US20210108122A1 - Cross-linked plugging agent stimulated by high density brine and preparing method thereof - Google Patents
Cross-linked plugging agent stimulated by high density brine and preparing method thereof Download PDFInfo
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- US20210108122A1 US20210108122A1 US17/131,737 US202017131737A US2021108122A1 US 20210108122 A1 US20210108122 A1 US 20210108122A1 US 202017131737 A US202017131737 A US 202017131737A US 2021108122 A1 US2021108122 A1 US 2021108122A1
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- plugging agent
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- 239000012267 brine Substances 0.000 title claims abstract description 42
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 title claims abstract description 42
- 238000000034 method Methods 0.000 title claims description 16
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 144
- 239000003349 gelling agent Substances 0.000 claims abstract description 42
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 31
- LWIHDJKSTIGBAC-UHFFFAOYSA-K potassium phosphate Substances [K+].[K+].[K+].[O-]P([O-])([O-])=O LWIHDJKSTIGBAC-UHFFFAOYSA-K 0.000 claims abstract description 24
- ZPWVASYFFYYZEW-UHFFFAOYSA-L dipotassium hydrogen phosphate Chemical compound [K+].[K+].OP([O-])([O-])=O ZPWVASYFFYYZEW-UHFFFAOYSA-L 0.000 claims abstract description 12
- 229910000396 dipotassium phosphate Inorganic materials 0.000 claims abstract description 12
- 229910000402 monopotassium phosphate Inorganic materials 0.000 claims abstract description 12
- 229910000404 tripotassium phosphate Inorganic materials 0.000 claims abstract description 12
- 238000002474 experimental method Methods 0.000 claims abstract description 10
- 235000019797 dipotassium phosphate Nutrition 0.000 claims abstract description 7
- 235000019796 monopotassium phosphate Nutrition 0.000 claims abstract description 7
- AJPJDKMHJJGVTQ-UHFFFAOYSA-M sodium dihydrogen phosphate Chemical compound [Na+].OP(O)([O-])=O AJPJDKMHJJGVTQ-UHFFFAOYSA-M 0.000 claims abstract description 7
- 235000019798 tripotassium phosphate Nutrition 0.000 claims abstract description 7
- 239000000230 xanthan gum Substances 0.000 claims abstract description 7
- 229920001285 xanthan gum Polymers 0.000 claims abstract description 7
- 235000010493 xanthan gum Nutrition 0.000 claims abstract description 7
- 229940082509 xanthan gum Drugs 0.000 claims abstract description 7
- 239000007836 KH2PO4 Substances 0.000 claims abstract description 6
- ZNOZWUKQPJXOIG-XSBHQQIPSA-L [(2r,3s,4r,5r,6s)-6-[[(1r,3s,4r,5r,8s)-3,4-dihydroxy-2,6-dioxabicyclo[3.2.1]octan-8-yl]oxy]-4-[[(1r,3r,4r,5r,8s)-8-[(2s,3r,4r,5r,6r)-3,4-dihydroxy-6-(hydroxymethyl)-5-sulfonatooxyoxan-2-yl]oxy-4-hydroxy-2,6-dioxabicyclo[3.2.1]octan-3-yl]oxy]-5-hydroxy-2-( Chemical compound O[C@@H]1[C@@H](O)[C@@H](OS([O-])(=O)=O)[C@@H](CO)O[C@H]1O[C@@H]1[C@@H]2OC[C@H]1O[C@H](O[C@H]1[C@H]([C@@H](CO)O[C@@H](O[C@@H]3[C@@H]4OC[C@H]3O[C@H](O)[C@@H]4O)[C@@H]1O)OS([O-])(=O)=O)[C@@H]2O ZNOZWUKQPJXOIG-XSBHQQIPSA-L 0.000 claims abstract description 6
- PJNZPQUBCPKICU-UHFFFAOYSA-N phosphoric acid;potassium Chemical compound [K].OP(O)(O)=O PJNZPQUBCPKICU-UHFFFAOYSA-N 0.000 claims abstract description 6
- GNSKLFRGEWLPPA-UHFFFAOYSA-M potassium dihydrogen phosphate Chemical compound [K+].OP(O)([O-])=O GNSKLFRGEWLPPA-UHFFFAOYSA-M 0.000 claims abstract description 6
- RYCLIXPGLDDLTM-UHFFFAOYSA-J tetrapotassium;phosphonato phosphate Chemical compound [K+].[K+].[K+].[K+].[O-]P([O-])(=O)OP([O-])([O-])=O RYCLIXPGLDDLTM-UHFFFAOYSA-J 0.000 claims abstract description 6
- 238000001879 gelation Methods 0.000 claims description 43
- 238000003756 stirring Methods 0.000 claims description 3
- 239000012530 fluid Substances 0.000 description 16
- 230000035699 permeability Effects 0.000 description 13
- 230000032683 aging Effects 0.000 description 10
- 239000007789 gas Substances 0.000 description 10
- 230000005484 gravity Effects 0.000 description 8
- BDAGIHXWWSANSR-UHFFFAOYSA-M Formate Chemical compound [O-]C=O BDAGIHXWWSANSR-UHFFFAOYSA-M 0.000 description 7
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 6
- 230000015556 catabolic process Effects 0.000 description 6
- 238000006731 degradation reaction Methods 0.000 description 6
- 239000008187 granular material Substances 0.000 description 6
- 239000000243 solution Substances 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 4
- 239000012065 filter cake Substances 0.000 description 4
- 229920000642 polymer Polymers 0.000 description 4
- 238000011084 recovery Methods 0.000 description 4
- JHJLBTNAGRQEKS-UHFFFAOYSA-M sodium bromide Chemical compound [Na+].[Br-] JHJLBTNAGRQEKS-UHFFFAOYSA-M 0.000 description 4
- VNDYJBBGRKZCSX-UHFFFAOYSA-L zinc bromide Chemical compound Br[Zn]Br VNDYJBBGRKZCSX-UHFFFAOYSA-L 0.000 description 4
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 description 4
- 230000008901 benefit Effects 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 229910000019 calcium carbonate Inorganic materials 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000006073 displacement reaction Methods 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 150000003839 salts Chemical class 0.000 description 3
- CPELXLSAUQHCOX-UHFFFAOYSA-M Bromide Chemical compound [Br-] CPELXLSAUQHCOX-UHFFFAOYSA-M 0.000 description 2
- 229920002134 Carboxymethyl cellulose Polymers 0.000 description 2
- 229920002873 Polyethylenimine Polymers 0.000 description 2
- -1 ZnBr2 compound Chemical class 0.000 description 2
- ATZQZZAXOPPAAQ-UHFFFAOYSA-M caesium formate Chemical compound [Cs+].[O-]C=O ATZQZZAXOPPAAQ-UHFFFAOYSA-M 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000005553 drilling Methods 0.000 description 2
- 239000000706 filtrate Substances 0.000 description 2
- 238000011010 flushing procedure Methods 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 231100000647 material safety data sheet Toxicity 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000011592 zinc chloride Substances 0.000 description 2
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical class [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 description 1
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical class [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 238000000418 atomic force spectrum Methods 0.000 description 1
- 239000002981 blocking agent Substances 0.000 description 1
- SXDBWCPKPHAZSM-UHFFFAOYSA-M bromate Inorganic materials [O-]Br(=O)=O SXDBWCPKPHAZSM-UHFFFAOYSA-M 0.000 description 1
- SXDBWCPKPHAZSM-UHFFFAOYSA-N bromic acid Chemical compound OBr(=O)=O SXDBWCPKPHAZSM-UHFFFAOYSA-N 0.000 description 1
- WGEFECGEFUFIQW-UHFFFAOYSA-L calcium dibromide Chemical compound [Ca+2].[Br-].[Br-] WGEFECGEFUFIQW-UHFFFAOYSA-L 0.000 description 1
- 239000001768 carboxy methyl cellulose Substances 0.000 description 1
- 235000010948 carboxy methyl cellulose Nutrition 0.000 description 1
- 239000008112 carboxymethyl-cellulose Substances 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- WYYQVWLEPYFFLP-UHFFFAOYSA-K chromium(3+);triacetate Chemical compound [Cr+3].CC([O-])=O.CC([O-])=O.CC([O-])=O WYYQVWLEPYFFLP-UHFFFAOYSA-K 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 230000002860 competitive effect Effects 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 239000003431 cross linking reagent Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000007667 floating Methods 0.000 description 1
- 239000008398 formation water Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- WFIZEGIEIOHZCP-UHFFFAOYSA-M potassium formate Chemical compound [K+].[O-]C=O WFIZEGIEIOHZCP-UHFFFAOYSA-M 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000010079 rubber tapping Methods 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 230000008719 thickening Effects 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
- 235000005074 zinc chloride Nutrition 0.000 description 1
Images
Classifications
-
- 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
-
- 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
- C04B28/34—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 cold phosphate binders
- C04B28/344—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 cold phosphate binders the phosphate binder being present in the starting composition solely as one or more phosphates
-
- 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
- C09K8/50—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
-
- 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
- C09K8/516—Compositions for plastering borehole walls, i.e. compositions for temporary consolidation of borehole walls characterised by their form or by the form of their components, e.g. encapsulated material
-
- E—FIXED CONSTRUCTIONS
- E21—EARTH OR ROCK DRILLING; MINING
- E21B—EARTH OR ROCK 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
- the present invention relates to oilfield chemistry, which is widely applied in well completion and workover under high temperature, high pressure, multi-pressure oil and gas environment and is applied in temporary blocking agent, perforating protect fluid and water shutoff agent.
- the present invention is more particularly related to the cross-linked plugging agent stimulated by high density brine and the preparing method thereof.
- the high density killing fluid would leak into the low-pressure reservoir if the differential of pressure is bigger than the pressure bearing limitation of the reservoir.
- the fluid loss results in more requirements of killing fluid to keep the pressure, which increases the cost. In serious condition, the fluid loss damages the reservoir and reduces the outcome. In an even more serious condition, the fluid loss induces safety risk.
- the plugging and leak-prevention technology for high-density well killing fluid is critical in workover and well completion operations under high temperature and multi-pressure environment.
- plugging agent can deal with compatibility and floating problem caused by high density killing fluid used in workover and well completion operations in high pressure formation.
- the plugging agent is able to meet the requirements such as high temperature and salt endurance, easy to prepare, controllable plugging strength, low cost and environmentally friendly.
- the conventional preparing method of the high density plugging agent applied on site falls into the below two categories.
- haloid which is mainly Zinc bromide (ZnBr 2 ), Zinc chloride (ZnCl 2 ), Sodium bromide (NaBr), Calcium bromide (CaBr 2 ), Calcium chloride (CaCl 2 ) and so on, which is still an important technical objective for different big drilling fluid companies to reach and related research is carried out due to lack of corresponding strategy for deep reservoir.
- Technical contests are carried out and each company has its own formula which is well-kept secret. Although each company has its own production code and product naming convention, the research theory and technology adopted is similar.
- Zhiliang Zhou uses sulfonated phenolic resin (SMP-II), calcium carbonate (CaCO 3 ), carboxymethyl cellulose (CMC) and so on with ZnBr 2 to prepare high density low damage plugging agent;
- Kexiang Peng uses SMP-II, sulfonated wood coal (SMC), sulfonated resin modified filtrate reducer GJL-1 and GJL-2 with ZnBr 2 compound to prepare filtrate reducing high density plugging agent.
- Haloid especially bromide solution is highly corrosive under high temperature and high density environment and difficult to degrade, which accumulates in food chain and is not environmentally friendly. Environment protection is more and more urgent than ever before and the conventional bromide high density plugging agent is gradually replaced by new low damage and pollution plugging agent.
- Two types of plugging agents prepared based on formate are used in large scale.
- One is thickening plugging agent which is prepared by adding polymer into the formate water system to increase viscosity of the killing fluid and to reduce killing fluid filtration and loss in the low permeability reservoir, such as 4 mate series of acrylamide-sulfonated methyl propane copolymer system, xanthan gum system, CMC system and etc. produced by Cabot Corporation.
- the application of this type of plugging agent is limited and this type of plugging agent is not able to be used under high pressure difference.
- the other type is bridge plugging agent.
- the plugging agent dissolves in the formate water system to form small granules.
- One or more sizes of small granules form a bridge on the fluid loss formation, such as fine mesh calcium carbonate, modified graphite “G-Seal”, which is a mixture of, various cellulose and high strength granules.
- G-Seal modified graphite
- the size of the granule is important. If the size of the granule is not selected carefully, the granules easily enter the reservoir and damage the reservoir.
- the plugging agent prepared based on formate has the advantages of wide density range and effectively protecting the reservoir, the price of the formate especially cesium formate is much higher than halide salt, which restrict the use of the plugging agent.
- An object of the present invention is to provide a cross-linked plugging agent stimulated by high density brine and preparing method thereof.
- the present invention adopts the main agent to stimulate the gelling agent to cross link without the extra use of other crosslinking agents such as phenol formaledlyde, chromium (III) acetate and polyethyleneimine (PEI).
- the present invention of the cross-linked plugging agent stimulated by high density brine and the preparing method thereof is able to be applied in operations under high temperature, high pressure, multi-pressure series of strata oil and gas environment when temporary blockage and leak proof is required, protection of reservoir near perforations and water plugging.
- the advantages of the plugging agent of the present invention are being able to be easily prepared on site, controllable gelation time and degradation time under high temperature and high salt density, and rapid core permeability recovery after flowback.
- the present invention provide the below technical solution.
- the cross-linked plugging agent stimulated by high density brine comprising:
- main agent 10 wt %-90 wt %
- gelling agent 0.5 wt %-9 wt % and pure water.
- cross-linked plugging agent stimulated by high density brine further comprises main agent of 30 wt %-70 wt %.
- the main agent is selected from the group consisting of a Dipotassium phosphate (K 2 HPO 4 ), a Tripotassium phosphate (K 3 PO 4 ), and a Potassium pyrophosphate (K 4 P 2 O 7 ).
- the main agent further comprises a Potassium Dihydrogen Phosphate (KH 2 PO 4 ), a Sodium dihydrogen phosphate (NaH 2 PO 4 )
- the gelling agent is selected from the group consisting of a Xanthan gum and a kappa carrageenan.
- the process of preparing a cross-linked plugging agent stimulated by high density brine comprises the following steps of:
- the main agent dissolves in the pure water and releases large quantity of ions; the ions and the gelling agent cross linked to form covalent bonds; the molecular chains of various gelling agents are entangled to form compound synergist; hydrogen bond is formed between the molecular of the plugging agent and the water molecular and the plugging agent system obtains water absorption feature.
- the three type of reactions work together to form the cross-linked plugging agent stimulated by high density brine.
- the components in the cross-linked plugging agent stimulated by high density brine do not need to be prepared in advance.
- the plugging agent is able to be prepared on site conveniently and the process is easy to be carried out.
- the main agent dissolves in the pure water to form brine which stimulates the gelling agent to induce a cross linking reaction and form a cross-linked plugging agent by compound synergy.
- the cross-linked plugging agent is able to endure high temperature and density salt and the gelation strength is controllable.
- the gelation time and gelation strength is decided according to the Gel Strength Codes (GSC) proposed by Sydansk and Argabright in 1988.
- GSC Gel Strength Codes
- the gelation time is decided by observing the gel forms.
- the initial gelation time refers to the period while the form of the gelling agent changing from no detachable gel (A) to highly flowing gel (B).
- the final gelation time refers to the period while the form of the gelling agent changing from original polymer solution to the final strength. Normally, the gelation time refers to the period when most of the gelling agent flows to the bottle cap by gravity upon inversion (C).
- the thermal stability of the cross-linked plugging agent stimulated by high density is good. All components of the plugging agent are innoxious and harmless. The degradation of the plugging agent is controllable. The corrosion of the oil tubing and casing by the plugging agent is little. The plugging agent is able to be widely applied in operations such as well completion and workover when temporary blockage and leak proof is required, protection of reservoir near perforations and water shutoff and profile control under high temperature, high pressure, multi pressure series of strata oil and gas environment.
- the present invention has the following benefits:
- MSDS material safety data sheet
- the cross-linked plugging agent stimulated by high density brine is applied in a temperature range 90° C.-160° C.; the gelation time is controlled within 0.5-12 hours; the final gelation strength is controllable within GSC C to H; the plugging agent is controllable for degradation within 20-168 hours after the plugging task is completed.
- the viscosity of the plugging agent is less than 100 mPa ⁇ s before gelation and the pumpability is good; the plugging agent system is a solid-free fluid after degradation, the viscosity of which is less than 50 mPa ⁇ s; the plugging agent is able to be discharged in well flushing cycle without residue and effectively protect the reservoir.
- FIG. 1 illustrates values of elastic modulus and loss modulus in embodiment 1 of various gelling agent content after aging for three days;
- FIG. 2 is a curve chart which displays viscosity and shear force of the plugging agent with 2 wt % of gelling agent content at the initial time, after two days and after five days in embodiment 2;
- FIG. 3 is a shear viscosity curve chart of a cross-linked plugging agent stimulated by high density brine under different temperature in embodiment 6;
- FIG. 4 is an elastic modulus curve chart of the cross-linked plugging agent stimulated by high density brine under different temperature in embodiment 7;
- FIG. 5 is a loss modulus curve chart of the cross-linked plugging agent stimulated by high density brine under different temperature in embodiment 7;
- FIG. 6 is a curve chart which displays flowback time and core permeability recovery rate in embodiment 8.
- a cross-linked plugging agent stimulated by high density brine comprises:
- main agent 10 wt %-90 wt %
- gelling agent 0.5 wt %-9 wt % and pure water.
- the main agent is selected from the group consisting of a Dipotassium phosphate (K 2 HPO 4 ), a Tripotassium phosphate (K 3 PO 4 ) and a Potassium pyrophosphate (K 4 P 2 O 7 ),
- the main agent further comprises a Potassium Dihydrogen Phosphate (KH 2 PO 4 ) and a Sodium dihydrogen phosphate (NaH 2 PO 4 ),
- the gelling agent is selected from the group consisting of a Xanthan gum and a kappa carrageenan.
- the cross-linked plugging agent stimulated by the high density brine is able to be applied in well completion and workover under high temperature, high pressure, multi pressure series of strata oil and gas environment when temporary blockage and leak proof is required, protection of reservoir near perforations and water plugging, which is exclusively designed according to geological characteristics of the reservoir, well temperature and plugging agent consumption.
- the plugging agent is prepared by the following steps of: adding main agent, gelling agent into pure water in sequence with respective percentage by mass; stirring evenly; setting an experiment temperature at 90° C.-160° C.; and determining a gelation time and a gelation strength of the plugging agent by gel strength codes.
- a cross-linked plugging agent stimulated by high density brine for temporary blockage comprises the mixture of main agent of 70 wt %, gelling agent of 5 wt %-8 wt % and pure water.
- the experiment temperature is 120° C.
- the gelation time and a gelation strength are shown in the below table 2.
- the gelation time is within 2-4 hours; the final forming strength is G; no syneresis happens within 12 days.
- the values of elastic modulus and loss modulus of various gelling agent content after aging for three days prove that the strength of the plugging agent is able to be adjusted by adjusting the gelling agent content.
- a cross-linked plugging agent stimulated by high density brine for protection of reservoir near perforations comprises main agent of 70 wt %, gelling agent of 1.5 wt %-3 wt % and pure water.
- the experiment temperature is 160° C.
- the gelation time and a gelation strength are shown in the below Table 3.
- the gelation time is within 4-8 hours; the final forming strength is D or E; syneresis and degradation occur on the third day; the plugging agent degrades to solid-free and low viscosity fluid 48 hours after syneresis begins.
- the viscosity and shear force curve of the plugging agent with 2 wt % of gelling agent content at the initial time, after two days and after five days illustrates the viscosity of the plugging agent at the initial time is below 100 mPa ⁇ s and is able to be pumped easily; the viscosity of the plugging agent increases significantly after two days and the plugging agent is high viscosity liquid; the plugging agent degrades to solid-free fluid after five days and the viscosity is below 50 mPa ⁇ s, which is able to be discharged in well flushing cycle without gel breaking.
- a cross-linked plugging agent stimulated by high density brine for temporary blockage comprises main agent of 70 wt %, gelling agent of 6 wt %-8 wt % and pure water.
- the experiment temperature is 90° C.
- the gelation time and a gelation strength are shown in the below table 4.
- the gelation time is within 2-4 hours; the final forming strength is F, G or H; no syneresis happens within 7 days.
- the plugging agent is able to be applied in temporary blockage and water plugging when different gel strength is required.
- a cross-linked plugging agent stimulated by high density brine for protection of reservoir near perforations comprises main agent of 70 wt %, gelling agent of 2.5 wt %-4 wt % and pure water.
- the experiment temperature is 90° C.
- the gelation time and a gelation strength are shown in the below table 5.
- the gelation time is within 2-4 hours; the final forming strength is C, D or E; no syneresis happens within 7 days.
- the plugging agent is able to be applied in protection of reservoir near perforations when different gel strength is required.
- a cross-linked plugging agent stimulated by high density brine for temporary blockage comprises main agent of 70 wt %, gelling agent of 5 wt %-8 wt % and pure water.
- the experiment temperature is 90° C.
- the gelation time and a gelation strength are shown in the below table 6.
- the gelation time is within 2-4 hours; the final forming strength is C, D or E; no syneresis happens within 7 days.
- the plugging agent is able to be applied in temporary blockage and water plugging when different gel strength is required.
- the formula of the plugging agent stimulated by high density brine in the embodiment is the main agent which density is 1.5 g/cm 3 and gelling agent of 3 wt %.
- the prepared plugging agent is put into a laboratory oven ageing for four hours under 90° C., 120° C., 140° C., and 160° C. respectively.
- the plugging agent is assumed to be pumped to reservoir in four hours.
- FIG. 3 shows the viscosities of the plugging agent when the plugging agent passes through the casing or oil tube and reaches the target place.
- the viscosity of the plugging agent sample decrease with the rising temperature after ageing for four hours, which reaches a magnitude of 10 4 mPa ⁇ s.
- the plugging agent is in a semi-solid status, which does not easily loss in the reservoir and is able to bear pressure.
- the formula of the plugging agent stimulated by high density brine in the embodiment is the main agent which density is 1.5 g/cm 3 and gelling agent of 6 wt %.
- the prepared plugging agent is put into a laboratory oven ageing for four hours under 90° C., 120° C., 140° C., and 160° C. respectively.
- the observed elastic and loss modulus are shown in the FIG. 4 and FIG. 5 .
- the elastic modulus reaches the magnitude of 10 3 Pa and the gel strength is high enough to fulfill the requirement for temporary blockage and leak-proof task under pressure difference (no fluid loss in the reservoir under 20 MPa pressure difference after temporary blockage shown in embodiment 8).
- the formula of the plugging agent stimulated by high density brine in the embodiment is the main agent which density is 1.5 g/cm 3 and gelling agent of 6 wt %.
- the core (with saturated formation water) is put in an integrated displacement equipment.
- Sufficient plugging agent stimulated by high density brine covers a front end of the simulated well casing. Pure water is injected on the plugging agent stimulated by high density brine to simulate the working fluid. Pressure is applied on the front end of the core to simulate the pressure difference on the well casing.
- the chart 7 shows the observed the fluid loss from a back end of the core.
- K gi(dry) stands for the gas permeability of the dry core
- K gi(Swc) stands for the gas permeability at irreducible water saturation S wc .
- filter cake After being blocked for two hours under a pressure difference of 20 MPa, filter cake forms on the contact surface of the core and the gelling agent.
- the filter cake prevents the gelling agent from leak deep into the core (no more than 3 mm-5 mm) and fluid loss.
- the permeability is able to be rapidly recovered after the filter cake is being removed.
- Chart 8 and FIG. 6 show the permeability recovery of the flowback after the blockage. After the being blocked for two hours under a pressure difference of 20 MPa, the filter cake on the front end of the core is being removed, the core is put in the displacement equipment and the displacement is reversed by gas to simulate the well cleaning process during the flowback and the induced flow of the reservoir. The experiment result shows: the permeability is able to recover to 80% of permeability before the blockage after the reservoir being blocked under 20 MPa and the flow is induced under 3 MPa negative pressure difference.
- K gi(Swc) stands for the gas permeability at irreducible water saturation S wc .
- K gf stands for the gas permeability after flowback breakthrough by air.
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Abstract
The present invention disclosed a cross-linked plugging agent stimulated by high density brine which comprises main agent: 10 wt %-90 wt %, gelling agent: 0.5 wt %-9 wt % and pure water; wherein the main agent is selected from the group consisting of a Dipotassium phosphate (K2HPO4), a Tripotassium phosphate (K3PO4) and a Potassium pyrophosphate (K4P2O7), a Potassium Dihydrogen Phosphate (KH2PO4), a Sodium dihydrogen phosphate (NaH2PO4); the gelling agent is selected from the group consisting of a Xanthan gum and a kappa carrageenan. The gelling time is controlled within 0.5-12 h under an experiment temperature of 90° C.-160° C. The final gelling strength is controlled within D-H. The density is controlled within 1.0-1.55 g/cm3. The plugging agent is able to be applied in well completion and workover under high temperature, high pressure, multi-pressure series of strata oil and gas environment when temporary blockage and leak proof is required, protection of reservoir near perforations and water plugging.
Description
- This is a Continuation Application of the International Application PCT/CN2020/076004, filed Feb. 2, 2020, which claims priority under 35 U.S.C. 119(a-d) to CN 202010094980.1, filed Feb. 17, 2020.
- The present invention relates to oilfield chemistry, which is widely applied in well completion and workover under high temperature, high pressure, multi-pressure oil and gas environment and is applied in temporary blocking agent, perforating protect fluid and water shutoff agent. The present invention is more particularly related to the cross-linked plugging agent stimulated by high density brine and the preparing method thereof.
- The reservoir development goes deeper and deeper to reach deep and ultra-deep formation where the geological condition is complicate and prone to change. Many challenges and difficulties need to be dealt with such as high temperature, high pressure, multi-pressure environment in reservoir, blowout and fluid loss. In case of drilling a well with ultra high pressure, the contradiction of well killing and fluid loss in low-pressure reservoir is the main technical difficulty which results in high cost during well completion and workover. According to the conventional principles, in case of multi-pressure oil and gas reservoir with ultra high pressure, well killing fluid is planned in advance and the killing fluid is selected based on the principle of ‘the pressure of killing fluid need to be higher than reservoir’. The high density killing fluid column brings high positive pressure on the low-pressure reservoir when the well control requirement is fulfilled. The high density killing fluid would leak into the low-pressure reservoir if the differential of pressure is bigger than the pressure bearing limitation of the reservoir. The fluid loss results in more requirements of killing fluid to keep the pressure, which increases the cost. In serious condition, the fluid loss damages the reservoir and reduces the outcome. In an even more serious condition, the fluid loss induces safety risk. The plugging and leak-prevention technology for high-density well killing fluid is critical in workover and well completion operations under high temperature and multi-pressure environment.
- Well completion and workover in the high temperature and multi-pressure reservoir requires high performance plugging agent. On one hand, the plugging agent can deal with compatibility and floating problem caused by high density killing fluid used in workover and well completion operations in high pressure formation. On the other hand, the plugging agent is able to meet the requirements such as high temperature and salt endurance, easy to prepare, controllable plugging strength, low cost and environmentally friendly.
- The conventional preparing method of the high density plugging agent applied on site falls into the below two categories.
- (1) One of the conventional preparing method of plugging agent for high temperature and pressure well killing is based on haloid which is mainly Zinc bromide (ZnBr2), Zinc chloride (ZnCl2), Sodium bromide (NaBr), Calcium bromide (CaBr2), Calcium chloride (CaCl2) and so on, which is still an important technical objective for different big drilling fluid companies to reach and related research is carried out due to lack of corresponding strategy for deep reservoir. Technical contests are carried out and each company has its own formula which is well-kept secret. Although each company has its own production code and product naming convention, the research theory and technology adopted is similar. For example, Zhiliang Zhou uses sulfonated phenolic resin (SMP-II), calcium carbonate (CaCO3), carboxymethyl cellulose (CMC) and so on with ZnBr2 to prepare high density low damage plugging agent; Kexiang Peng uses SMP-II, sulfonated wood coal (SMC), sulfonated resin modified filtrate reducer GJL-1 and GJL-2 with ZnBr2 compound to prepare filtrate reducing high density plugging agent. Haloid especially bromide solution is highly corrosive under high temperature and high density environment and difficult to degrade, which accumulates in food chain and is not environmentally friendly. Environment protection is more and more urgent than ever before and the conventional bromide high density plugging agent is gradually replaced by new low damage and pollution plugging agent.
- (2) Plugging agent prepared based on formate.
- Two types of plugging agents prepared based on formate (mainly potassium formate, cesium formate and etc.) are used in large scale. One is thickening plugging agent which is prepared by adding polymer into the formate water system to increase viscosity of the killing fluid and to reduce killing fluid filtration and loss in the low permeability reservoir, such as 4 mate series of acrylamide-sulfonated methyl propane copolymer system, xanthan gum system, CMC system and etc. produced by Cabot Corporation. The application of this type of plugging agent is limited and this type of plugging agent is not able to be used under high pressure difference. The other type is bridge plugging agent. The plugging agent dissolves in the formate water system to form small granules. One or more sizes of small granules form a bridge on the fluid loss formation, such as fine mesh calcium carbonate, modified graphite “G-Seal”, which is a mixture of, various cellulose and high strength granules. The size of the granule is important. If the size of the granule is not selected carefully, the granules easily enter the reservoir and damage the reservoir. Although the plugging agent prepared based on formate has the advantages of wide density range and effectively protecting the reservoir, the price of the formate especially cesium formate is much higher than halide salt, which restrict the use of the plugging agent.
- An object of the present invention is to provide a cross-linked plugging agent stimulated by high density brine and preparing method thereof. The present invention adopts the main agent to stimulate the gelling agent to cross link without the extra use of other crosslinking agents such as phenol formaledlyde, chromium (III) acetate and polyethyleneimine (PEI). The present invention of the cross-linked plugging agent stimulated by high density brine and the preparing method thereof is able to be applied in operations under high temperature, high pressure, multi-pressure series of strata oil and gas environment when temporary blockage and leak proof is required, protection of reservoir near perforations and water plugging. The advantages of the plugging agent of the present invention are being able to be easily prepared on site, controllable gelation time and degradation time under high temperature and high salt density, and rapid core permeability recovery after flowback.
- To solve the problems of the conventional technology, the present invention provide the below technical solution.
- The cross-linked plugging agent stimulated by high density brine, comprising:
- main agent: 10 wt %-90 wt %, gelling agent: 0.5 wt %-9 wt % and pure water.
- wherein the cross-linked plugging agent stimulated by high density brine further comprises main agent of 30 wt %-70 wt %.
- Furthermore, the main agent is selected from the group consisting of a Dipotassium phosphate (K2HPO4), a Tripotassium phosphate (K3PO4), and a Potassium pyrophosphate (K4P2O7).
- Furthermore, the main agent further comprises a Potassium Dihydrogen Phosphate (KH2PO4), a Sodium dihydrogen phosphate (NaH2PO4)
- Furthermore, the gelling agent is selected from the group consisting of a Xanthan gum and a kappa carrageenan.
- The process of preparing a cross-linked plugging agent stimulated by high density brine comprises the following steps of:
- adding main agent, gelling agent into pure water in sequence with respective percentage by mass; stirring evenly; setting an experiment temperature at 90° C.-160° C.; controlling the gelation time within 0.5-12 hours; determining the gelation time and the gelation strength of the plugging agent by gel strength codes. The final forming strength is controlled within flowing gel (gel strength code C) to slightly deformation non flowing gel (gel strength code H). The density of the plugging agent system is able to be controlled within 1.0-1.55 g/cm3.
- Three type of reactions occur as below: the main agent dissolves in the pure water and releases large quantity of ions; the ions and the gelling agent cross linked to form covalent bonds; the molecular chains of various gelling agents are entangled to form compound synergist; hydrogen bond is formed between the molecular of the plugging agent and the water molecular and the plugging agent system obtains water absorption feature. The three type of reactions work together to form the cross-linked plugging agent stimulated by high density brine.
- The components in the cross-linked plugging agent stimulated by high density brine do not need to be prepared in advance. The plugging agent is able to be prepared on site conveniently and the process is easy to be carried out. The main agent dissolves in the pure water to form brine which stimulates the gelling agent to induce a cross linking reaction and form a cross-linked plugging agent by compound synergy. The cross-linked plugging agent is able to endure high temperature and density salt and the gelation strength is controllable.
- The gelation time and gelation strength is decided according to the Gel Strength Codes (GSC) proposed by Sydansk and Argabright in 1988. The gelation time is decided by observing the gel forms. The initial gelation time refers to the period while the form of the gelling agent changing from no detachable gel (A) to highly flowing gel (B). The final gelation time refers to the period while the form of the gelling agent changing from original polymer solution to the final strength. Normally, the gelation time refers to the period when most of the gelling agent flows to the bottle cap by gravity upon inversion (C).
-
TABLE 1 Gel Strength Codes Gel strength code Gel name Gel description A No detectable gel No detectable gel formed: The gel appears to have the same viscosity as the original polymer solution B Highly flowing The gel appears to be only slightly more viscous than gel the initial polymer solution C Flowing gel Most of the gel flows to the bottle cap by gravity upon inversion D Moderately Only a small portion (<15%) of the gel dose not flow to flowing gel the bottle by gravity upon inversion (usually characterized as tonguing gel) E Barely flowing The gel can barely flow to the bottle cap and or a gel significant portion (>15%) of the gel does not flow by gravity upon inversion F Highly The gel does not flow to the bottle cap by gravity upon deformable non inversion flowing gel G Moderately The gel deforms about half way down the bottle by deformable non gravity upon inversion flowing gel H Slightly Only the gel surface slightly deforms by gravity upon deformable non inversion flowing gel I Rigid gel There is no gel surface deformation by gravity upon inversion J Ringing rigid gel A tuning fork-like mechanical vibration can be felt upon tapping the bottle - The thermal stability of the cross-linked plugging agent stimulated by high density is good. All components of the plugging agent are innoxious and harmless. The degradation of the plugging agent is controllable. The corrosion of the oil tubing and casing by the plugging agent is little. The plugging agent is able to be widely applied in operations such as well completion and workover when temporary blockage and leak proof is required, protection of reservoir near perforations and water shutoff and profile control under high temperature, high pressure, multi pressure series of strata oil and gas environment.
- Compared to the conventional technology, the present invention has the following benefits:
- (1) all the components are instant soluble, easy to prepare and operate;
- (2) the costs of all the components is lower than bromate plugging agent and formate plugging agent and the plugging agent is price competitive.
- (3) the material safety data sheet (MSDS) of each component fulfils the requirements for food; the plugging agent is innoxious, harmless, corrosion-free and non pollutive; the degradation of the plugging agent is controllable; the plugging agent is oil casing friendly and ecofriendly;
- (4) the cross-linked plugging agent stimulated by high density brine is applied in a
temperature range 90° C.-160° C.; the gelation time is controlled within 0.5-12 hours; the final gelation strength is controllable within GSC C to H; the plugging agent is controllable for degradation within 20-168 hours after the plugging task is completed. - (5) the viscosity of the plugging agent is less than 100 mPa·s before gelation and the pumpability is good; the plugging agent system is a solid-free fluid after degradation, the viscosity of which is less than 50 mPa·s; the plugging agent is able to be discharged in well flushing cycle without residue and effectively protect the reservoir.
-
FIG. 1 illustrates values of elastic modulus and loss modulus inembodiment 1 of various gelling agent content after aging for three days; -
FIG. 2 is a curve chart which displays viscosity and shear force of the plugging agent with 2 wt % of gelling agent content at the initial time, after two days and after five days in embodiment 2; -
FIG. 3 is a shear viscosity curve chart of a cross-linked plugging agent stimulated by high density brine under different temperature inembodiment 6; -
FIG. 4 is an elastic modulus curve chart of the cross-linked plugging agent stimulated by high density brine under different temperature inembodiment 7; -
FIG. 5 is a loss modulus curve chart of the cross-linked plugging agent stimulated by high density brine under different temperature inembodiment 7; -
FIG. 6 is a curve chart which displays flowback time and core permeability recovery rate inembodiment 8. - The below embodiments further explain the present invention. The embodiments are based on the present invention and give detailed explanation. The protection scope of the present invention does not limited by the below embodiments.
- A cross-linked plugging agent stimulated by high density brine comprises:
- main agent: 10 wt %-90 wt %, gelling agent: 0.5 wt %-9 wt % and pure water.
- The main agent is selected from the group consisting of a Dipotassium phosphate (K2HPO4), a Tripotassium phosphate (K3PO4) and a Potassium pyrophosphate (K4P2O7),
- wherein the main agent further comprises a Potassium Dihydrogen Phosphate (KH2PO4) and a Sodium dihydrogen phosphate (NaH2PO4),
- The gelling agent is selected from the group consisting of a Xanthan gum and a kappa carrageenan.
- The cross-linked plugging agent stimulated by the high density brine is able to be applied in well completion and workover under high temperature, high pressure, multi pressure series of strata oil and gas environment when temporary blockage and leak proof is required, protection of reservoir near perforations and water plugging, which is exclusively designed according to geological characteristics of the reservoir, well temperature and plugging agent consumption. The plugging agent is prepared by the following steps of: adding main agent, gelling agent into pure water in sequence with respective percentage by mass; stirring evenly; setting an experiment temperature at 90° C.-160° C.; and determining a gelation time and a gelation strength of the plugging agent by gel strength codes.
- A cross-linked plugging agent stimulated by high density brine for temporary blockage comprises the mixture of main agent of 70 wt %, gelling agent of 5 wt %-8 wt % and pure water. The experiment temperature is 120° C. The gelation time and a gelation strength are shown in the below table 2.
-
TABLE 2 gelation time and a gelation strength in embodiment 1Gelling agent Aging time/gel strength code content Wt % Initial 2 h 4 h 12 h 1 D 3 D 5 D 7 D 9 D 12 D 5 A D G G G G G G G G 7 A D G G G G G G G G 8 A D G G G G G G G G - As shown in Table 2, the gelation time is within 2-4 hours; the final forming strength is G; no syneresis happens within 12 days.
- As shown in
FIG. 1 , the values of elastic modulus and loss modulus of various gelling agent content after aging for three days prove that the strength of the plugging agent is able to be adjusted by adjusting the gelling agent content. - A cross-linked plugging agent stimulated by high density brine for protection of reservoir near perforations comprises main agent of 70 wt %, gelling agent of 1.5 wt %-3 wt % and pure water. The experiment temperature is 160° C. The gelation time and a gelation strength are shown in the below Table 3.
-
TABLE 3 gelation time and a gelation strength in embodiment 2 Gelling agent Aging time/gel strength code content Wt % Initial 4 h 8 h 1 D 2 D 3 D 4 D 1.5 A B D D D D A syneresis 2 A B D D D D D syneresis 2.5 A B E E E E E syneresis 3 A B E E E E E - As shown in table 3, the gelation time is within 4-8 hours; the final forming strength is D or E; syneresis and degradation occur on the third day; the plugging agent degrades to solid-free and low viscosity fluid 48 hours after syneresis begins.
- As shown in
FIG. 2 , the viscosity and shear force curve of the plugging agent with 2 wt % of gelling agent content at the initial time, after two days and after five days illustrates the viscosity of the plugging agent at the initial time is below 100 mPa·s and is able to be pumped easily; the viscosity of the plugging agent increases significantly after two days and the plugging agent is high viscosity liquid; the plugging agent degrades to solid-free fluid after five days and the viscosity is below 50 mPa·s, which is able to be discharged in well flushing cycle without gel breaking. - A cross-linked plugging agent stimulated by high density brine for temporary blockage comprises main agent of 70 wt %, gelling agent of 6 wt %-8 wt % and pure water. The experiment temperature is 90° C. The gelation time and a gelation strength are shown in the below table 4.
-
TABLE 4 gelation time and a gelation strength in embodiment 3 Gelling agent Aging time/gel strength code content Wt % Initial 2 h 4 h 12 h 1 D 3 D 5 D 7 D 9 D 12 D 6 A D F F F F F F F F 7 A D F G G G G G G G 8 A D G H H H H H H H - As shown in table 4, the gelation time is within 2-4 hours; the final forming strength is F, G or H; no syneresis happens within 7 days. The plugging agent is able to be applied in temporary blockage and water plugging when different gel strength is required.
- A cross-linked plugging agent stimulated by high density brine for protection of reservoir near perforations comprises main agent of 70 wt %, gelling agent of 2.5 wt %-4 wt % and pure water. The experiment temperature is 90° C. The gelation time and a gelation strength are shown in the below table 5.
-
TABLE 5 gelation time and a gelation strength in embodiment 4 Gelling agent Aging time/gel strength code content Wt % Initial 2 h 4 h 12 h 1 D 3 D 5 D 7 D 9 D 12 D 2.5 A A B B B C C C C C 3 A A C D D D D D D D 3.5 A B D E E E E E E E 4 A C D E E E E E E E - As shown in table 5, the gelation time is within 2-4 hours; the final forming strength is C, D or E; no syneresis happens within 7 days. The plugging agent is able to be applied in protection of reservoir near perforations when different gel strength is required.
- A cross-linked plugging agent stimulated by high density brine for temporary blockage comprises main agent of 70 wt %, gelling agent of 5 wt %-8 wt % and pure water. The experiment temperature is 90° C. The gelation time and a gelation strength are shown in the below table 6.
-
TABLE 6 gelation time and a gelation strength in embodiment 5Gelling agent Aging time/gel strength code content Wt % Initial 2 h 4 h 12 h 1 D 3 D 5 D 7 D 9 D 12 D 5 A D F F G G G G G G 6 A D F G G G G G H H 7 A E G H H H H H H H 8 A F H H H H H H H H - As shown in table 6, the gelation time is within 2-4 hours; the final forming strength is C, D or E; no syneresis happens within 7 days. The plugging agent is able to be applied in temporary blockage and water plugging when different gel strength is required.
- The formula of the plugging agent stimulated by high density brine in the embodiment is the main agent which density is 1.5 g/cm3 and gelling agent of 3 wt %. The prepared plugging agent is put into a laboratory oven ageing for four hours under 90° C., 120° C., 140° C., and 160° C. respectively. The plugging agent is assumed to be pumped to reservoir in four hours.
FIG. 3 shows the viscosities of the plugging agent when the plugging agent passes through the casing or oil tube and reaches the target place. The viscosity of the plugging agent sample decrease with the rising temperature after ageing for four hours, which reaches a magnitude of 104 mPa·s. The plugging agent is in a semi-solid status, which does not easily loss in the reservoir and is able to bear pressure. - The formula of the plugging agent stimulated by high density brine in the embodiment is the main agent which density is 1.5 g/cm3 and gelling agent of 6 wt %. The prepared plugging agent is put into a laboratory oven ageing for four hours under 90° C., 120° C., 140° C., and 160° C. respectively. The observed elastic and loss modulus are shown in the
FIG. 4 andFIG. 5 . The elastic modulus reaches the magnitude of 103 Pa and the gel strength is high enough to fulfill the requirement for temporary blockage and leak-proof task under pressure difference (no fluid loss in the reservoir under 20 MPa pressure difference after temporary blockage shown in embodiment 8). - The formula of the plugging agent stimulated by high density brine in the embodiment is the main agent which density is 1.5 g/cm3 and gelling agent of 6 wt %. The core (with saturated formation water) is put in an integrated displacement equipment. Sufficient plugging agent stimulated by high density brine covers a front end of the simulated well casing. Pure water is injected on the plugging agent stimulated by high density brine to simulate the working fluid. Pressure is applied on the front end of the core to simulate the pressure difference on the well casing. The
chart 7 shows the observed the fluid loss from a back end of the core. -
CHART 7data sheet of the pressure bearing capability of the core Pressure No. of Kgi(Dry)/Kgi(Swc) difference Fluid loss rate core (mD) (MPa) (ml/min) 1 54.25/5.49 20 0 5 528/219 20 0.012 7 2056/961 20 0.05 - wherein Kgi(dry) stands for the gas permeability of the dry core; Kgi(Swc) stands for the gas permeability at irreducible water saturation Swc.
- After being blocked for two hours under a pressure difference of 20 MPa, filter cake forms on the contact surface of the core and the gelling agent. The filter cake prevents the gelling agent from leak deep into the core (no more than 3 mm-5 mm) and fluid loss. The permeability is able to be rapidly recovered after the filter cake is being removed.
-
Chart 8 andFIG. 6 show the permeability recovery of the flowback after the blockage. After the being blocked for two hours under a pressure difference of 20 MPa, the filter cake on the front end of the core is being removed, the core is put in the displacement equipment and the displacement is reversed by gas to simulate the well cleaning process during the flowback and the induced flow of the reservoir. The experiment result shows: the permeability is able to recover to 80% of permeability before the blockage after the reservoir being blocked under 20 MPa and the flow is induced under 3 MPa negative pressure difference. -
CHART 8the recovery of permeability of the core Flowback breakthrough Permeability recover No. of Kgi(Swc) Kgf pressure rate after two hours core (mD) (mD) (MPa) (%) 1 5.49 5.00 2.74 91 5 219 186 2 85 7 961 788 1.8 82 - wherein Kgi(Swc) stands for the gas permeability at irreducible water saturation Swc. Kgf stands for the gas permeability after flowback breakthrough by air.
- The embodiments above are just an exemplary and based on the contrivance of the present invention. The embodiments are not a limitation of the present invention. All modifications and alterations are within the protection scope of the present invention.
Claims (11)
1. A cross-linked plugging agent stimulated by high density brine, comprising:
main agent: 10 wt %-90 wt %, gelling agent: 0.5 wt %-9 wt % and pure water; wherein the main agent is selected from the group consisting of a Dipotassium phosphate (K2HPO4), a Tripotassium phosphate (K3PO4) and a Potassium pyrophosphate (K4P2O7) a Sodium dihydrogen phosphate (NaH2PO4); wherein the gelling agent is selected from the group consisting of a Xanthan gum and a kappa carrageenan.
2. The cross-linked plugging agent stimulated by high density brine, as recited in claim 1 , further comprising main agent of 30 wt %-70 wt %.
3. The cross-linked plugging agent stimulated by the high-density brine, as recited in claim 1 , wherein the main agent further comprises a Potassium Dihydrogen Phosphate (KH2PO4) and a Sodium dihydrogen phosphate (NaH2PO4).
4. The cross-linked plugging agent stimulated by the high-density brine, as recited in claim 1 , wherein a density of the plugging agent is controlled within 1.0-1.55 g/cm3.
5. A method of preparing a cross-linked plugging agent stimulated by high density brine, comprising following steps of:
adding main agent, gelling agent into pure water in sequence with respective percentage by mass; stirring evenly; setting an experiment temperature at 90° C.-160° C.; and determining a gelation time and a gelation strength of the plugging agent by gel strength codes; wherein the main agent is 10 wt %-90 wt % and the gelling agent is 0.5 wt %-9 wt %, wherein the main agent is selected from the group consisting of a Dipotassium phosphate (K2HPO4), a Tripotassium phosphate (K3PO4) and a Potassium pyrophosphate (K4P2O7); wherein the gelling agent is selected from the group consisting of a Xanthan gum and a kappa carrageenan.
6. The method of preparing a cross-link plugging agent stimulated by high density brine, as recited in claim 4 , wherein the main agent is further of 30 wt %-70 wt %.
7. The method of preparing a cross-link plugging agent stimulated by high density brine, as recited in claim 4 , wherein the main agent further comprises a Potassium Dihydrogen Phosphate (KH2PO4), a Sodium dihydrogen phosphate (NaH2PO4).
8. The method of preparing a cross-linked plugging agent stimulated by high density brine, as recited in claim 3 , wherein a density of the plugging agent is controlled within 1.0 g/cm3-1.55 g/cm3.
9. A method of applying a cross-linked plugging agent stimulated by the high density brine, comprising a step of applying the plugging agent in well completion and workover under high temperature, high pressure, multi pressure series of strata oil and gas environment when temporary blockage and leak proof is required, protection of reservoir near perforations and water plugging; wherein the cross-linked plugging agent stimulated by the high density brine comprises main agent which is 10 wt %-90 wt %, gelling agent which is 0.5 wt %-9 wt % and pure water, wherein the main agent is high density brine; wherein the main agent is selected from the group consisting of a Dipotassium phosphate (K2HPO4) and a Tripotassium phosphate (K3PO4) and a Potassium pyrophosphate (K4P2O7); wherein the gelling agent is selected from the group consisting of a Xanthan gum and a kappa carrageenan.
10. The method of preparing a cross-link plugging agent stimulated by high density brine, as recited in claim 7 , wherein the main agent further comprises a Potassium Dihydrogen Phosphate (KH2PO4), a Sodium dihydrogen phosphate (NaH2PO4).
11. The method of applying a cross-linked plugging agent stimulated by the high density brine, as recited in claim 5 , comprising a step of applying the plugging agent in well completion and workover under high temperature, high pressure, multi pressure series of strata oil and gas environment when temporary blockage and leak proof is required, protection of reservoir near the perforations and water plugging; wherein a density of the plugging agent is controlled within 1.0-1.55 g/cm3.
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CN202010094980.1 | 2020-02-17 | ||
CN202010094980.1A CN111454705A (en) | 2020-02-17 | 2020-02-17 | High-density saline water stimulated crosslinking type plugging agent and preparation method and application thereof |
PCT/CN2020/076004 WO2021163952A1 (en) | 2020-02-17 | 2020-02-20 | High-density saline stimulated crosslinking type plugging agent, and preparation method therefor and application thereof |
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US17/131,737 Abandoned US20210108122A1 (en) | 2020-02-17 | 2020-12-22 | Cross-linked plugging agent stimulated by high density brine and preparing method thereof |
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Cited By (2)
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CN116103026A (en) * | 2023-02-17 | 2023-05-12 | 西南石油大学 | Competitive crosslinking type high-density salt-resistant cured water microgel temporary plugging agent and preparation method thereof |
CN116731250A (en) * | 2023-06-16 | 2023-09-12 | 广汉市华星新技术开发研究所(普通合伙) | Preparation method of high-temperature-resistant acid liquid gelatinizing agent |
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CN107642357A (en) * | 2017-09-15 | 2018-01-30 | 西南石油大学 | A kind of temperature resistance type low corrosion high density Solid Free test fluid and preparation method thereof |
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2020
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN116103026A (en) * | 2023-02-17 | 2023-05-12 | 西南石油大学 | Competitive crosslinking type high-density salt-resistant cured water microgel temporary plugging agent and preparation method thereof |
CN116731250A (en) * | 2023-06-16 | 2023-09-12 | 广汉市华星新技术开发研究所(普通合伙) | Preparation method of high-temperature-resistant acid liquid gelatinizing agent |
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