CN114621392A - High-temperature-resistant organic silicon polymer gel plugging agent, preparation method and application thereof - Google Patents
High-temperature-resistant organic silicon polymer gel plugging agent, preparation method and application thereof Download PDFInfo
- Publication number
- CN114621392A CN114621392A CN202011460958.0A CN202011460958A CN114621392A CN 114621392 A CN114621392 A CN 114621392A CN 202011460958 A CN202011460958 A CN 202011460958A CN 114621392 A CN114621392 A CN 114621392A
- Authority
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- Prior art keywords
- organic silicon
- polymer
- monomer
- solution
- plugging agent
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Links
- 239000003795 chemical substances by application Substances 0.000 title claims abstract description 75
- 229920001558 organosilicon polymer Polymers 0.000 title claims abstract description 58
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 239000000178 monomer Substances 0.000 claims abstract description 84
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 48
- 239000010703 silicon Substances 0.000 claims abstract description 48
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 44
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 41
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims abstract description 34
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- BAPJBEWLBFYGME-UHFFFAOYSA-N Methyl acrylate Chemical compound COC(=O)C=C BAPJBEWLBFYGME-UHFFFAOYSA-N 0.000 claims description 16
- 238000006243 chemical reaction Methods 0.000 claims description 14
- 229920005573 silicon-containing polymer Polymers 0.000 claims description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 13
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- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 10
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 claims description 9
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 9
- -1 amide compound Chemical class 0.000 claims description 9
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 8
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 8
- KXDAEFPNCMNJSK-UHFFFAOYSA-N Benzamide Chemical compound NC(=O)C1=CC=CC=C1 KXDAEFPNCMNJSK-UHFFFAOYSA-N 0.000 claims description 8
- ZHNUHDYFZUAESO-UHFFFAOYSA-N Formamide Chemical compound NC=O ZHNUHDYFZUAESO-UHFFFAOYSA-N 0.000 claims description 8
- JIGUQPWFLRLWPJ-UHFFFAOYSA-N Ethyl acrylate Chemical compound CCOC(=O)C=C JIGUQPWFLRLWPJ-UHFFFAOYSA-N 0.000 claims description 7
- PNJWIWWMYCMZRO-UHFFFAOYSA-N pent‐4‐en‐2‐one Natural products CC(=O)CC=C PNJWIWWMYCMZRO-UHFFFAOYSA-N 0.000 claims description 7
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- XDLMVUHYZWKMMD-UHFFFAOYSA-N 3-trimethoxysilylpropyl 2-methylprop-2-enoate Chemical compound CO[Si](OC)(OC)CCCOC(=O)C(C)=C XDLMVUHYZWKMMD-UHFFFAOYSA-N 0.000 claims description 6
- DWAQJAXMDSEUJJ-UHFFFAOYSA-M Sodium bisulfite Chemical compound [Na+].OS([O-])=O DWAQJAXMDSEUJJ-UHFFFAOYSA-M 0.000 claims description 6
- CQEYYJKEWSMYFG-UHFFFAOYSA-N butyl acrylate Chemical compound CCCCOC(=O)C=C CQEYYJKEWSMYFG-UHFFFAOYSA-N 0.000 claims description 6
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 6
- 235000010267 sodium hydrogen sulphite Nutrition 0.000 claims description 6
- KZNICNPSHKQLFF-UHFFFAOYSA-N succinimide Chemical compound O=C1CCC(=O)N1 KZNICNPSHKQLFF-UHFFFAOYSA-N 0.000 claims description 6
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 5
- 150000001252 acrylic acid derivatives Chemical class 0.000 claims description 5
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 5
- 239000011790 ferrous sulphate Substances 0.000 claims description 5
- 235000003891 ferrous sulphate Nutrition 0.000 claims description 5
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims description 5
- 229910000359 iron(II) sulfate Inorganic materials 0.000 claims description 5
- 238000006116 polymerization reaction Methods 0.000 claims description 5
- 238000000967 suction filtration Methods 0.000 claims description 5
- LFQCEHFDDXELDD-UHFFFAOYSA-N tetramethyl orthosilicate Chemical compound CO[Si](OC)(OC)OC LFQCEHFDDXELDD-UHFFFAOYSA-N 0.000 claims description 5
- YUYCVXFAYWRXLS-UHFFFAOYSA-N trimethoxysilane Chemical compound CO[SiH](OC)OC YUYCVXFAYWRXLS-UHFFFAOYSA-N 0.000 claims description 5
- DLFVBJFMPXGRIB-UHFFFAOYSA-N Acetamide Chemical compound CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 claims description 4
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 4
- 239000000872 buffer Substances 0.000 claims description 4
- 239000006172 buffering agent Substances 0.000 claims description 4
- GGSUCNLOZRCGPQ-UHFFFAOYSA-N diethylaniline Chemical compound CCN(CC)C1=CC=CC=C1 GGSUCNLOZRCGPQ-UHFFFAOYSA-N 0.000 claims description 4
- 238000010528 free radical solution polymerization reaction Methods 0.000 claims description 4
- 239000012263 liquid product Substances 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 4
- NELRINSZCVVEAD-UHFFFAOYSA-N chloro-ethenyl-methylsilane Chemical compound C[SiH](Cl)C=C NELRINSZCVVEAD-UHFFFAOYSA-N 0.000 claims description 3
- 238000004090 dissolution Methods 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 3
- QLNJFJADRCOGBJ-UHFFFAOYSA-N propionamide Chemical compound CCC(N)=O QLNJFJADRCOGBJ-UHFFFAOYSA-N 0.000 claims description 3
- 229940080818 propionamide Drugs 0.000 claims description 3
- 239000012966 redox initiator Substances 0.000 claims description 3
- 229960002317 succinimide Drugs 0.000 claims description 3
- 239000004342 Benzoyl peroxide Substances 0.000 claims description 2
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical compound C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 claims description 2
- LSDPWZHWYPCBBB-UHFFFAOYSA-N Methanethiol Chemical compound SC LSDPWZHWYPCBBB-UHFFFAOYSA-N 0.000 claims description 2
- 235000019400 benzoyl peroxide Nutrition 0.000 claims description 2
- 239000003638 chemical reducing agent Substances 0.000 claims description 2
- 229940065472 octyl acrylate Drugs 0.000 claims description 2
- ANISOHQJBAQUQP-UHFFFAOYSA-N octyl prop-2-enoate Chemical compound CCCCCCCCOC(=O)C=C ANISOHQJBAQUQP-UHFFFAOYSA-N 0.000 claims description 2
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- 230000001590 oxidative effect Effects 0.000 claims description 2
- JRKICGRDRMAZLK-UHFFFAOYSA-L peroxydisulfate Chemical compound [O-]S(=O)(=O)OOS([O-])(=O)=O JRKICGRDRMAZLK-UHFFFAOYSA-L 0.000 claims description 2
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 2
- GQIUQDDJKHLHTB-UHFFFAOYSA-N trichloro(ethenyl)silane Chemical compound Cl[Si](Cl)(Cl)C=C GQIUQDDJKHLHTB-UHFFFAOYSA-N 0.000 claims description 2
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
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- ARYZCSRUUPFYMY-UHFFFAOYSA-N methoxysilane Chemical class CO[SiH3] ARYZCSRUUPFYMY-UHFFFAOYSA-N 0.000 description 2
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- DZSVIVLGBJKQAP-UHFFFAOYSA-N 1-(2-methyl-5-propan-2-ylcyclohex-2-en-1-yl)propan-1-one Chemical compound CCC(=O)C1CC(C(C)C)CC=C1C DZSVIVLGBJKQAP-UHFFFAOYSA-N 0.000 description 1
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- 239000012299 nitrogen atmosphere Substances 0.000 description 1
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- 235000011007 phosphoric acid Nutrition 0.000 description 1
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- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Inorganic materials [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 1
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- 238000005303 weighing Methods 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/52—Amides or imides
- C08F220/54—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide
- C08F220/56—Acrylamide; Methacrylamide
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/12—Esters of monohydric alcohols or phenols
- C08F220/14—Methyl esters, e.g. methyl (meth)acrylate
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/12—Esters of monohydric alcohols or phenols
- C08F220/16—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
- C08F220/18—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms with acrylic or methacrylic acids
- C08F220/1804—C4-(meth)acrylate, e.g. butyl (meth)acrylate, isobutyl (meth)acrylate or tert-butyl (meth)acrylate
-
- 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
- C09K8/02—Well-drilling compositions
- C09K8/03—Specific additives for general use in well-drilling compositions
- C09K8/035—Organic additives
-
- 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
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/141—Feedstock
Abstract
The invention relates to a high-temperature-resistant organic silicon polymer gel plugging agent, a preparation method and application thereof, belonging to the technical field of drilling fluid plugging in the field of petroleum exploration and development. The organic silicon gel plugging agent is formed by crosslinking an organic silicon polymer in water, wherein the organic silicon polymer is formed by polymerizing a vinyl monomer and an organic silicon monomer. The invention also provides a preparation method and application of the organic silicon polymer gel plugging agent. The organic silicon polymer gel plugging agent has controllable gelling time, better temperature and pressure resistance, simple preparation method and low cost, and the use temperature condition can reach more than 150 ℃.
Description
Technical Field
The invention belongs to the technical field of drilling fluid plugging in the field of petroleum exploration and development, and particularly relates to a high-temperature-resistant organic silicon polymer gel plugging agent, a preparation method and application thereof.
Background
Along with the gradual exhaustion of conventional oil and gas resources, unconventional oil and gas resources such as heavy oil, oil sand, shale oil, shale gas, coal bed gas and the like increasingly become hot spots for development. The deep oil gas resources in China have wide distribution range and large reserves, and become main backup energy for relieving the contradiction between energy supply and demand in China. The depth of deep reservoirs (Tarim, Sichuan, Bohai Bay and the like) in China generally exceeds 6000m, the deepest depth is 9000m, and the bottom temperature is 180-260 ℃. The ultra-deep well has the characteristics of high temperature and pressure, complex geological conditions (mostly salt-gypsum layers), multiple sets of pressure layer systems in the same open hole well section and the like, a target stratum in the drilling process mostly contains complex structures such as broken, cracks and karst caves, the very serious well leakage problem is often caused in the drilling operation process, the drilling construction progress can be seriously influenced, the operation cost is improved, multiple problems such as drilling fluid leakage, reservoir damage, well mouth collapse, drilling sticking, well blowout and the like are easily caused, and even the great influence is caused on the development of deep layer oil gas.
For the treatment of the lost circulation problem, the most critical part is to select the lost circulation material, and different types of materials such as fibrous materials, granular materials, flaky materials and the like are generally used in a synergistic and composite mode, so that a good treatment effect can be achieved for the lost circulation problem. However, the use limitation of the traditional materials is obvious, and in the case of large and numerous leak-off layer cracks, a good sealing layer is difficult to form around the well bore. At present, a chemical gelling plugging technology is adopted to obtain a very obvious effect in the treatment process aiming at the well leakage problem, but the treatment time and the control time of gel are difficult to accurately master, so that the conditions of thermal degradation, dehydration shrinkage and the like of the temperature resistance of the gel are caused due to the influence of the environmental temperature of a high-temperature layer, and finally the problems of gel viscosity reduction, great strength reduction and the like are caused.
Chinese patent document CN106928402A discloses a polymer gel formed from a polymer in water by physical actions such as van der waals forces, hydrogen bonding and electrostatic interactions. The polymer is formed by polymerizing an acrylamide monomer, a hydrophobic monomer unit and a functional monomer, and the provided polymer gel has low viscosity under high-speed shearing and good injectability, and can ensure the high-dose injection of a plugging system; the composite material has good shearing restorability and high viscoelasticity, so that the front-edge slug of the composite material in a near-wellbore area is stable, the plugging success rate is high, a subsequent water drive seepage path can be effectively changed, and the swept volume is increased; has good temperature resistance and salt tolerance, and has long-term stability. However, the polymer gel forms adsorption with clay through physical actions such as van der waals force, hydrogen bond and electrostatic action, the heat resistance is generally below 120 ℃, and the heat resistance of the gel per se is subjected to thermal degradation and syneresis and the like due to the influence of the environmental temperature of a high-temperature layer. In addition, the polymer gel has high viscosity-average molecular weight (some of which are more than 4000 ten thousand), which can cause macromolecular retention damage of reservoir pore canals. The gelling time of the gel is not easy to control, the stability at the high temperature of more than 120 ℃ is not ideal, and the requirement of high-temperature stratum leak stoppage cannot be met.
Chinese patent document CN106749899A discloses a preparation method of a polymer gelling agent for high-temperature and high-salt resistant profile control and water plugging, which is prepared by the polymerization reaction of an acrylamide monomer, a methacrylamide monomer, an N-tert-butyl acrylamide monomer, 2-acrylamide-2-methylpropanesulfonic acid and a modification auxiliary agent in the presence of an initiator, by properly adjusting the mole percentage of the functional monomer and the amide group through designing the molecular main chain, so that the gel formed by crosslinking the synthesized polymer under extreme oil reservoir conditions (the temperature is more than or equal to 110 ℃, the mineralization degree is more than or equal to 10 ten thousand ppm) has higher strength and better thermal stability, the polymer has low viscosity-average molecular weight (less than 1000 ten thousand), good solubility, strong high-temperature and high-salt resistance, free and controllable gelling time, high gelling strength and good thermal stability. However, the crosslinking agent of the liquid rubber plug is mainly an organic crosslinking agent, and the reaction process is that the active group of the polymer and the crosslinking agent undergo a condensation reaction to form a strong covalent bond, which also causes the gel breaking difficulty of a gel system under the high temperature condition, and restricts the application range of the polymer gel liquid rubber plug.
The Chinese patent application CN 105567190A discloses a gel plugging agent in the drilling plugging operation of an oil and gas field and a preparation method thereof, wherein the plugging agent is formed by copolymerizing four monomers, and the first monomer provides hydrophilicity for the plugging agent and promotes the water absorption expansion of the material; the second monomer is a cationic monomer, provides a group with positive charges, and increases the charge attraction effect of the plugging agent and the leakage hole channel wall; the third monomer is unsaturated organic silicon coupling agent monomer which can improve the retention capacity of the plugging agent at the leaking layer; the fourth type of monomer is a polyunsaturated bond functional monomer, so that the plugging agent forms chemical crosslinking. The invention adopts aqueous solution polymerization, has simple process and convenient operation. The plugging agent prepared by the invention has the advantages of strong water absorption and expansion capacity and capability of improving the retention capacity of the plugging material in a leaking layer by containing various functional groups capable of forming mechanical interaction with the leaking layer, but the gel plugging agent does not pay attention to high temperature resistance.
Disclosure of Invention
Aiming at the defects and shortcomings of the existing gel plugging agent, the invention provides a high-temperature resistant organic silicon polymer and an organic silicon polymer plugging material.
The invention also provides a preparation method of the high-temperature-resistant organic silicon polymer plugging material.
The invention also provides an application of the high-temperature-resistant organic silicon polymer gel plugging agent.
The technical problems mainly solved by the invention include, but are not limited to: the gelling time of the existing gel plugging material is difficult to accurately master; the existing gel plugging material has insufficient temperature resistance, and the problems of gel viscosity reduction, great strength reduction and the like are finally caused by the conditions of thermal degradation, syneresis and the like under the high-temperature condition.
The invention aims to synthesize an organic silicon polymer, avoid using an organic solvent, and preferably select an organic silicon monomer capable of forming a more compact space network structure. And the organic silicon polymer gel plugging material is developed by combining the characteristics of the organic silicon polymer material, so that the aim of effectively plugging the crack pores under the conditions of high temperature and complex stratum structures is fulfilled. The organic silicon polymer gel plugging material has better viscoelasticity and shearing dilutability; the gelling time of the gel is controllable.
The invention achieves the above purpose through the following technical scheme.
An organosilicon polymer plugging material is formed by crosslinking an organosilicon polymer in water, wherein the organosilicon polymer is formed by polymerizing a vinyl monomer and an organosilicon monomer; the vinyl monomer is a combination of acrylic acid or acrylate monomer and amide compound.
Preferably, the content of the vinyl monomer is 25-35% by mass of the organosilicon polymer lost circulation material; the organic silicon monomer accounts for 0.5 to 2.0 percent of the vinyl monomer.
The organic silicon monomer is one or more of methyl vinyl chlorosilane, vinyl trichlorosilane and gamma-methacryloxypropyl trimethoxysilane.
Preferably, the organosilicon monomer is gamma-methacryloxypropyltrimethoxysilane.
The acrylate monomer is one or more of Methyl Acrylate (MA), Ethyl Acrylate (EA), Butyl Acrylate (BA) and octyl acrylate (EHA);
preferably, the acrylate monomer is one or more of Methyl Acrylate (MA), Ethyl Acrylate (EA) and Butyl Acrylate (BA);
more preferably, the acrylate monomer is one or more of Methyl Acrylate (MA) and Ethyl Acrylate (EA);
the amide compound is one or more of formamide, acetamide, propionamide, acrylamide, N-dimethylformamide, benzamide and succinimide.
Preferably, the amide compound is one or more of formamide, acrylamide, N-dimethylformamide, benzamide and succinimide.
Still preferably, the amide compound is one or more of formamide, acrylamide, N-dimethylformamide and benzamide.
Wherein the viscosity average molecular weight of the organic silicon polymer is 100-1000 ten thousand;
preferably, the viscosity average molecular weight of the organosilicon polymer is 100-500 ten thousand;
and preferably low, the viscosity average molecular weight of the organic silicon polymer is 150-250 ten thousand.
The invention also provides a high-temperature resistant organic silicon polymer which is formed by polymerizing the vinyl monomer and the organic silicon monomer; the vinyl monomer is a combination of an acrylic acid or acrylate monomer and an amide compound.
The acrylic acid or acrylate monomer, the amide compound and the organosilicon monomer are selected as described above.
The preparation method of the high-temperature resistant organic silicon polymer can adopt the prior art.
As a preferred embodiment, the present invention provides the following method for producing a silicone polymer.
A preparation method of a high temperature resistant organic silicon polymer comprises the steps of carrying out polymerization reaction on a vinyl monomer and an organic silicon monomer at 50-60 ℃ in the presence of an initiator and a buffering agent; the polymerization reaction is solution polymerization; the initiator is a redox initiator combination and is selected from one group of ammonium persulfate/sodium bisulfite, potassium persulfate/sodium bisulfite, ammonium persulfate/ferrous sulfate, hydrogen peroxide/ferrous sulfate, benzoyl peroxide/N, N-diethylaniline, potassium persulfate/silver nitrate or persulfate/mercaptan combination.
The dosage of the initiator is 0.2 to 0.5 percent of the total amount of the vinyl monomer.
The molar ratio of the oxidant to the reductant is 1-2: 1-2.
The buffer is one or more of ethanol, acetic acid, sodium acetate, phosphoric acid and sodium phosphate.
The dosage of the buffer is 0.1-0.2% of the total amount of the vinyl monomer.
The solution polymerization is carried out in a solvent, and the solvent is water; preferably deionized water.
The invention relates to a preparation method of an organic silicon polymer, which specifically comprises the following steps:
(1) weighing vinyl monomers, and fully dissolving the vinyl monomers in deionized water to obtain a solution A;
(2) dissolving an initiator and a buffering agent in deionized water to obtain a solution B;
(3) adjusting the pH value of the solution A to 4-6 by using a sodium hydroxide solution, adding an organic silicon monomer, mixing with the solution B, and stirring to prepare a suspension;
(4) stirring the suspension at a constant temperature of 50-60 ℃ for reaction for 6-8h to obtain a synthetic product;
(5) and repeatedly washing the synthesized product by using absolute ethyl alcohol, filtering, and drying to obtain the organic silicon polymer.
The dissolving and mixing processes in the steps (1) to (3) are carried out under the condition of heating in a water bath at the temperature of 24-26 ℃.
The stirring in the step (3) is performed at a rotation speed of 150-300r/min for 20-35 minutes.
The mass concentration of the sodium hydroxide solution in the step (4) is 15-25%; preferably a sodium hydroxide solution with a mass concentration of 20%.
The rotation speed of the constant-temperature stirring in the step (4) is 300-.
Before the reaction in the step (4), nitrogen can be used for deoxygenation, and a condensation cycle can be adopted in the reaction process.
And (3) performing suction filtration in the step (5) by using a Buchner funnel to obtain a solid product, and drying the solid product in a vacuum drying oven at the temperature of 45-55 ℃ for 6-8 hours.
The amount of the absolute ethyl alcohol for washing in the step (5) is determined according to needs, and the addition amount of the absolute ethyl alcohol for washing is continuously stirred until the precipitate is completely precipitated.
The invention also provides a preparation method of the organic silicon gel plugging agent, which comprises the following steps:
adding an organic silicon polymer into deionized water under the stirring condition for fully dissolving, and adjusting the pH value of the solution to 7 by using a sodium hydroxide solution to obtain a solution 1;
dropping crosslinking agent slowly into the solution 1, with stirring speed of 800-; the addition of the cross-linking agent is 0.05-0.4% of the total amount of the vinyl monomer, and viscoelastic fluid, namely the organic silicon gel plugging agent liquid product, is obtained.
The cross-linking agent is one or more of ethyl orthosilicate, methyl orthosilicate, trimethoxy silane and acrylate compounds;
preferably, the cross-linking agent is one or more of ethyl orthosilicate, trimethoxy silane and acrylate compounds;
preferably, the cross-linking agent is one or more of ethyl orthosilicate and acrylate compounds;
further preferably, the cross-linking agent is ethyl orthosilicate.
The dosage of the cross-linking agent is 1.0-2.0% of the total amount of the vinyl monomer.
The organic silicon gel plugging agent liquid product can be directly applied as a plugging agent.
Further, in order to facilitate the transportation and storage of the product and to make the polymer concentration easier to control when in use, the product obtained in the second step is post-treated as follows:
thirdly, placing the viscoelastic fluid in the step II in a vacuum drying oven, and keeping the temperature for 6-8 hours to obtain an organic silicon gel plugging agent solid product;
fourthly, taking out the solid product of the organic silicon gel plugging agent obtained in the third step, cutting the solid product into small blocks, placing the small blocks in a vacuum drying box, continuously drying the small blocks for 24 to 36 hours at a constant temperature, taking out the small blocks, and making powder to obtain the powder product of the organic silicon gel plugging agent.
In the preparation of the organic silicon gel plugging agent, the rotating speed of stirring in the step I is 150-300 r/min.
In the third step, the drying temperature of the vacuum drying oven is 50-60 ℃, and the vacuum pressure is 0.05-0.08 MPa.
In the preparation of the organic silicon gel plugging agent, in the step II, the cross-linking agent is the same as or different from the cross-linking agent in the preparation method of the organic silicon polymer. In the step (II), the cross-linking agent is selected from one or more of ethyl orthosilicate, methyl orthosilicate, trimethoxy silane and acrylate compounds.
In some preferred embodiments, the crosslinking agent is dissolved in deionized water in advance when used, and is prepared into a solution with the mass concentration of 35-45%, so that the crosslinking speed can be controlled conveniently.
The organic silicon gel plugging agent is a viscoelastic body, and the storage modulus and the energy consumption modulus are kept stable under the condition of stress change. At phase angles below 20 °, the gel always has good viscoelasticity.
The organosilicon polymer gel plugging agent is applied as a plugging agent of water-based drilling fluid, and a powdery product or a solid product of the prepared organosilicon gel plugging agent is added with water to prepare fluid for use; preferably, the fluid is used in a configuration such that the polymer has a mass concentration of 3 to 6 wt.%.
Compared with the prior art, the invention has the beneficial effects that:
compared with the prior art, the preparation method of the invention introduces the organic silicon functional monomer when designing the molecular main chain of the organic silicon polymer, improves the thermal stability of the polymer, particularly controls the pH value of the reaction by adding a buffering agent in the synthesis process, controls the hydrolysis speed of the organic silicon monomer in aqueous solution, ensures that organic silane in the polymer functional monomer can be hydrolyzed to generate silicon hydroxyl, and ensures that a part of silicon hydroxyl is condensed with each other to form a Si-O-Si space network structure.
Compared with the prior art, the invention obtains the target product by free radical polymerization in the aqueous solvent, avoids the damage of subsequent application to the stratum caused by using an organic solvent and effectively reduces the production cost. The invention uses the buffer to control the hydrolysis speed of the organic silicon monomer, and can overcome the related technical problems. The acrylamide monomer in the polymer is a hydrophilic group, so that the polymer has good water solubility. The organic silicon monomer in the polymer has hydrophobic property and good temperature resistance, and the other part of silicon hydroxyl can also form Si-O-Si chemical bonds with the silicon hydroxyl on the surface of the clay in the stratum, so that the adsorption strength of polymer molecules and the surface of the clay in the stratum under the high-temperature condition is increased; the gamma-methacryloxypropyl trimethoxysilane is particularly preferred, the C ═ C double bond on the main chain of the monomer is easier to copolymerize with other vinyl monomers, 3 methoxysilanes exist on the side chain, the hydrolyzed monomer has excellent adhesive force and durability, the adsorption capacity of the polymer and the clay surface can be greatly improved, and in addition, 3 methoxysilanes are crosslinked to form a more compact space network structure.
The organic silicon polymer is subjected to secondary crosslinking in water through the crosslinking agent to prepare the gel plugging agent, so that a formed grid structure is more uniform, a membrane is formed among chains, a main chain, a branch chain and an interchain membrane tend to form a three-dimensional pore channel structure, the binding force on water is strongest, the small-molecule polymer is filled in pores of a new polymer macromolecular grid to form a membrane, the membrane is full in layers, the binding capacity on water is stronger, larger deformation resistance is generated, the concentration-increased polymer is distributed in a flocculent form, meanwhile, the viscosity-average molecular weight of the polymer is lower, the solubility is better, the gel plugging material formed through crosslinking shows low apparent viscosity at a high shear rate, shows high apparent viscosity at a low shear rate, has better viscoelasticity and shear dilution, and is favorable for pumping gel into a leaking layer. Temperature resistance tests further prove that the temperature resistance of the plugging agent can reach more than 150 ℃, and the gel is determined to be viscoelastic fluid through gel viscoelasticity evaluation, so that the storage modulus and the energy consumption modulus are kept stable under the stress change condition. At phase angles below 20 °, the gel always has good viscoelasticity.
Aiming at the problems of the existing chemical gel plugging agent, the invention develops a novel organic silicon polymer gel plugging material which has the capabilities of high temperature resistance, strong stability and self-crosslinking, and also has better viscoelasticity and shearing dilutability, controllable gelling time of gel, and better temperature and pressure resistance. So that the water-absorbing agent can fully and smoothly enter a stratum fracture under the action of differential pressure, and can absorb water to expand after a certain time to form a bridge plug so as to achieve the purpose of effectively plugging the pore of the fracture.
The organic silicon monomer in the organic silicon polymer gel plugging agent has certain hydrophobic capacity, and simultaneously plays a role in supporting a macromolecular skeleton in the polymer, so that the toughness and the stability of the gel are enhanced, and the effective plugging time of gel particles on crack pores is greatly prolonged.
The organic silicon polymer gel particles do not influence the performance of the drilling fluid, and the preparation process is simple and is suitable for field operation. The organic silicon polymer gel plugging agent is generally used at the temperature of 80-150 ℃, is still effective for extreme oil reservoir conditions above 150 ℃ and can reach 180 ℃ at most.
Drawings
FIG. 1 the infrared spectrum of the silicone polymer synthesized in example 1.
FIG. 2 is an infrared spectrum of the silicone polymer gel prepared in example 2.
Fig. 3 is a thermogravimetric analysis curve of the silicone gel plugging agent.
FIG. 4 is a plot of leakage versus pressure for different formation conditions.
FIG. 5 is a graph of leakage versus pressure for different temperature conditions.
FIG. 6 is a graph of gel stress scan results for silicone polymers prepared at different polymer concentrations and crosslinker loadings.
FIG. 7 is a frequency sweep of silicone polymer gels prepared at different polymer concentrations and crosslinker loadings.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other examples, which may be modified or appreciated by those of ordinary skill in the art based on the examples given herein, are intended to be within the scope of the present invention.
Unless otherwise specified,% in examples are mass percentages.
Example 1:
a preparation method of an organic silicon polymer comprises the following steps:
(1) acrylic acid, acrylamide according to 2: 3, fully dissolving the mixture in deionized water to obtain a solution A;
(2) anhydrous ethanol and ethyl orthosilicate are mixed according to the weight ratio of 1: 4, dissolving in deionized water, and adding an initiator accounting for 0.2 percent of the total amount of the vinyl monomers, wherein the initiator is a mixture of potassium persulfate and sodium bisulfite with the molar ratio of 1: 1 to obtain a solution B;
(3) adjusting the pH value of the solution A to be 4 by utilizing a prepared 20% sodium hydroxide solution in advance, and adding gamma-methacryloxypropyltrimethoxysilane accounting for 0.5% of the total mass of acrylic acid and acrylamide monomers to obtain a solution C; adding the solution C and the solution B into a three-neck flask in sequence, and stirring at the rotating speed of 300r/min for 30 minutes to prepare a suspension;
(4) the stirring speed is increased to 500r/min, the mixture is heated in a water bath to the reaction temperature of 60 ℃, and the organic silicon polymer synthetic product is obtained after the constant temperature reaction for 6 hours;
(5) and repeatedly washing the synthesized product by using absolute ethyl alcohol, performing suction filtration by using a Buchner funnel to obtain a solid product, placing the solid product in a vacuum drying oven, and drying for 6 hours at the temperature of 50 ℃ to obtain the organic silicon polymer.
The IR spectrum of the silicone polymer synthesized in this example is shown in FIG. 1. The viscosity average molecular weight was 2004594.
Example 2:
an organosilicon gel plugging agent is prepared by carrying out secondary crosslinking on the organosilicon polymer in example 1. The amount of the crosslinking agent added for the secondary crosslinking was 0.1% of the total amount of the vinyl monomers (acrylic acid + acrylamide).
A preparation method of an organic silicon gel plugging agent comprises the following steps:
(1) adding the organic silicon polymer prepared in the example 1 into deionized water under the condition of stirring at a low speed of 200-250 r/min, fully dissolving to prepare a polymer aqueous solution with the concentration of 6%, and adjusting the pH of the solution to 7 by using a pre-prepared 20% sodium hydroxide solution to obtain a solution 1;
(2) slowly dripping 0.1 percent of cross-linking agent ethyl orthosilicate into the solution 1, improving the stirring speed to 800r/min, stirring for 15min, and reacting at the temperature of 70 ℃; obtaining the viscoelastic fluid, namely the organic silicon gel plugging agent liquid product.
(3) And (3) placing the viscoelastic fluid obtained in the step (2) in a vacuum drying oven, setting the constant temperature to be 50 ℃, setting the vacuum pressure to be 0.05MPa, and reacting at constant temperature for 6 hours to obtain the organic silicon gel plugging agent solid product.
(4) And (4) taking out the solid product of the organic silicon gel plugging agent obtained in the step (3), cutting the solid product into small pieces, placing the small pieces in a vacuum drying box, drying at a constant temperature of 50 ℃, taking out the small pieces after 24 hours, and making powder to obtain the powder product of the organic silicon gel plugging agent.
The infrared spectrum of the silicone polymer gel plugging agent synthesized in this example is shown in fig. 1.
Example 3 Effect of crosslinker addition on gelling
As described in step (2) of example 2, the crosslinking agents were added in mass concentrations of 0.05%, 0.1%, 0.2%, 0.3% and 0.4%, respectively, and placed in a forced air drying oven, and the influence of the addition amount of the crosslinking agent on gelling was examined, under experimental conditions: DVT-3 Brookfield viscometer, 70 ℃ and 3 r/min. A viscosity of more than 200 pas indicates completion of the gelling, corresponding to the results shown in Table 1 below.
TABLE 1 Effect of crosslinker loading on crosslinking time
The experimental results in table 1 show that: in the process of increasing the addition amount of the cross-linking agent continuously, the gelling rate tends to increase first and then decrease, and the reason is that linear polymer molecules are cross-linked to form a spatial network structure through the bridging action of covalent bonds or ionic bonding lines by the cross-linking agent at a certain concentration. With the addition of the cross-linking agent, the gelling rate gradually becomes stable, the addition amount of the cross-linking agent is the optimal addition amount, however, the situation of excessive cross-linking of the whole gel system occurs due to the continuous increase of the addition amount of the cross-linking agent, and finally the stability of the whole system is reduced.
Example 4 Effect of temperature on gel formation of Polymer
An aqueous solution of a polymer having a mass fraction of 6.0% was prepared as described in step (1) of example 2, and a crosslinking agent having a mass fraction of 0.1% was added thereto as described in step (2) of example 2, and divided into 5 groups. The solutions were placed in ovens at different temperatures, and the apparent viscosity of the polymer solution was measured at 3r/min with the aid of a Brookfield viscometer model DVT-3 (No. 64 spindle), and when the apparent viscosity was greater than 200Pa s, the gelling of the polymer was complete, and the experimental results are shown in Table 2.
TABLE 2 influence of temperature on gel formation of the polymer.
As can be seen from Table 2: with the increase of the temperature, the gelling speed of the polymer solution can be rapidly increased, because the increase of the temperature can accelerate the transport rate of polymer molecules, the movement rate of macromolecular chains in the polymer solution is increased, the molecular chains of the polymer are stretched, and Si-OCH on the side chains of the polymer are rapidly adsorbed3The Si-O-Si bonds formed after hydrolysis form molecular chains with a net structure, so that the interaction force among different chains is continuously improved, and the gelling time is also reduced to a great extent. The optimum temperature is known to be 70 ℃ for the bonding requirements.
Example 5 preparation method of an organosilicon polymer gel plugging agent
The method comprises the following steps:
(1) methyl acrylate, N-dimethylformamide as 4: 3 is fully dissolved in deionized water to obtain a solution A;
(2) anhydrous ethanol and methyl orthosilicate are mixed according to the weight ratio of 1: 4, dissolving in deionized water, and adding potassium persulfate/sodium bisulfite (molar ratio of 1: 2) accounting for 0.2 percent of the total amount of the vinyl monomers to obtain solution B;
(3) adjusting the pH value of the solution A to be 4 by utilizing a prepared 20% sodium hydroxide solution, and adding methyl vinyl chlorosilane of which the total mass is 0.5% of that of the vinyl monomer to obtain a solution C; adding the solution C and the solution B into a three-neck flask in sequence, and stirring at the rotating speed of 300r/min for 30 minutes to prepare a suspension;
(4) the stirring speed is increased to 500r/min, the mixture is heated in a water bath to the reaction temperature of 60 ℃, and the organic silicon polymer synthetic product is obtained after the constant temperature reaction for 6 hours;
(5) and repeatedly washing the synthesized product by using absolute ethyl alcohol, performing suction filtration by using a Buchner funnel to obtain a solid product, placing the solid product in a vacuum drying oven, and drying for 6 hours at the temperature of 50 ℃ to obtain the organic silicon polymer.
(6) Adding the organic silicon polymer prepared in the step (5) into deionized water under the condition of stirring at a low speed of 200r/min for full dissolution to prepare a polymer aqueous solution with the concentration of 6%, and adjusting the pH of the solution to 7 by using a pre-prepared 20% sodium hydroxide solution to obtain a solution 1;
(7) slowly dropwise adding a cross-linking agent of methyl orthosilicate into the solution 1, increasing the stirring speed to 800r/min, stirring for 15min, reacting at the temperature of 70 ℃, and adding the cross-linking agent in an amount of 0.1 percent of the mass of the vinyl monomer to obtain viscoelastic fluid;
(8) and (3) placing the viscoelastic fluid obtained in the step (7) in a vacuum drying oven, setting the constant temperature to be 50 ℃, setting the vacuum pressure to be 0.05MPa, carrying out constant temperature reaction for 6h, taking out after primary drying, dividing into small blocks, placing in a vacuum drying oven for drying at constant temperature, taking out after 24h, and carrying out powder making to obtain the organic silicon gel plugging agent powder.
The plugging properties of the silicone polymer gel plugging agent powder synthesized in this example are shown in table 3.
Example 6 preparation method of an organosilicon polymer gel plugging agent
The method comprises the following steps:
(1) butyl acrylate and propionamide according to 3: 5 to obtain a solution A;
(2) anhydrous ethanol and ethyl orthosilicate are mixed according to the weight ratio of 1: 4 is dissolved in deionized water, and ammonium persulfate/ferrous sulfate (molar ratio is 1: 1) with the total amount of vinyl monomers being 0.2 percent is added to obtain solution B;
(3) adjusting the pH value of the solution A to be 4 by utilizing a prepared 20% sodium hydroxide solution, and adding gamma-methacryloxypropyltrimethoxysilane accounting for 0.5% of the total mass of the vinyl monomers to obtain a solution C; adding the solution C and the solution B into a three-neck flask in sequence, and stirring at the rotating speed of 300r/min for 30 minutes to prepare a suspension;
(4) the stirring speed is increased to 500r/min, the mixture is heated in a water bath to the reaction temperature of 60 ℃, and the organic silicon polymer synthetic product is obtained after the constant temperature reaction for 6 hours;
(5) repeatedly washing the synthesized product by using absolute ethyl alcohol, performing suction filtration by using a Buchner funnel to obtain a solid product, placing the solid product in a vacuum drying oven, and drying for 6 hours at the temperature of 50 ℃ to obtain an organic silicon polymer;
(6) adding the organic silicon polymer prepared in the step (5) into deionized water under the condition of stirring at a low speed of 200r/min for full dissolution to prepare a polymer aqueous solution with the concentration of 6%, and adjusting the pH of the solution to 7 by using a pre-prepared 20% sodium hydroxide solution to obtain a solution 1;
(7) slowly dropwise adding crosslinking agent trimethoxy silane into the solution 1, increasing the stirring speed to 800r/min, stirring for 15min, reacting at the temperature of 70 ℃, and adding the crosslinking agent in an amount of 0.1 percent of the mass of the vinyl monomer to obtain viscoelastic fluid;
(8) and (3) placing the viscoelastic fluid obtained in the step (7) in a vacuum drying oven, setting the constant temperature to be 50 ℃, setting the vacuum pressure to be 0.05MPa, carrying out constant temperature reaction for 6h, taking out after primary drying, dividing into small blocks, placing in a vacuum drying oven for drying at constant temperature, taking out after 24h, and carrying out powder making to obtain the organic silicon gel plugging agent powder.
The plugging performance of the silicone polymer gel plugging agent synthesized in this example is shown in table 3.
TABLE 3 evaluation of plugging Properties of organic silicon polymer gel plugging agent
Experimental example: evaluation of product Properties
The silicone gel plugging agent prepared in example 2 was characterized and performance evaluated.
Characterization of the Silicone gel plugging agent
1. Thermal analysis
In the thermogravimetric and simultaneous thermal analysis (TGA) of METTLERTODO, an aluminum crucible was used and the purge flow was 50mL min-1Thermogravimetric analysis (TGA) was performed on the silicone gel plugging agent solid powder under nitrogen atmosphere and at an initial heating temperature of 40 ℃. The initial temperature for thermal analysis was 40 ℃ and the final temperature was 800 ℃ and the TGA curve is shown in FIG. 3.
For the TGA curve (fig. 3), when the temperature is in the range of 40 ℃ to 165 ℃, the temperature at this stage belongs to the first stage of thermal degradation, and the corresponding weight loss rate is 10.4%, which is mainly caused by the fact that moisture exists in the polymer and is lost after being heated, and the essential reason is that the polymer itself is considered to be added with a structural monomer with hydrophilic property in the design process, so that the polymer itself absorbs water. When the temperature is in the range of 165-649 ℃, the second stage of thermal degradation is represented, the corresponding weight loss ratio is 19.6%, and the key point of mass loss is that the temperature influences the polymer to further cause the phase state change of the polymer; for the range of 310 ℃ to 426 ℃, the corresponding weight loss rate is 29.6 percent, and when the temperature condition is in the range, the corresponding side chain of the polymer gradually starts to degrade; the weight loss rate in 426-649 ℃ stage is 15.1%, and the weight loss in the stage is caused by the gradual degradation of the main chain of the polymer molecule. In the case of a temperature in the range of 649 ℃ to 800 ℃, which is the third stage, the weight loss of the polymer at this temperature is 16.8%, which is probably mainly due to the decomposition of the polymer main chain due to high temperature, and the final polymer species after the thermal analysis experiment is only 8.5% of the original mass. The main reason for the weight loss of the polymer is caused by the combination of molecules and water vapor within the polymer itself. In the low temperature stage, the polymer has high C-N, C-C and other bond binding force, so that the polymer has high price and high heat resistance. However, when the temperature exceeds 310 ℃, the polymer main chain will start to be broken and degraded. Meanwhile, the long-side chain of the gamma-MPS hydrophobic monomer and the AM macromolecular side group are introduced into the molecular chain, so that the heat resistance and the stability of the polymer are greatly improved.
2. Infrared spectrometry
Uniformly mixing the organic silicon gel plugging agent and potassium bromide according to a certain proportion, pressing for 5 minutes at the pressure of 2MPa to prepare a sheet, and utilizing an IR-TRacer-100 infrared series spectrophotometer at 400-4000cm-1Absorption spectra in the infrared region are obtained in the wavenumber range.
FIG. 2 shows that the molecular structure of the silicone gel plugging agent material is determined to contain all the structural functional groups of the reactants, and the silicone gel plugging agent material is a target product. Comparing FIG. 1 with FIG. 2, it can be seen that FIG. 2 is at 1210cm-1The characteristic peak of the asymmetric stretching vibration of Si-O appears, which proves that the original Si-OH is hydrolyzed and condensed to generate Si-O-Si bonds after the secondary crosslinking of the plugging agent.
3. Measurement of Performance
3.1 evaluation of plugging Properties
3.1.1 Sand bed experiment leakage of different mesh
The plugging performance of the organic silicon gel plugging agent is evaluated by adopting the following method: the indoor evaluation is carried out through a sand bed experiment, which is one of the main performances of the plugging agent, 250g of gravels screened into different meshes are respectively filled into different sand cylinders, the gravels are pressed and compacted by using a mould after being filled, so as to simulate loose and easily leaked stratum, the plugging agent which is completely gelatinized is added into 4.0 percent of drilling fluid base slurry and poured into the sand cylinders, when the temperature reaches the experiment set condition, a top valve is opened and the pressure is adjusted, the total filtration loss of 10min is recorded, if no filtration loss exists, the depth of liquid in the sand cylinders entering the sand bed is measured by using a steel ruler, the filtration loss in each group of experiments is lowest, or the plugging effect is best when the minimum liquid invasion depth exists in the sand bed, and the plugging bearing capacity under different pressures and different temperatures is researched and analyzed, so as to evaluate the plugging performance of the gel. By means of sand with different meshes, the leakage stoppage agent leakage loss conditions of different strata are simulated, and the change state of the leakage stoppage agent leakage loss under different pressures is researched and tested, and the specific result is shown in figure 4.
The experimental results show that: the experimental leakage of the sand beds with different meshes increases along with the increase of the pressure, and the leakage is relatively smaller when the meshes of the sand beds are larger, because the larger the meshes of the sand beds are, the smaller the simulated gaps of the sand beds are, the more difficult the leakage is. For the 10-20-mesh sand bed model experiment group, when the pressure is increased, the leakage amount is continuously increased, the leakage is caused due to the large gap of the leakage layer, and the leakage amount of 10min is only 2.13mL though the leakage amount is large in the 3 groups of sand bed simulation leakage layers. In comparison, in a 20-40-mesh sand bed simulation experiment group, the experiment pressure is set to be in a range of 1MPa to 5MPa, and the leakage loss is kept unchanged in the pressure lifting process, which indicates that the matching degree of the plugging agent in the range of 20-40 meshes and stratum gaps is the best, the plugging agent can easily enter a leakage layer to be matched with a leakage passage, the leakage passage is plugged through an adhesion effect, and when the pressure is increased to 6-7 MPa, the loss is continuously increased due to the fact that the pressure is large. For a 40-60-mesh sand bed simulation experiment group, no leakage occurs when the pressure is less than 2.4 MPa; when the pressure is more than 3MPa, the leakage increases along with the increase of the pressure, because the 40-60-mesh sand bed gap is smaller, the filtration is difficult to occur when the pressure is smaller, the leakage rapidly rises when the pressure is increased to 3-4 MPa, and the leakage basically keeps unchanged when the pressure is in the range of 4-6 MPa, because the gel is continuously extruded into the sand bed gap along with the increase of the pressure, and the leakage channel is blocked through the adhesion. The sand bed experiment proves that the gel plugging material has higher pressure-bearing plugging capability.
3.1.2 plugging Properties under different temperature conditions
The plugging performance of the organic silicon gel plugging agent under the high-temperature condition is evaluated through a high-temperature sand bed experiment, the relevance between the plugging agent and the sealing temperature is researched by means of setting of different temperatures, simulation is carried out on different easily-leaking stratum states by means of 10-20-mesh gravels, the testing temperatures are respectively 30 ℃, 80 ℃ and 150 ℃, the accumulated leakage amount for 10min is respectively recorded, and the corresponding relation between the pressure-sealing leakage amounts under different temperature conditions is shown in figure 5.
The experimental results show that: during the temperature rise, the initial fluid loss will be continuously increased, thus it can be demonstrated that the temperature rise will affect the initial plugging performance of the gel. When the temperature is 30 ℃, the leakage amount slowly rises along with the increase of the pressure; when the temperature is 80 ℃ and 140 ℃, the accumulated leakage amount within 10min is increased and then reduced in the process of continuously increasing the pressure, the main reason is that the gel cannot completely enter the gap to form leakage stoppage under the state of lower pressure, the gel enters the gap of a leakage layer simulated by the sand bed under the action of pressure to form effective leakage stoppage after the pressure is increased, and the leakage amount is basically kept unchanged when the pressure is increased from 6MPa to 7MPa, which indicates that the gel forms complete leakage stoppage. Therefore, when the pressure is 7MPa, the 10-20-mesh sandstone simulation leak layer has the leakage rate of 2mL in 10min at 30 ℃, the leakage rate of 2.5mL in 10min at 80 ℃ and the leakage rate of 3mL in 10min at 180 ℃. The high-temperature sand bed experiment proves that the gel plugging material still has better plugging performance under the high-temperature condition.
3.2 evaluation of viscoelasticity of Silicone gel plugging agent gel
The gel is formed by connecting macromolecules in a polymer solution under a certain condition to form a spatial network structure, and the fluidity of the polymer is reduced due to the increase of viscosity, so that the system is ensured to have uniform appearance. The elastic body shows the character that the strain develops along with the time and has elasticity, when the elastic body is acted by external stress, the stress can be converted into elastic deformation, when the stress is removed, the strain is gradually reduced, and the fluid can be gradually restored to the original shape; in the case of a viscous fluid, the action of the stress on the fluid itself is converted into the thermal energy of the fluid itself, and if the stress is released, the fluid will remain unchanged in the original state. By gel, it is meant a fluid in an intermediate state between a viscous fluid and an elastic fluid, which can be measured for its ability to displace formation fluids by viscoelasticity. For elastic fluids, according to the formula tan δ ═ G "/G', the closer G"/G is to 0, the stronger the elasticity of the gel is, and in the case where the phase angle δ does not exceed 20 °, the gel is in the linear viscoelastic region, i.e., tan δ < 1, the storage modulus is greater than the dissipation modulus, and the elasticity of the gel is stronger.
Adding water to the polymer in the step (1) of the example 2 to prepare an organic silicon polymer solution with the mass fractions of 5.0% and 6.0%, respectively adding 0.1% and 0.2% of cross-linking agents to the solution, placing the solution in a constant-temperature oven with the temperature of 70 ℃ to wait for gelling, and performing stress and frequency scanning on the gel by using a HAAKE RS6000 rheometer at the temperature of 30 ℃, wherein the experimental conditions of the stress scanning are as follows: the fixed frequency is 1Hz, and the stress amplitude is 0.1-100 Pa; the experimental conditions for the frequency sweep were: the fixed stress is 1Pa, the vibration frequency is 0.01-15Hz, and the experimental results are shown in FIG. 6 and FIG. 7.
As can be seen from fig. 6: the cross-linking agent has little influence on the viscoelasticity of a gel system, the addition of the polymer has great influence on the viscoelasticity of the gel, and the viscoelasticity of the gel is obviously enhanced as the addition of the polymer is increased from 5% to 6%. Under the condition of 1Hz, the stress is less than 75Pa, the gel is viscoelastic fluid, and the energy consumption modulus G 'and the storage modulus G' are basically not changed along with the change of the shear stress.
As can be seen from fig. 7: under the conditions that the stress is 1.0Pa and the corresponding vibration frequency is 0.01-15Hz, the storage modulus and the energy modulus are continuously improved when the vibration frequency is continuously improved, and the potential angle delta is always smaller than 20 degrees in the experimental frequency range through calculation, so that the gel can be concluded to belong to a linear viscoelastic region in the range, and the gel has good viscoelasticity under the condition.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. An organic silicon gel plugging agent is characterized in that: the organic silicon gel plugging agent is prepared by crosslinking an organic silicon polymer in water, wherein the organic silicon polymer is formed by polymerizing a vinyl monomer and an organic silicon monomer; the vinyl monomer is a combination of acrylic acid or acrylate monomer and amide compound;
the content of the vinyl monomer is 25-35% by mass of the organic silicon gel plugging agent; the organic silicon monomer accounts for 0.5 to 2.0 percent of the vinyl monomer.
2. The silicone gel lost circulation additive of claim 1, wherein: the organic silicon monomer is one or more of methyl vinyl chlorosilane, vinyl trichlorosilane and gamma-methacryloxypropyl trimethoxysilane; the content of the organic silicon monomer is 0.5-2.0% of the total mass of the vinyl monomer.
3. The silicone gel lost circulation additive of claim 1, wherein: the acrylate monomer is one or more of methyl acrylate, ethyl acrylate, butyl acrylate and octyl acrylate;
the amide compound is one or more of formamide, acetamide, propionamide, acrylamide, N-dimethylformamide, benzamide and succinimide.
4. A silicone polymer characterized by: the organic silicon polymer is formed by polymerizing a vinyl monomer and an organic silicon monomer; the vinyl monomer is a combination of an acrylic acid or acrylate monomer and an amide compound.
5. A method for producing the silicone polymer according to claim 4, characterized in that: the preparation method comprises the steps of carrying out polymerization reaction on a vinyl monomer and an organic silicon monomer at 50-60 ℃ in the presence of an initiator and a buffer; the polymerization reaction is solution polymerization.
6. The method of preparing the silicone polymer of claim 5, wherein: the initiator is a redox initiator combination;
the redox initiator combination is one of ammonium persulfate/sodium bisulfite, potassium persulfate/sodium bisulfite, ammonium persulfate/ferrous sulfate, hydrogen peroxide/ferrous sulfate, benzoyl peroxide/N, N-diethylaniline, potassium persulfate/silver nitrate or persulfate/mercaptan oxidation combination;
the amount of the initiator is 0.2 to 0.5 percent of the total amount of the vinyl monomer;
the molar ratio of the oxidant to the reductant is 1-2: 1-2.
7. The method of preparing the silicone polymer of claim 5, wherein: the method specifically comprises the following steps:
(1) fully dissolving a vinyl monomer in deionized water to obtain a solution A;
(2) dissolving an initiator and a buffering agent in deionized water to obtain a solution B;
(3) adjusting the pH value of the solution A to 4-6 by using a sodium hydroxide solution, adding an organic silicon monomer, mixing with the solution B, and stirring to prepare a suspension;
(4) stirring the suspension at a constant temperature of 50-60 ℃ for reaction for 6-8h to obtain a synthetic product;
(5) and (4) repeatedly washing the synthetic product obtained in the step (4) by using absolute ethyl alcohol, and performing suction filtration and drying to obtain the organic silicon polymer.
8. A method for preparing the silicone gel plugging agent as defined in claim 1, characterized in that: the method comprises the following specific steps:
adding the organic silicon polymer in the claim 4 or the organic silicon polymer prepared by the method in any one of the claims 5 to 7 into deionized water for fully dissolving, and adjusting the pH of the solution to 6 to 8 by using sodium hydroxide solution to obtain solution 1;
adding a cross-linking agent into the solution 1 and stirring; the addition amount of the cross-linking agent is 0.05-0.4% of the total amount of the vinyl monomer, and viscoelastic fluid, namely the organic silicon gel plugging agent liquid product, is obtained.
9. The method of claim 8, wherein: the dissolution is carried out under low-speed stirring, and the rotating speed of the low-speed stirring is 150-;
the cross-linking agent in the step (II) is selected from one or more of tetraethoxysilane, methyl orthosilicate, trimethoxy silane and acrylate compounds; the cross-linking agent is dissolved in deionized water in advance when in use to prepare a solution with the mass concentration of 35-45%; the stirring speed of the step II is 800-.
10. Use of the silicone polymer gel plugging agent according to claim 1 or the silicone gel plugging agent prepared by the method according to any one of claims 8-9 as a plugging agent for water-based drilling fluids.
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