - - - -alcohol SSA-1TM silica 6008 600g - - - - - - -flour _$_ Components Batch Batch Batch Batch Batch Batch Batch ZONE SEAL
2000'' 9g 18g - - 20g 20g - - - -surfactant ' MICRO SAND
TM crystalline- - - 600g 600g 600g - - -silica ethoxylated - - - - 45g 45g 45g - - - -alcohol AQF 2.LM
9g surfactant HC-2TM ' - - - - 4.Sg - - - lOg Sg surfactant HOWCO
SUDSTM _ _ _ _ _ _ _ _ _ _ _ lOg surfactant CFASTm ammonium - - - - - - - - - - - -decasulfate UnstableUnstableUnstableUnstableUnstableUnstableUnstable Comments foam foam foam foam foam foam foam Components Batch Batch Batch Batch 11 Batch 12 LATEX
600g 600g 600g 600g 675g 2OOOTM latex Components Batch Batch Batch Batch 11 Batch 12 FLEXCEM
COMPONENT
LTM di 6g 6g 6g 6g 8.4g hi t o carbamate Zinc Oxide 30g 30g 30g 30g l3.Sg Sulfur 18g 18g 18g 18g l3.Sg Stearic acid- - - - - -.- l3.Sg acetylenic - - - - - - - - -alcohol SSA-1TM silica flour ZONE SEAL
2OOOTM - __ __ _ 2pg surfactant MICROSANDT
crystalline - - - - 200g 2008 600g silica ethoxylated - - - - - - -alcohol 1 Og - - - - - - -surfactant Sg 5g 12g 20g --surfactant Components Batch Batch Batch Batch 11 Batch 12 HOWCO
SUDSTM _ _ _ - - _ _ _ -surfactant CFASTM
ammonium - - lOg - - - - -decasulfate Foamed and placed in Foamed and cell; heated to placed in cell UnstableUnstableUnstable for 2 hours; sand Conunents for 48 hours at foam foam foam settled from top 150F; set inches of 8 inch stable foam column TABLES 3A and 3B show that the eleventh and twelfth batches set.
To test curing properties of the first embodiment, 300 grams of LATEX
2000TM latex, 2 grams D-AIR3TM acetylenic alcohol, and components in the amounts listed in TABLE 4 were added to form eight batches. Each of the batches was mixed in a blaring blender. The batches were poured into receptacles and incubated in a 150°F water bath.
Batch Batch Batch Batch Batch Batch Batch Batch Component FLEXCEM
COMPONEN
3 g 3 g 3 g - - - - - - 3 g T L~ dithio carbamate Batch Batch Batch Batch Batch Batch Batch Batch Component Zinc Oxide - - 15g 15g 15g 15g - - - - - -Sulfur 9g - - 9g 9g - - 9g - - - -Stearic acid3g 3g - - 3g - - - - 3g - -Comments No No set Set No No set No No No set set set set set TABLE 4 shows that the fourth batch set.
To test shear bond properties of the first embodiment, 450 grams of LATEX
2000TM latex, 1.5 grams of FLEXCEM COMPONENT L~ dithio carbamate, 2 grams of D-AIR3TM acetylenic alcohol, and components in the amounts listed in TABLE
were added to form eight batches. Each of the batches was mixed in a blaring blender. The batches were poured into receptacles and incubated before having their shear bond strengths tested. Batches 1-4 were tested after incubation for 48 hours at 200°F. Batches 5-8 were tested after incubation for 12 days at 200°F.
In a conventional shear bond test, the batches were placed in metal cylinders with a metal bar disposed in each of the cylinders. Once a batch set, the bar was supported and positioned by the composition. Shear bond strength was determined by the force required to push the bar out of the cylinder. The shear bond testing method is conventional, and is described in a paper by L. G. Carter and G. W. Evans entitled "A Study of Cement-Pipe Bonding," presented at the Society of Petroleum Engineers California Regional Meeting, held in Santa Barbara, CA, on Oct 24-25, 1963.
Batch Batch Batch Batch Batch Batch Batch Batch Component Zinc Oxide l3.Sg l3.Sg 27g 27g l3.Sg l3.Sg l3.Sg l3.Sg Batch Batch Batch Batch Batch Batch Batch Batch Component Sulfur 9g 18g 9g 18g 9g 9g 9g 9g 600g 600g 600g 600g -- 200g 400g 600g silica flour Shear bond 21 14 psi 26 22 psi 11 28 psi 34 34 psi psi psi psi psi TABLE 5 shows that all the batches bond to metal. Batch 1 also shear bond strengths of 40 psi at 72 hours, 38 psi at 96 hours, and 55 psi at 30 days.
To test thickening times (TT) for reaching viscosities of 70 BC for the first embodiment, 600 grams of LATEX 2000TM latex, 3 grams of D-AIR3TM acetylenic alcohol, and components listed in the amounts listed in TABLE 6 were added to form ten batches. Each of the batches was mixed in a blaring blender. The batches were poured into receptacles and incubated at the temperatures listed in TABLE 6.
Bat. Bat. Bat. Bat. Bat. Bat. Sat. Bat. Bat. Bat.
Component FLEXCEM
COMPONEN
6g 0.75g0.75gl.lg 0.75g1g lg 2g - --T LTM dithio carbamate Zinc Oxide 30g 3g 6g 12g 18g 18g 18g 18g 18g 18g Sulfur 18g 12g 12g 12g 12g 12g 12g 12g 12g 12g Stearic acid6g 6g 6g 6g 6g 12g - - 12g -- -TT (hr:min) 1:39;
at 12+ 10:268:20 7:37 7:44 6:00 3:39 - - --150F 1:53 Bat. Bat. Bat. Bat. Bat. Bat. Bat. Bat. Bat. Bat.
Component TT (hr:min) at -- -- -- -- -- 1:59 1:45 1:35 6:42 11+
TABLE 6 shows that the set up times can be controlled by varying the amounts of components.
To test applied pressure for the first and second embodiments, LATEX 2000TM
latex, and components listed in the amounts listed in TABLE 7 were added to form three batches. Each of the batches was mixed in a blaring blender.
The first batch, representing the first embodiment, was poured into a test cell, which was sealed and heated to 200°F for 72 hours. After 72 hours, a valve positioned under a 325 mesh screen on the bottom of the test cell was opened, and a force of 1000 psi was applied to the test cell via a piston from the top of the cell.
After approximately an hour, the volume of the batch had reduced by an amount listed in TABLE 7.
The second batch, representing the second embodiment, was poured into a test cell, which was sealed and heated to 170°F. After 48 hours, a force of 1000 psi was applied to the test cell via a piston, and the volume of the batch had reduced by an amount listed in TABLE 7. After seven days, pressure was released, and the volume of the batch returned to 85% of its original size.
The third batch, representing the second embodiment, was poured into a test cell, heated to 170°F, and thereafter, a force of 1000 psi was applied to the test cell via a piston. The volume of the batch was reduced by an amount listed in TABLE 7.
After twenty four hours, pressure was released, and the volume of the batch returned to its original size. Thereafter, a force of 1000 psi was applied again and the volume of the batch was reduced by an amount listed in TABLE 7. After twenty four hours, pressure was again released, and the volume of the batch returned to 88% of its original size.
Batch 1 Batch 2 Batch 3 Component Non-foamed LatexSet Foamed LatexLiquid Foam Latex LATEX 2000TM 450g 600g 600g latex FLEXCEM
COMPONENT LTM l.Sg 6g 6g dithio carbamate Zinc Oxide l3.Sg 30g 30 Sulfur 9g 18g 6g HC-2TM surfactant- 20g 20g SSA-1TM silica 400g - - -flour Volume reduction30% 40% 36%
TABLE 7 shows that the first embodiment is compressible in its set state when placed against a porous geological formation, and the second embodiment is compressible in both set and unset states when placed in a sealed system.
Although only a few exemplary embodiments of this invention have been described in detail above, those skilled in the art will readily appreciate that many other modifications are possible in the exemplary embodiments without materially departing from the novel teachings and advantages of this invention.
Accordingly, all such modifications are intended to be included within the scope of this invention as defined in the following claims.
The composition may further comprise stearic acid. The stearic acid is preferably present in an amount that is 0.1-2 percent of the latex by weight.
The composition may further comprise a weighting agent. The weighting agent is preferably present in an' amount that is 0.1-150 percent of the.latex by weight.
The composition may further comprise acetylenic alcohol for defoaming, such as is available from Halliburton Energy of Duncan, Okta.,.under the trademark "D-AlR3n''s " _ The acetylene alcohol is. preferably present in an amount that is 0.001-0.2 percent of the .
latex by weight.
In a second embodiment, the composition comprises a mixture of latex, dithio carbamate, zinc oxide, sulfur, and a foaming agent, wherein the mixture is foamed.
Preferably, the .amount of.latex is maintained at a 41-90 percent ratio by weight of the composition. The dithio, carbamate is prefereably present in an amount that ~is 0.1-2 percent of the latex by.weight. The zinc oxide is preferably present in an amount that is 2-5 percent of the latex by weight. The sulfur is preferably present in an amount that is 1-4 percent of the latex by weight. The foaming agent is preferably present in an amount that is 2-4 percent by the latex by weight.
The composition may further comprise steanc acid. The stearic acid is preferably present in an amount that is 0:1-2 percent of the latex by weight.
The composition may further comprise a weighting agent. The weighting agent is .preferably present in an amount that is 0.1-150 percent of the latex by weight.
As will be understood by those skilled in the art, the Latex for either embodiment may be any of a variety of well known rubber materials commercially available which contain. unsaturation in the backbone ~ of the polymer. These include natural rubber (cis-1,4-polyisoprene), modified types thereof, synthetic polymers, and blends of the foregoing. The synthetic polymers include styrene/butadiene rubber, cis-1,4-polybutadiene, neoprene rubber, acrylonitrile styrene/butadiene rubber, and cis-1,4-polyisoprenerubber.
For either embodiment, the composition preferably includes a latex comprising a styrene/butadiene copolymer latex emulsion prepared by emulsion polymerization.
The weight ratio of styrene to butadiene in the latex can range from 10:90 to 90:10.
The emulsion is a colloidal dispersion of the copolymer. The colloidal dispersion includes water from about 40-70% by weight of the emulsion. In addition to the dispersed copolymer, the latex often includes small quantities of an emulsifier, polymerization catalysts, chain modifying agents and the like. Also, styrene/butadiene latexes are often commercially produced as terpolymer latexes which include up to about 3% by weight of a third monomer to assist in stabilizing the latex emulsions.
Non-ionic groups which exhibit stearic effects and which contain long ethoxylate or hydrocarbon tails can also be present.
Most preferably for either embodiments, the composition includes a latex with a styrene/butadiene weight ratio of about 25:75, with the styrene/butadiene copolymer suspended in a 50% by weight aqueous emulsion, available from Halliburton Energy Services of Duncan, Okla., under the trademark "LATEX 2000''M ."
The weighting agent for either embodiment may be silica flour, such as is available from Halliburton Energy Services of Duncan, Okla., under the trademark "SSA-1TM ." Alternatively, the weighting agent may be manganese oxide weighting additive, available from Halliburton Energy Services of Duncan, Okla., under the trademark "MICROMAX~ ." Alternatively, the weighting agent may be crystalline silica with an average particle size of 10 microns, available from Halliburton Energy Services of Duncan, Okla., under the trademark "MICROSANDTM ."
Dithio carbamate for either embodiment is available from Halliburton Energy Services of Duncan, under the trademark "FLEXCEM COMPONENT LTM ."
The foaming agent for the second embodiment may be an ethoxylated alcohol ether sulfate surfactant, which is available from Halliburton Energy Services of Duncan, under the trademark "ZONE SEAL 2000 ." The ZONE SEAL 2000 surfactant is the subject of U.S. Patent No. 6,063,738, the entire disclosure of which is incorporated herein as if reproduced in its entirety. Alternatively, the foaming agent may be an amidopropylbetaine surfactant, which is available from Halliburton Energy Services of Duncan, under the trademark "HC-2TM ." The HC-2TM surfactant is discussed in U.S. Patent No. 5,588,489, the entire disclosure ofwhich is incorporated herein as if reproduced in its entirety.
The following examples are illustrative of the methods and compositions discussed above.
To test curing properties of the first embodiment, 450 grams of LATEX
2000 latex, and components in the amounts listed in TABLE 1 were added to form three batches. Each of the batches was mixed in a blaring blender. The batches were poured into receptacles and incubated at the temperatures listed.
Component Batch 1 Batch 2 Batch 3 FLEXCEM
COMPONENT LTM 5.6g 5.6g 4.5g dithio carbamate Zinc Oxide 9g 9g 22.58 Sulfur 9g 9g 13.58 Stearic acid - - 9g 4.5g D-AIR3TM acetylenic 14.68 14.68 3g alcohol SSA-1TM silica flour600g 600g - -Component Batch 1 Batch 2 Batch 3 No Set; Set; Set;
Comments 48hr at 80F 48hr at 150F 5.5hr at 150F
TABLE 1 shows that the second and third batches set.
To test curing properties of the first embodiment with a different weighting agent, 100 grams of LATEX 2000 latex (with the exception of Batch 8), and components in the amounts listed in TABLE 2 (including a C~5 alcohol ethoxylated with 15 moles of ethylene oxide, which is available from Halliburton Energy Services of Duncan, under the trademark "434B ~") were added to form eight batches.
Each of the batches was mixed in a blaring blender. The batches were poured into receptacles and incubated at the temperatures listed.
Batch Batch Batch Batch Batc Batch Batch 8 Component Batch 2 3 4 h 5 6 7 (500 g latex) FLEXCEM
COMPONEN
5.6g 5.6g 0.75g 0.75g 4.5g 4.5g 1.5g 2g T LTM dithio carbamate Zinc Oxide 9g 9g 14g 14g 22.Sg 22.5g 14g 15g Sulfur 9g 9g 9g 9g 13.58 13.5g 9g lOg Stearic acid- - - - 4.5g - - - - - - - -Batch Batch Batch Batch Batc Batch Batch 8 Component Batch 2 3 4 h 6 7 (500 5 g latex) acetylenic 14.6g 14.6g 3g 3g 3g 3g - - Sg alcohol MICROMAx TM manganese 600g 600g 400g 400g 400g 400g 400g 400g oxide ( 1 S .3 lb/gal) ethoxylated - - 45g 45g 45g 45g 45g 26g lOg alcohol Set;
No set;No No set; No set;No No set;
set; set;
Latex 48hr Comments 48hr 24hr 24hr 48hr 24hr 72hr at at at at at at inverted at TABLE 2 shows that the fifth batch set without stearic acid.
To test curing properties of the second embodiment, LATEX 2000TM latex in the amounts listed in TABLES 3A and 3B, were mixed with components in the amounts listed in TABLES 3A and 3B (including a C~5 alcohol ethoxylated with moles of ethylene oxide, which is available from Halliburton Energy Services of Duncan, under the trademark "4340 ~;" a sodium salt of alpha-olefinic sulfonic acid surfactant which is discussed in U.S. Patent No. 5,588,489, the entire disclosure of which is incorporated herein as if reproduced in its entirety, and is available from _7-Halliburton Energy Services of Duncan, under the trademark "AQF-2TM;" an alcohol ether sulfate surfactant which is discussed in U.S. Patent No. 5,588,489, the entire disclosure of which is incorporated herein as if reproduced in its entirety, and is available from Halliburton Energy Services of Duncan, under the trademark "HOWCO SUDS;" and ammonium decasulfate, which is available from Halliburton Energy Services of Duncan, under the trademark "CFASTM") were added to form twelve batches. Each of the batches was mixed in a blaring blender with a sealable metal canister. The batches were poured into receptacles and incubated at the temperatures listed.
Components Batch Batch Batch Batch Batch Batch Batch LATEX
450g 450g 450g 450g 450g 600g 600g TM
latex FLEXCEM
COMPONEN
5.6g 5.6g 5.6g 5.6g 5.6g 6g 6g T LTM dithio carbamate Zinc Oxide 9g 9g 9g 9g 9g 30g 30g Sulfur 9g 9g 9g 9g 9g 18g 18g Stearic acid9g 9g 9g 9g 9g - - -aceiylenic 14.6g 14.68 - - - - - - - -alcohol SSA-1TM silica 6008 600g - - - - - - -flour _$_ Components Batch Batch Batch Batch Batch Batch Batch ZONE SEAL
2000'' 9g 18g - - 20g 20g - - - -surfactant ' MICRO SAND
TM crystalline- - - 600g 600g 600g - - -silica ethoxylated - - - - 45g 45g 45g - - - -alcohol AQF 2.LM
9g surfactant HC-2TM ' - - - - 4.Sg - - - lOg Sg surfactant HOWCO
SUDSTM _ _ _ _ _ _ _ _ _ _ _ lOg surfactant CFASTm ammonium - - - - - - - - - - - -decasulfate UnstableUnstableUnstableUnstableUnstableUnstableUnstable Comments foam foam foam foam foam foam foam Components Batch Batch Batch Batch 11 Batch 12 LATEX
600g 600g 600g 600g 675g 2OOOTM latex Components Batch Batch Batch Batch 11 Batch 12 FLEXCEM
COMPONENT
LTM di 6g 6g 6g 6g 8.4g hi t o carbamate Zinc Oxide 30g 30g 30g 30g l3.Sg Sulfur 18g 18g 18g 18g l3.Sg Stearic acid- - - - - -.- l3.Sg acetylenic - - - - - - - - -alcohol SSA-1TM silica flour ZONE SEAL
2OOOTM - __ __ _ 2pg surfactant MICROSANDT
crystalline - - - - 200g 2008 600g silica ethoxylated - - - - - - -alcohol 1 Og - - - - - - -surfactant Sg 5g 12g 20g --surfactant Components Batch Batch Batch Batch 11 Batch 12 HOWCO
SUDSTM _ _ _ - - _ _ _ -surfactant CFASTM
ammonium - - lOg - - - - -decasulfate Foamed and placed in Foamed and cell; heated to placed in cell UnstableUnstableUnstable for 2 hours; sand Conunents for 48 hours at foam foam foam settled from top 150F; set inches of 8 inch stable foam column TABLES 3A and 3B show that the eleventh and twelfth batches set.
To test curing properties of the first embodiment, 300 grams of LATEX
2000TM latex, 2 grams D-AIR3TM acetylenic alcohol, and components in the amounts listed in TABLE 4 were added to form eight batches. Each of the batches was mixed in a blaring blender. The batches were poured into receptacles and incubated in a 150°F water bath.
Batch Batch Batch Batch Batch Batch Batch Batch Component FLEXCEM
COMPONEN
3 g 3 g 3 g - - - - - - 3 g T L~ dithio carbamate Batch Batch Batch Batch Batch Batch Batch Batch Component Zinc Oxide - - 15g 15g 15g 15g - - - - - -Sulfur 9g - - 9g 9g - - 9g - - - -Stearic acid3g 3g - - 3g - - - - 3g - -Comments No No set Set No No set No No No set set set set set TABLE 4 shows that the fourth batch set.
To test shear bond properties of the first embodiment, 450 grams of LATEX
2000TM latex, 1.5 grams of FLEXCEM COMPONENT L~ dithio carbamate, 2 grams of D-AIR3TM acetylenic alcohol, and components in the amounts listed in TABLE
were added to form eight batches. Each of the batches was mixed in a blaring blender. The batches were poured into receptacles and incubated before having their shear bond strengths tested. Batches 1-4 were tested after incubation for 48 hours at 200°F. Batches 5-8 were tested after incubation for 12 days at 200°F.
In a conventional shear bond test, the batches were placed in metal cylinders with a metal bar disposed in each of the cylinders. Once a batch set, the bar was supported and positioned by the composition. Shear bond strength was determined by the force required to push the bar out of the cylinder. The shear bond testing method is conventional, and is described in a paper by L. G. Carter and G. W. Evans entitled "A Study of Cement-Pipe Bonding," presented at the Society of Petroleum Engineers California Regional Meeting, held in Santa Barbara, CA, on Oct 24-25, 1963.
Batch Batch Batch Batch Batch Batch Batch Batch Component Zinc Oxide l3.Sg l3.Sg 27g 27g l3.Sg l3.Sg l3.Sg l3.Sg Batch Batch Batch Batch Batch Batch Batch Batch Component Sulfur 9g 18g 9g 18g 9g 9g 9g 9g 600g 600g 600g 600g -- 200g 400g 600g silica flour Shear bond 21 14 psi 26 22 psi 11 28 psi 34 34 psi psi psi psi psi TABLE 5 shows that all the batches bond to metal. Batch 1 also shear bond strengths of 40 psi at 72 hours, 38 psi at 96 hours, and 55 psi at 30 days.
To test thickening times (TT) for reaching viscosities of 70 BC for the first embodiment, 600 grams of LATEX 2000TM latex, 3 grams of D-AIR3TM acetylenic alcohol, and components listed in the amounts listed in TABLE 6 were added to form ten batches. Each of the batches was mixed in a blaring blender. The batches were poured into receptacles and incubated at the temperatures listed in TABLE 6.
Bat. Bat. Bat. Bat. Bat. Bat. Sat. Bat. Bat. Bat.
Component FLEXCEM
COMPONEN
6g 0.75g0.75gl.lg 0.75g1g lg 2g - --T LTM dithio carbamate Zinc Oxide 30g 3g 6g 12g 18g 18g 18g 18g 18g 18g Sulfur 18g 12g 12g 12g 12g 12g 12g 12g 12g 12g Stearic acid6g 6g 6g 6g 6g 12g - - 12g -- -TT (hr:min) 1:39;
at 12+ 10:268:20 7:37 7:44 6:00 3:39 - - --150F 1:53 Bat. Bat. Bat. Bat. Bat. Bat. Bat. Bat. Bat. Bat.
Component TT (hr:min) at -- -- -- -- -- 1:59 1:45 1:35 6:42 11+
TABLE 6 shows that the set up times can be controlled by varying the amounts of components.
To test applied pressure for the first and second embodiments, LATEX 2000TM
latex, and components listed in the amounts listed in TABLE 7 were added to form three batches. Each of the batches was mixed in a blaring blender.
The first batch, representing the first embodiment, was poured into a test cell, which was sealed and heated to 200°F for 72 hours. After 72 hours, a valve positioned under a 325 mesh screen on the bottom of the test cell was opened, and a force of 1000 psi was applied to the test cell via a piston from the top of the cell.
After approximately an hour, the volume of the batch had reduced by an amount listed in TABLE 7.
The second batch, representing the second embodiment, was poured into a test cell, which was sealed and heated to 170°F. After 48 hours, a force of 1000 psi was applied to the test cell via a piston, and the volume of the batch had reduced by an amount listed in TABLE 7. After seven days, pressure was released, and the volume of the batch returned to 85% of its original size.
The third batch, representing the second embodiment, was poured into a test cell, heated to 170°F, and thereafter, a force of 1000 psi was applied to the test cell via a piston. The volume of the batch was reduced by an amount listed in TABLE 7.
After twenty four hours, pressure was released, and the volume of the batch returned to its original size. Thereafter, a force of 1000 psi was applied again and the volume of the batch was reduced by an amount listed in TABLE 7. After twenty four hours, pressure was again released, and the volume of the batch returned to 88% of its original size.
Batch 1 Batch 2 Batch 3 Component Non-foamed LatexSet Foamed LatexLiquid Foam Latex LATEX 2000TM 450g 600g 600g latex FLEXCEM
COMPONENT LTM l.Sg 6g 6g dithio carbamate Zinc Oxide l3.Sg 30g 30 Sulfur 9g 18g 6g HC-2TM surfactant- 20g 20g SSA-1TM silica 400g - - -flour Volume reduction30% 40% 36%
TABLE 7 shows that the first embodiment is compressible in its set state when placed against a porous geological formation, and the second embodiment is compressible in both set and unset states when placed in a sealed system.
Although only a few exemplary embodiments of this invention have been described in detail above, those skilled in the art will readily appreciate that many other modifications are possible in the exemplary embodiments without materially departing from the novel teachings and advantages of this invention.
Accordingly, all such modifications are intended to be included within the scope of this invention as defined in the following claims.
Claims (54)
1. A method of sealing a subterranean zone penetrated by a well bore comprising:
preparing a sealing composition comprising latex, dithio carbamate, zinc oxide, sulfur and acetylenic alcohol, placing the sealing composition into the subterranean zone; and allowing the sealing composition to set therein.
preparing a sealing composition comprising latex, dithio carbamate, zinc oxide, sulfur and acetylenic alcohol, placing the sealing composition into the subterranean zone; and allowing the sealing composition to set therein.
2. The method of claim 1 wherein the latex is a styrene/butadiene copolymer latex emulsion.
3. The method of claim 2 wherein the latex has a styrene/butadiene weight ratio of about 25:75, with the styrene/butadiene copolymer suspended in a 50% by weight aqueous emulsion.
4. The method of claim 1 wherein the latex is present in a range of 41% to 90%
by weight of the sealing composition.
by weight of the sealing composition.
5. The method of claim 1 wherein the dithio carbamate is present in a range of 0.1% to 2% by weight of the latex in the sealing composition.
6. The method of claim 1 wherein the zinc oxide is present in a range of 2% to 5%
by weight of the latex in the sealing composition.
by weight of the latex in the sealing composition.
7. The method of claim 1 wherein the sulfur is present in a range of 1% to 4%
by weight of the latex in the sealing composition.
by weight of the latex in the sealing composition.
8. The method of claim 1 wherein the sealing composition further comprises stearic acid.
9. The method of claim 8 wherein the stearic acid is present in a range of 0.1% to 2% by weight of the latex in the sealing composition.
10. The method of claim 1 wherein the sealing composition further comprises a weighting agent.
11. The method of claim 10 wherein the weighting agent is present in a range of 0.1% to 150% by weight of the latex in the sealing composition.
12. The method of claim 1 wherein the acetylenic alcohol is present in a range of 0.001% to 0.2% by weight of the latex in the sealing composition.
13. The method of claim 1 wherein the sealing composition further comprises a foaming agent.
14. The method of claim 13 wherein the foaming agent is present in a range of 2% to 4% by weight of the latex in the sealing composition.
15. A composition for sealing a subterranean zone penetrated by a well bore comprising: latex, dithio carbamate, zinc oxide, sulfur and acetylenic alcohol.
16. The sealing composition of claim 15 wherein the latex is a styrene/butadiene copolymer latex emulsion.
17. The sealing composition of claim 16 wherein the latex has a styrene/butadiene weight ratio of about 25:75, with the styrene/butadiene copolymer suspended in a 50%
by weight aqueous emulsion.
by weight aqueous emulsion.
18. The sealing composition of claim 15 wherein the latex is present in a range of 41% to 90% by weight of the sealing composition.
19. The sealing composition of claim 15 wherein the dithio carbamate is present in a range of 0.1% to 2% by weight of the latex in the sealing composition.
20. The sealing composition of claim 15 wherein the zinc oxide is present in a range of 2% to 5% by weight of the latex in the sealing composition.
21. The sealing composition of claim 15 wherein the sulfur is present in a range of 1% to 4% by weight of the latex in the sealing composition.
22. The sealing composition of claim 15 further comprising stearic acid.
23. The sealing composition of claim 22 wherein the stearic acid is present in a range of 0.1% to 2% by weight of the latex in the sealing composition.
24. The sealing composition of claim 15 further comprising a weighting agent.
25. The sealing composition of claim 24 wherein the weighting agent is present in a range of 0.1% to 150% by weight of the latex in the sealing composition.
26. The sealing composition of claim 15 wherein the acetylenic alcohol is present in a range of 0.001% to 0.2% by weight of the latex in the sealing composition.
27. The sealing composition of claim 15 further comprising a foaming agent.
28. The sealing composition of claim 27 wherein the foaming agent is present in a range of 2% to 4% by weight of the latex in the sealing composition.
29. A method of sealing a subterranean zone penetrated by a well bore comprising:
preparing a sealing composition consisting essentially of latex, ditho carbamate, zinc oxide, and sulfur; placing the sealing composition into the subterranean zone;
and allowing the sealing composition to set therein.
preparing a sealing composition consisting essentially of latex, ditho carbamate, zinc oxide, and sulfur; placing the sealing composition into the subterranean zone;
and allowing the sealing composition to set therein.
30. The method of claim 29 wherein the latex is a styrene/butadiene copolymer latex emulsion.
31. The method of claim 30 wherein the latex has a styrene/butadiene weight ratio of about 25:75, with the styrene/butadiene copolymer suspended in a 50% by weight aqueous emulsion.
32. The method of claim 29 wherein the latex is present in a range of 41% to 90% by weight of the sealing composition.
33. The method of claim 29 wherein the dithio carbamate is present in a range of 0.1% to 2% by weight of the latex in the sealing composition.
34. The method of claim 29 wherein the zinc oxide is present in a range of 2%
to 5%
by weight of the latex in the sealing composition.
to 5%
by weight of the latex in the sealing composition.
35. The method of claim 29 wherein the sulfur is present in a range of 1% to 4% by weight of the latex in the sealing composition.
36. The method of claim 29 wherein the sealing composition further consists essentially of stearic acid.
37. The method of claim 36 wherein the stearic acid is present in a range of 0.1% to 2% by weight of the latex in the sealing composition.
38. The method of claim 29 wherein the sealing composition further consists essentially of a weighting agent.
39. The method of claim 38 wherein the weighting agent is present in a range of 0.1% to 150% by weight of the latex in the sealing composition.
40. The method of claim 29 wherein the sealing composition further consists essentially of a foaming agent.
41. The method of claim 40 wherein the foaming agent is present in a range of 2% to 4% by weight of the latex in the sealing composition.
42. A composition for sealing a subterranean zone penetrated by a well bore consisting essentially of latex, dithio carbamate, zinc oxide, and sulfur.
43. The sealing composition of claim 42 wherein the latex is a styrene/butadiene copolymer latex emulsion.
44. The sealing composition of claim 43 wherein the latex has a styrene/butadiene weight ratio of about 25:75, with the styrene/butadiene copolymer suspended in a 50%
by weight aqueous emulsion.
by weight aqueous emulsion.
45. The sealing composition of claim 42 wherein the latex is present in a range of 41% to 90% by weight of the sealing composition.
46. The sealing composition of claim 42 wherein the dithio carbamate is present in a range of 0.1% to 2% by weight of the latex in the sealing composition.
47. The sealing composition of claim 42 wherein the zinc oxide is present in a range of 2% to %% by weight of the latex in the sealing composition.
48. The sealing composition of claim 42 wherein the sulfur is present in a range of 1% to 4% by weight of the latex in the sealing composition.
49. The sealing composition of claim 42 further consisting essentially of stearic acid.
50. The sealing composition of claim 49 wherein the stearic acid is present in a range of 0.1% to 2% by weight of the latex in the sealing composition.
51. The sealing composition of claim 42 further consisting essentially of a weighting agent.
52. The sealing composition of claim 51 wherein the weighting agent is preset in a range of 0.1% to 150% by weight of the latex in the sealing composition.
53. The sealing composition of claim 42 further consisting essentially of a foaming agent.
54. The sealing composition of claim 53 wherein the foaming agent is present in a range of 2% to 4% by weight of the latex in the sealing composition.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US10/006,109 | 2001-12-04 | ||
| US10/006,109 US6668928B2 (en) | 2001-12-04 | 2001-12-04 | Resilient cement |
| PCT/GB2002/005447 WO2003048515A1 (en) | 2001-12-04 | 2002-12-02 | Resilient cement |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CA2468940A1 true CA2468940A1 (en) | 2003-06-12 |
Family
ID=21719353
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CA002468940A Abandoned CA2468940A1 (en) | 2001-12-04 | 2002-12-02 | Resilient cement |
Country Status (8)
| Country | Link |
|---|---|
| US (1) | US6668928B2 (en) |
| EP (1) | EP1451441A1 (en) |
| AU (1) | AU2002349152A1 (en) |
| CA (1) | CA2468940A1 (en) |
| DE (1) | DE60228991D1 (en) |
| MX (1) | MXPA04005438A (en) |
| NO (1) | NO20042726L (en) |
| WO (1) | WO2003048515A1 (en) |
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| US6271181B1 (en) | 1999-02-04 | 2001-08-07 | Halliburton Energy Services, Inc. | Sealing subterranean zones |
| US6328106B1 (en) | 1999-02-04 | 2001-12-11 | Halliburton Energy Services, Inc. | Sealing subterranean zones |
| US6234251B1 (en) | 1999-02-22 | 2001-05-22 | Halliburton Energy Services, Inc. | Resilient well cement compositions and methods |
| MXPA01010126A (en) | 1999-04-09 | 2002-04-24 | Shell Int Research | Method for annular sealing. |
-
2001
- 2001-12-04 US US10/006,109 patent/US6668928B2/en not_active Expired - Fee Related
-
2002
- 2002-11-29 DE DE60228991T patent/DE60228991D1/en not_active Expired - Lifetime
- 2002-12-02 WO PCT/GB2002/005447 patent/WO2003048515A1/en not_active Application Discontinuation
- 2002-12-02 EP EP02781431A patent/EP1451441A1/en not_active Withdrawn
- 2002-12-02 AU AU2002349152A patent/AU2002349152A1/en not_active Abandoned
- 2002-12-02 MX MXPA04005438A patent/MXPA04005438A/en not_active Application Discontinuation
- 2002-12-02 CA CA002468940A patent/CA2468940A1/en not_active Abandoned
-
2004
- 2004-06-29 NO NO20042726A patent/NO20042726L/en not_active Application Discontinuation
Also Published As
| Publication number | Publication date |
|---|---|
| NO20042726L (en) | 2004-06-29 |
| MXPA04005438A (en) | 2004-10-11 |
| WO2003048515A1 (en) | 2003-06-12 |
| AU2002349152A1 (en) | 2003-06-17 |
| EP1451441A1 (en) | 2004-09-01 |
| DE60228991D1 (en) | 2008-10-30 |
| US20030121659A1 (en) | 2003-07-03 |
| US6668928B2 (en) | 2003-12-30 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| EEER | Examination request | ||
| FZDE | Discontinued |