CN117361943A - Reinforced well cementation cement paste and application thereof - Google Patents
Reinforced well cementation cement paste and application thereof Download PDFInfo
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- CN117361943A CN117361943A CN202210779008.7A CN202210779008A CN117361943A CN 117361943 A CN117361943 A CN 117361943A CN 202210779008 A CN202210779008 A CN 202210779008A CN 117361943 A CN117361943 A CN 117361943A
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- cement
- hydrochloric acid
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- aniline
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- 239000004568 cement Substances 0.000 title claims abstract description 75
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 50
- 239000002002 slurry Substances 0.000 claims abstract description 38
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 23
- 230000002687 intercalation Effects 0.000 claims abstract description 23
- 238000009830 intercalation Methods 0.000 claims abstract description 23
- 229920000767 polyaniline Polymers 0.000 claims abstract description 23
- 239000002270 dispersing agent Substances 0.000 claims abstract description 17
- 239000013530 defoamer Substances 0.000 claims abstract description 13
- 150000001875 compounds Chemical class 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 11
- 239000000706 filtrate Substances 0.000 claims abstract description 11
- 238000002360 preparation method Methods 0.000 claims abstract description 11
- 239000003381 stabilizer Substances 0.000 claims abstract description 11
- 239000000945 filler Substances 0.000 claims abstract description 9
- 239000003129 oil well Substances 0.000 claims abstract description 9
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 32
- 229910002804 graphite Inorganic materials 0.000 claims description 27
- 239000010439 graphite Substances 0.000 claims description 27
- 239000000243 solution Substances 0.000 claims description 23
- 239000003999 initiator Substances 0.000 claims description 21
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 claims description 16
- 238000003756 stirring Methods 0.000 claims description 14
- MMCPOSDMTGQNKG-UHFFFAOYSA-N anilinium chloride Chemical compound Cl.NC1=CC=CC=C1 MMCPOSDMTGQNKG-UHFFFAOYSA-N 0.000 claims description 10
- 239000003795 chemical substances by application Substances 0.000 claims description 10
- 239000007788 liquid Substances 0.000 claims description 10
- 239000000654 additive Substances 0.000 claims description 9
- 239000011259 mixed solution Substances 0.000 claims description 9
- 239000002244 precipitate Substances 0.000 claims description 9
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 8
- 239000006185 dispersion Substances 0.000 claims description 8
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 7
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 7
- 239000002994 raw material Substances 0.000 claims description 7
- 238000000926 separation method Methods 0.000 claims description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 6
- 229920000642 polymer Polymers 0.000 claims description 6
- XHZPRMZZQOIPDS-UHFFFAOYSA-N 2-Methyl-2-[(1-oxo-2-propenyl)amino]-1-propanesulfonic acid Chemical compound OS(=O)(=O)CC(C)(C)NC(=O)C=C XHZPRMZZQOIPDS-UHFFFAOYSA-N 0.000 claims description 5
- 230000000996 additive effect Effects 0.000 claims description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 5
- -1 azodiisoheptonitrile Chemical compound 0.000 claims description 5
- 238000005119 centrifugation Methods 0.000 claims description 5
- 239000012295 chemical reaction liquid Substances 0.000 claims description 5
- 229920000536 2-Acrylamido-2-methylpropane sulfonic acid Polymers 0.000 claims description 4
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 4
- UFWIBTONFRDIAS-UHFFFAOYSA-N Naphthalene Chemical compound C1=CC=CC2=CC=CC=C21 UFWIBTONFRDIAS-UHFFFAOYSA-N 0.000 claims description 4
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 4
- 239000006229 carbon black Substances 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 230000008569 process Effects 0.000 claims description 4
- 229910021487 silica fume Inorganic materials 0.000 claims description 4
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 3
- 238000001354 calcination Methods 0.000 claims description 3
- 239000002245 particle Substances 0.000 claims description 3
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 3
- 239000000843 powder Substances 0.000 claims description 3
- LCPVQAHEFVXVKT-UHFFFAOYSA-N 2-(2,4-difluorophenoxy)pyridin-3-amine Chemical compound NC1=CC=CN=C1OC1=CC=C(F)C=C1F LCPVQAHEFVXVKT-UHFFFAOYSA-N 0.000 claims description 2
- OZAIFHULBGXAKX-UHFFFAOYSA-N 2-(2-cyanopropan-2-yldiazenyl)-2-methylpropanenitrile Chemical compound N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 claims description 2
- 239000004721 Polyphenylene oxide Substances 0.000 claims description 2
- 239000002253 acid Substances 0.000 claims description 2
- 239000011324 bead Substances 0.000 claims description 2
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 2
- 238000009833 condensation Methods 0.000 claims description 2
- 230000005494 condensation Effects 0.000 claims description 2
- 239000010881 fly ash Substances 0.000 claims description 2
- 229910052742 iron Inorganic materials 0.000 claims description 2
- ZQMHJBXHRFJKOT-UHFFFAOYSA-N methyl 2-[(1-methoxy-2-methyl-1-oxopropan-2-yl)diazenyl]-2-methylpropanoate Chemical compound COC(=O)C(C)(C)N=NC(C)(C)C(=O)OC ZQMHJBXHRFJKOT-UHFFFAOYSA-N 0.000 claims description 2
- 239000005543 nano-size silicon particle Substances 0.000 claims description 2
- JRKICGRDRMAZLK-UHFFFAOYSA-L persulfate group Chemical group S(=O)(=O)([O-])OOS(=O)(=O)[O-] JRKICGRDRMAZLK-UHFFFAOYSA-L 0.000 claims description 2
- 229920000570 polyether Polymers 0.000 claims description 2
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical group [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 2
- CHQMHPLRPQMAMX-UHFFFAOYSA-L sodium persulfate Substances [Na+].[Na+].[O-]S(=O)(=O)OOS([O-])(=O)=O CHQMHPLRPQMAMX-UHFFFAOYSA-L 0.000 claims description 2
- IRLPACMLTUPBCL-KQYNXXCUSA-N 5'-adenylyl sulfate Chemical group C1=NC=2C(N)=NC=NC=2N1[C@@H]1O[C@H](COP(O)(=O)OS(O)(=O)=O)[C@@H](O)[C@H]1O IRLPACMLTUPBCL-KQYNXXCUSA-N 0.000 claims 1
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical group [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 claims 1
- 239000010428 baryte Substances 0.000 claims 1
- 229910052601 baryte Inorganic materials 0.000 claims 1
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 claims 1
- 235000012239 silicon dioxide Nutrition 0.000 claims 1
- 238000005553 drilling Methods 0.000 abstract description 2
- 239000004575 stone Substances 0.000 description 10
- 230000000052 comparative effect Effects 0.000 description 8
- 239000007789 gas Substances 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 4
- 239000003921 oil Substances 0.000 description 4
- 239000008186 active pharmaceutical agent Substances 0.000 description 3
- 229940126062 Compound A Drugs 0.000 description 2
- NLDMNSXOCDLTTB-UHFFFAOYSA-N Heterophylliin A Natural products O1C2COC(=O)C3=CC(O)=C(O)C(O)=C3C3=C(O)C(O)=C(O)C=C3C(=O)OC2C(OC(=O)C=2C=C(O)C(O)=C(O)C=2)C(O)C1OC(=O)C1=CC(O)=C(O)C(O)=C1 NLDMNSXOCDLTTB-UHFFFAOYSA-N 0.000 description 2
- 230000035699 permeability Effects 0.000 description 2
- 230000002035 prolonged effect Effects 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 1
- 239000010755 BS 2869 Class G Substances 0.000 description 1
- 201000005488 Capillary Leak Syndrome Diseases 0.000 description 1
- 241000125183 Crithmum maritimum Species 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 208000031932 Systemic capillary leak syndrome Diseases 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005465 channeling Effects 0.000 description 1
- 239000013065 commercial product Substances 0.000 description 1
- 229940052810 complex b Drugs 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 239000007770 graphite material Substances 0.000 description 1
- 229910052595 hematite Inorganic materials 0.000 description 1
- 239000011019 hematite Substances 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- LIKBJVNGSGBSGK-UHFFFAOYSA-N iron(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Fe+3].[Fe+3] LIKBJVNGSGBSGK-UHFFFAOYSA-N 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000011541 reaction mixture Substances 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 239000011435 rock Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
-
- 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
-
- 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
- C04B2201/00—Mortars, concrete or artificial stone characterised by specific physical values
- C04B2201/20—Mortars, concrete or artificial stone characterised by specific physical values for the density
-
- 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
- C04B2201/00—Mortars, concrete or artificial stone characterised by specific physical values
- C04B2201/50—Mortars, concrete or artificial stone characterised by specific physical values for the mechanical strength
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/91—Use of waste materials as fillers for mortars or concrete
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Inorganic Chemistry (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Structural Engineering (AREA)
- Curing Cements, Concrete, And Artificial Stone (AREA)
Abstract
The invention relates to the technical field of cement slurry preparation in drilling, and discloses enhanced well cementation cement slurry and application thereof, wherein the cement slurry comprises the following components: 100 parts of cement, 4-10 parts of filtrate reducer, 0.1-0.5 part of defoamer, 5-8 parts of nano filler, 1-5 parts of polyaniline/graphene intercalation compound, 35-110 parts of water, 0-30 parts of high-temperature stabilizer, 0-200 parts of density regulator, 0-2 parts of dispersant and 0-1.5 parts of retarder. According to the reinforced well cementation cement paste provided by the invention, the polyaniline/graphene intercalation compound is added, so that the overall mechanical strength of the well cementation cement can be effectively improved, and the reinforced well cementation cement paste can be suitable for all levels of API oil well cement.
Description
Technical Field
The invention relates to the technical field of cement slurry preparation in drilling, in particular to reinforced well cementation cement slurry and application thereof.
Background
The cement slurry is a working fluid used in well cementation, and the cement slurry has the function of well cementation. The well cementation operation is to inject cement slurry into the annular space between the well wall and the casing and return the cement slurry to a certain height, and then the cement slurry becomes cement stone to solidify the well wall and the casing to form a sealing cement ring.
Conventional well cementing slurries generally consist of water, cement, additives (fluid loss additives, retarders, dispersants, etc.), and external additives (fibers, silica fume, etc.). The cement stone formed by conventional cement paste is a brittle material, and cracks or micro annular gaps are easy to appear in a cement sheath in the later production or operation process of an oil well, so that the integrity of the cement sheath is damaged, the sealing is invalid, the safety production of an oil-gas well cannot be ensured, and potential safety hazards are provided.
Therefore, it is needed to provide an enhanced well cementation cement slurry capable of improving the hard and brittle characteristics of the cement stone and improving the mechanical properties of the cement stone.
Disclosure of Invention
The invention aims to solve the problem of poor mechanical properties of cement stones in the prior art, and provides enhanced well cementation cement paste, and the overall mechanical properties (such as compressive strength and impact strength) of cement stones formed by solidifying the cement paste are greatly improved compared with those of conventional cement stones, so that the hard and brittle properties of the cement stones can be improved at high temperature and high pressure, the permeability of the cement stones is reduced, the later exploitation is ensured, and the production life of oil and gas wells is prolonged.
In order to achieve the above object, a first aspect of the present invention provides an enhanced well cementing slurry, wherein the slurry comprises: 100 parts of cement, 4-10 parts of filtrate reducer, 0.1-0.5 part of defoamer, 5-8 parts of nano filler, 1-5 parts of polyaniline/graphene intercalation compound, 35-110 parts of water, 0-30 parts of high-temperature stabilizer, 0-200 parts of density regulator, 0-2 parts of dispersant and 0-1.5 parts of retarder.
A second aspect of the invention provides the use of an enhanced cementing slurry according to the first aspect of the invention in oil well cementing.
Through the technical scheme, the beneficial technical effects obtained by the invention are as follows:
1) According to the reinforced well cementation cement paste, the polyaniline/graphene intercalation compound with good hydrophilicity is added, so that the reinforcing effect is good, the overall mechanical strength, especially the compressive strength and the impact strength of the well cementation cement can be effectively improved, the high-temperature well cementation construction requirement is met, and the reinforced well cementation cement paste can be suitable for API oil well cements of various grades;
2) The enhanced well cementation cement slurry provided by the invention has the advantages of good compatibility among the components, easiness in slurry preparation, stable performance and simple preparation method, and is suitable for industrial popularization.
Detailed Description
The endpoints and any values of the ranges disclosed herein are not limited to the precise range or value, and are understood to encompass values approaching those ranges or values. For numerical ranges, one or more new numerical ranges may be found between the endpoints of each range, between the endpoint of each range and the individual point value, and between the individual point value, in combination with each other, and are to be considered as specifically disclosed herein.
The first aspect of the present invention provides an enhanced well cementing slurry, wherein the slurry comprises: 100 parts of cement, 4-10 parts of filtrate reducer, 0.1-0.5 part of defoamer, 5-8 parts of nano filler, 1-5 parts of polyaniline/graphene intercalation compound, 35-110 parts of water, 0-30 parts of high-temperature stabilizer, 0-200 parts of density regulator, 0-2 parts of dispersant and 0-1.5 parts of retarder.
The reinforced well cementation cement paste provided by the invention has the advantages that the interaction among the components can improve the overall mechanical strength of a cement sheath formed after the cement paste is solidified, the problem of channeling of an oil and gas layer caused by the damage of impact load generated in perforation development and fracturing transformation operation to the integrity of the cement sheath is solved, the safety of later exploitation is ensured, and the production life of an oil and gas well is prolonged.
In one embodiment of the invention, the amounts of the above components may be any value within the above-defined ranges. For example, the weight parts of fluid loss additive may be any number between 4 and 10, for example, 4, 4.5, 5, 5.5, 6, 6.5, 7, 7.5, 8, 8.5, 9, 9.5, and 10, and any number in the range of any two of the foregoing numbers. The parts by weight of the defoamer may be any value between 0.1 and 0.5, for example, 0.1, 0.15, 0.2, 0.25, 0.3, 0.35, 0.4, 0.45, and 0.5, and any value in the range of any two of the above values. The parts by weight of nanofiller may be any number between 5 and 8, for example, 5, 5.5, 6, 6.5, 7, 7.5 and 8, and any value in the range of any two of the foregoing numbers. The polyaniline/graphene intercalation complex may be any number between 1 and 5 in parts by weight, for example, 1, 1.5, 2, 2.5, 3, 3.5, 4, 4.5, and 5, and any number in the range of any two of the foregoing numbers. The water may be present in any amount by weight ranging between 35 and 110, for example 35, 40, 50, 60, 70, 80, 90, 100 and 110, and any amount within the range of any two of the foregoing amounts.
In one embodiment of the invention, the fluid loss additive is one or more of 2-acrylamido-2-methylpropanesulfonic Acid (AMPS) polymer, ketoaldehyde condensation and polyvinyl alcohol (PVA) systems.
In one embodiment of the invention, the defoamer is selected from polyether defoamers.
In one embodiment of the present invention, the nanofiller is one or more selected from the group consisting of liquid nanosilica, calcium carbonate, carbon black and white carbon black.
In one embodiment of the present invention, the preparation method of the polyaniline/graphene intercalation complex includes the steps of:
1) Under the ice bath condition, firstly dispersing the expanded graphite into aniline-hydrochloric acid mixed solution, and then adding an initiator to react to obtain a reaction solution containing precipitate;
2) Adding ammonia water into the reaction liquid containing the precipitate, and then carrying out solid-liquid separation to obtain the polyaniline/graphene intercalation compound.
In step 1):
in one embodiment of the invention, the expanded graphite is a vermicular expanded graphite. The preparation method of the vermicular expanded graphite comprises the following steps: calcining the graphite raw material at 800-1000 ℃ for 30-60s to obtain vermicular expanded graphite. The graphite raw material used for preparing the vermicular expanded graphite is not particularly limited, and the graphite raw material is a conventional commercial product and can be, for example, flake graphite.
In one embodiment of the invention, the graphite material has an expansion coefficient of 15-30mL/g and a particle size of 80-1200 mesh.
In step 2):
in one embodiment of the present invention, the present invention does not particularly limit the temperature of the ice bath, and the temperature of the ice bath may be 0 to 10 ℃, preferably 0 to 5 ℃.
In one embodiment of the present invention, the method for preparing the aniline-hydrochloric acid mixed solution includes: under the ice bath condition, aniline is added into the hydrochloric acid solution, and the mixture is stirred for 10-40min at the stirring speed of 300-600rpm, so as to obtain the aniline-hydrochloric acid mixed solution.
In one embodiment of the invention, the volume ratio of aniline to hydrochloric acid solution is 1:50-100, the concentration of the hydrochloric acid solution is 0.5-2.5mol/L.
In one embodiment of the present invention, the dispersing process includes: under the ice bath condition, adding the expanded graphite into the aniline-hydrochloric acid mixed solution, firstly carrying out ultrasonic crushing for 30-90min under the ultrasonic power of 100-500W, and then stirring for 2-6h at the stirring speed of 300-600rpm to obtain a dispersion liquid; wherein the dosage ratio of the expanded graphite to the aniline is 5-15mg:1mL.
In one embodiment of the invention, the initiator is selected from azo-type initiators and/or persulphate-type initiators; wherein the azo initiator is selected from one or more of azodiisobutyronitrile, azodiisoheptonitrile, dimethyl azodiisobutyrate and azodiisobutylamidine hydrochloride; the persulphate initiator is selected from potassium persulfate, sodium persulfate and ammonium persulfate. In a further preferred embodiment, the initiator is ammonium persulfate.
In one embodiment of the invention, the mass ratio of the initiator to the expanded graphite is 1-5g:10mg.
In one embodiment of the invention, the initiator is added dropwise to the dispersion as an aqueous initiator solution, more preferably as an initiator-hydrochloric acid solution; wherein, in the initiator-hydrochloric acid solution, the dosage ratio of the initiator to the hydrochloric acid is 2-8g:100mL, and the concentration of hydrochloric acid is 0.5-2.5mol/L.
In one embodiment of the invention, the dispersion is stirred during the dropwise addition at a stirring rate of 300-600 rpm.
In one embodiment of the present invention, after the completion of the reaction (i.e., after the completion of the dropwise addition), the reaction mixture was allowed to stand at room temperature for 12 to 20 hours to obtain a reaction solution containing a precipitate.
In step 3):
in one embodiment of the present invention, the concentration of the aqueous ammonia is 1 to 3mol/L, and the volume ratio of the aqueous ammonia to the reaction liquid containing the precipitate is 1:10-50.
In one embodiment of the present invention, the present invention does not particularly limit the separation, and the separation is preferably centrifugal separation; wherein the centrifugation speed is 8000-15000rpm, and the centrifugation time is 5-10min.
According to the invention, the inventor finds that the polyaniline/graphene intercalation compound with the weight of 1-5 parts is added into cement paste, so that the compressive strength, flexural strength and other overall mechanical properties of the cement paste can be remarkably improved, the cement paste has stronger capability of resisting external load impact, the permeability can be reduced, and the tightness and safety of an oil-gas well can be improved.
In one embodiment of the invention, the purity of the water is greater than or equal to 99.5%. Wherein, in the invention, the salt content in the water is preferably less than or equal to 0.5g/L.
In one embodiment of the invention, the high temperature stabilizer is selected from microsilica or amorphous silica having a purity of 95% or more.
In one embodiment of the invention, the density modulator is a weighting agent or a lightening agent.
In one embodiment of the invention, the weighting agent is a heavy stone and/or iron ore powder, the weight fraction of which is 0-200 parts, preferably 0-50 parts.
In one embodiment of the invention, the lightening agent is fly ash and/or floating beads; the weight portion of the lightening agent is 0-100 parts, preferably 0-35 parts.
In one embodiment of the present invention, the dispersant is selected from one or more of aldehyde ketone condensates, naphthalene based dispersants, and polycarboxylic acid dispersants.
In one embodiment of the invention, the retarder is AMPS polymer.
Wherein, the filtrate reducer, the defoamer, the dispersing agent and the retarder are all conventional additives in the field. The fluid loss additive and retarder may each be independently selected from AMPS polymers, preferably the fluid loss additive and retarder are different AMPS polymers.
In one embodiment of the invention, the cement slurry is prepared by mixing the cement, the filtrate reducer, the defoamer, the nanofiller, the polyaniline/graphene intercalation composite, water, optionally a high temperature stabilizer, optionally a density regulator, optionally a dispersant and optionally a retarder to obtain the cement slurry.
A second aspect of the invention provides the use of an enhanced cementing slurry according to the first aspect of the invention in oil well cementing.
According to the reinforced well cementation cement paste provided by the invention, the polyaniline/graphene intercalation compound is added, so that the overall mechanical strength of the well cementation cement can be effectively improved, and the reinforced well cementation cement paste can be suitable for all levels of API oil well cement.
The present invention will be described in detail by examples.
The cements in examples and comparative examples were jahua class G oil well cements, purchased from the samphire cement plant, sichuan. The filtrate reducer is DZJ-Y, the defoamer is DZX-1, the dispersant is SCD-150L, the retarder is DZH-2, the nano filler is nano silicon liquid, the model is SCLS, and the filtrate reducer is from Texas land frame oil engineering Co. The high temperature stabilizer is 80 mesh silica fume from Fengyang Guangming Industrial materials Co. The graphite raw material is purchased from Qingdao rock sea carbon material Co., ltd, the expansion coefficient is 20mL/g, and the particle size is 80-1200 meshes.
Preparation example 1 (polyaniline/graphene intercalation complex)
1) Adding 2mL of aniline into 200mL of hydrochloric acid solution (1 mol/L) under the ice bath condition of 0-5 ℃ and stirring for 30min at the stirring speed of 300rpm to obtain aniline-hydrochloric acid mixed solution;
placing a graphite raw material into a muffle furnace, and calcining for 30s at 900 ℃ to obtain vermicular expanded graphite; adding 20mg of vermicular expanded graphite into the aniline-hydrochloric acid mixed solution under the ice bath condition of 0-5 ℃, firstly carrying out ultrasonic crushing for 60min under the ultrasonic power of 300W, and then carrying out stirring at the stirring speed of 300rpm for 4h to obtain a dispersion liquid;
100mL (4.56 g) of ammonium persulfate hydrochloric acid solution is dropwise added into the dispersion liquid under the ice bath condition of 0-5 ℃, the stirring speed in the dropwise adding process is 300rpm, and the reaction liquid containing dark green precipitate is obtained after the dropwise adding is finished and is kept stand for 16h at room temperature;
2) 10mL of a 2mol/L concentrated aqueous ammonia solution was added to the above reaction solution, followed by centrifugation (10000 rpm,5 min) to obtain a polyaniline/graphene intercalation complex A.
Preparation example 2
The same as in preparation example 1, except that: in the step (1), 4mL of aniline was added to 200mL of hydrochloric acid solution (1 mol/L) to obtain polyaniline/graphene intercalation complex B.
Example 1
100g of cement, 5g of filtrate reducer, 0.2g of defoamer, 5g of nano filler, 2g of polyaniline/graphene intercalation compound A, 52g of water, 30g of high-temperature stabilizer, 1.2g of dispersing agent and 0.5g of retarder are uniformly mixed to obtain enhanced well cementing slurry.
Example 2
100g of cement, 5g of filtrate reducer, 0.2g of defoamer, 5g of nano filler, 3g of polyaniline/graphene intercalation compound A, 80g of water, 30g of high-temperature stabilizer, 70g of weighting agent (hematite powder, 250 meshes), 1.2g of dispersant and 0.5g of retarder are uniformly mixed to obtain enhanced well cementing slurry.
Example 3
100g of cement, 5g of filtrate reducer, 0.2g of defoamer, 5g of nano filler, 2g of polyaniline/graphene intercalation compound B, 52g of water, 30g of high-temperature stabilizer, 1.2g of dispersing agent and 0.5g of retarder are uniformly mixed to obtain enhanced well cementing slurry.
Comparative example 1
The same as in example 1, except that polyaniline/graphene intercalation complex was not added, a well cementing slurry was obtained.
Comparative example 2
The same as in example 2, except that polyaniline/graphene intercalation complex was not added, a well cementing slurry was obtained.
The compositions and contents of the cement slurries in examples and comparative examples are shown in Table 1:
TABLE 1
Test example 1
The cement slurries obtained in the examples and comparative examples were subjected to performance tests, and the results are shown in table 2:
wherein the density was tested according to GB/T50080. The cement slurries obtained in examples and comparative examples were cured at 80℃and 20MPa for 72 hours, and then tested for compressive strength and tensile strength according to GB/T50081, and tensile strength according to GB/T50081.
TABLE 2
| Density/g/cm 3 | Compressive Strength/MPa | Tensile strength/MPa | |
| Example 1 | 1.90 | 39.7 | 4.2 |
| Example 2 | 2.25 | 29.7 | 3.4 |
| Example 3 | 1.90 | 41.1 | 4.3 |
| Comparative example 1 | 1.90 | 27.1 | 2.9 |
| Comparative example 2 | 2.25 | 20.5 | 2.2 |
As can be seen from Table 2, the reinforced well cementing slurry provided by the invention can effectively improve the overall mechanical strength of the well cementing cement by adding the polyaniline/graphene intercalation compound, and can be suitable for API oil well cements at all levels.
The preferred embodiments of the present invention have been described in detail above, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, a number of simple variants of the technical solution of the invention are possible, including combinations of the individual technical features in any other suitable way, which simple variants and combinations should likewise be regarded as being disclosed by the invention, all falling within the scope of protection of the invention.
Claims (10)
1. An enhanced cementing slurry, the slurry comprising: 100 parts of cement, 4-10 parts of filtrate reducer, 0.1-0.5 part of defoamer, 5-8 parts of nano filler, 1-5 parts of polyaniline/graphene intercalation compound, 35-110 parts of water, 0-30 parts of high-temperature stabilizer, 0-200 parts of density regulator, 0-2 parts of dispersant and 0-1.5 parts of retarder.
2. The cement slurry of claim 1, wherein the fluid loss additive is one or more of a 2-acrylamido-2-methylpropanesulfonic acid polymer, a ketoaldehyde condensation type, and a polyvinyl alcohol system;
preferably, the defoamer is selected from polyether defoamers;
preferably, the nano filler is selected from one or more of liquid nano silicon dioxide, nano titanium dioxide, calcium carbonate, carbon black and white carbon black.
3. Cement paste according to claim 1 or 2, wherein the preparation method of the polyaniline/graphene intercalation complex comprises the following steps:
1) Under the ice bath condition, firstly dispersing the expanded graphite into aniline-hydrochloric acid mixed solution, and then adding an initiator to react to obtain a reaction solution containing precipitate;
2) Adding ammonia water into the reaction liquid containing the precipitate, and then carrying out solid-liquid separation to obtain the polyaniline/graphene intercalation compound.
4. A cement slurry according to claim 3, wherein the expanded graphite is a vermicular expanded graphite;
preferably, the preparation method of the vermiform expanded graphite comprises the following steps: calcining the graphite raw material at 800-1000 ℃ for 30-60s to obtain vermicular expanded graphite;
preferably, the expansion coefficient of the graphite raw material is 15-30mL/g, and the particle size is 80-1200 meshes.
5. A cement slurry according to claim 3 or 4, wherein the method of formulating the aniline-hydrochloric acid mixture comprises: adding aniline into the hydrochloric acid solution under the ice bath condition, and stirring for 10-40min at the stirring speed of 300-600rpm to obtain aniline-hydrochloric acid mixed solution;
preferably, the volume ratio of aniline to hydrochloric acid solution is 1:50-100, the concentration of the hydrochloric acid solution is 0.5-2.5mol/L.
6. A cement slurry according to any one of claims 3 to 5, wherein the dispersing process comprises: under the ice bath condition, adding the expanded graphite into the aniline-hydrochloric acid mixed solution, firstly carrying out ultrasonic crushing for 30-90min under the ultrasonic power of 100-500W, and then stirring for 2-6h at the stirring speed of 300-600rpm to obtain a dispersion liquid; wherein the dosage ratio of the expanded graphite to the aniline is 5-15mg:1mL.
7. Cement paste according to claim 6, wherein the initiator is selected from azo-type initiators and/or persulphate-type initiators; wherein the azo initiator is selected from one or more of azodiisobutyronitrile, azodiisoheptonitrile, dimethyl azodiisobutyrate and azodiisobutylamidine hydrochloride; the persulphate initiator is selected from potassium persulfate, sodium persulfate and ammonium persulfate;
preferably, the mass ratio of the initiator to the expanded graphite is 1-5g:10mg;
preferably, the initiator is added dropwise to the dispersion as an aqueous initiator solution, more preferably as an initiator-hydrochloric acid solution; wherein, in the initiator-hydrochloric acid solution, the dosage ratio of the initiator to the hydrochloric acid solution is 2-8g:100mL, the concentration of the hydrochloric acid solution is 0.5-2.5mol/L;
preferably, during the dropping, the dispersion is stirred at a stirring rate of 300 to 600 rpm;
preferably, after the completion of the dropwise addition, the mixture is allowed to stand at room temperature for 12 to 20 hours to obtain a reaction solution containing a precipitate.
8. Cement paste according to any of claims 3-7, wherein the concentration of the aqueous ammonia is 1-3mol/L, the volume ratio of aqueous ammonia to the reaction liquid containing the precipitate is 1:10-50;
preferably, the solid-liquid separation is a centrifugal separation; wherein the centrifugation speed is 8000-15000rpm, and the centrifugation time is 5-10min.
9. Cement paste according to any one of claims 1 to 8, wherein the high temperature stabilizer is selected from microsilica or amorphous silica having a purity of 95% or more;
preferably, the density regulator is a weighting agent or a lightening agent, wherein the weighting agent is selected from barite and/or iron ore powder, and the lightening agent is selected from fly ash and/or floating beads;
preferably, the dispersant is selected from one or more of aldehyde ketone condensate, naphthalene based dispersant and polycarboxylic acid dispersant;
preferably, the retarder is AMPS polymer.
10. Use of an enhanced cementing slurry according to any one of claims 1 to 9 in oil well cementing.
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