CN114479783B - Composite plugging material and preparation method and application thereof - Google Patents

Composite plugging material and preparation method and application thereof Download PDF

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Publication number
CN114479783B
CN114479783B CN202011166416.2A CN202011166416A CN114479783B CN 114479783 B CN114479783 B CN 114479783B CN 202011166416 A CN202011166416 A CN 202011166416A CN 114479783 B CN114479783 B CN 114479783B
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structural unit
starch
vinyl
composite
monomer
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CN114479783A (en
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赵凯强
韩洁
王晨
肖俊杰
曾虹钢
杨超
赵林
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Sinopec Dalian Petrochemical Research Institute Co ltd
China Petroleum and Chemical Corp
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China Petroleum and Chemical Corp
Sinopec Dalian Research Institute of Petroleum and Petrochemicals
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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
    • C09K8/02—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
    • E—FIXED CONSTRUCTIONS
    • E21—EARTH DRILLING; MINING
    • E21B—EARTH DRILLING, e.g. DEEP DRILLING; OBTAINING OIL, GAS, WATER, SOLUBLE OR MELTABLE MATERIALS OR A SLURRY OF MINERALS FROM WELLS
    • E21B21/00—Methods or apparatus for flushing boreholes, e.g. by use of exhaust air from motor
    • 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
    • C09K2208/00—Aspects relating to compositions of drilling or well treatment fluids
    • C09K2208/08—Fiber-containing well treatment fluids
    • 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
    • C09K2208/00—Aspects relating to compositions of drilling or well treatment fluids
    • C09K2208/10—Nanoparticle-containing well treatment fluids

Abstract

The invention discloses a composite plugging material and a preparation method and application thereof, wherein the composite plugging material comprises a crosslinked polymer, fibers and elastic particle materials; the crosslinked polymer comprises a structural unit A, a structural unit B, a structural unit D and a structural unit E; the structural unit B and the structural unit E are connected through a structural unit D; the structural unit A is starch; the structural unit B is a vinyl monomer-containing structural unit; the structural unit D is a silane coupling agent structural unit; the structural unit E is a clay mineral unit. And uniformly mixing the crosslinked polymer, the fiber and the elastic particle material to obtain the composite plugging material. The plugging material has the characteristics of high structural rigidity and high bearing capacity.

Description

Composite plugging material and preparation method and application thereof
Technical Field
The invention belongs to the technical field of petroleum exploitation, and particularly relates to a composite plugging material and a preparation method thereof.
Background
Lost circulation problems have been a technical problem that plagues global sites. Lost circulation generally occurs under conditions where the pressure of the working fluid in the wellbore is greater than the pore pressure of the fluid in the formation pores, fractures or vugs, and where there are lost circulation channels and large fluid-containing spaces in the formation. Common plugging methods fall into eight general categories: (1) adjusting drilling fluid properties; (2) static plugging method; (3) bridging material plugging method; (4) a high-fluid loss slurry plugging method; (5) temporary plugging method; (6) chemical plugging method; (7) inorganic gel plugging method; and (8) a composite plugging method. Conventional plugging materials are generally classified into four categories: particles, flakes, fibers, and mixtures of two or more of the foregoing. The plugging material is indispensable in the well drilling leakage prevention process, and the performance of the plugging material has important influence on the well drilling leakage prevention and leakage prevention.
CN106928938A discloses a plugging agent for inert materials while drilling, a preparation method and a use method thereof, wherein the plugging agent for inert materials while drilling comprises, by weight, 50 to 80 parts of rigid materials of 100 meshes to 150 meshes and 30 to 70 parts of mineral fibers of 100 meshes to 120 meshes. The plugging performance of the plugging agent of the partially acid-soluble rigid material is superior to that of the plugging agent sold in the domestic common market, and is equivalent to that of the plugging agent at abroad, and the cost of the plugging agent of the partially acid-soluble rigid material is lower than that of the plugging agent at abroad because the source of the raw materials of the plugging agent of the partially acid-soluble rigid material is wide and the raw materials are low, so that the cost performance of the plugging agent of the partially acid-soluble rigid material is superior to that of the plugging agent at abroad, and the plugging agent of the partially acid-soluble rigid material provides technical support for improving the complex treatment efficiency of well leakage.
CN110105934a discloses an acid-soluble pressure-bearing plugging agent for drilling fluid and a preparation method thereof, wherein the raw materials are as follows in parts by weight: 20-30 parts of crop straw extracted fiber, 5-10 parts of polyester fiber, 5-10 parts of cellulose acetate, 10-20 parts of glass fiber, 5-10 parts of asbestos fiber, 10-20 parts of cotton-hemp plant fiber, 10-20 parts of rock-making mineral powder, 5-10 parts of alginate, 3-5 parts of dimethyl diallyl ammonium chloride, 3-5 parts of polyvinyl acetate, 1-5 parts of alpha-n-octyl cyanoacrylate, 1-4 parts of diatomite and a proper amount of clear water. The acid-soluble pressure-bearing plugging agent for the drilling fluid and the preparation method thereof can realize that fibers extracted from crop straws with lower cost are adopted as main raw materials of the plugging agent, so that the purposes of saving the production cost of the plugging agent while guaranteeing the plugging effect and the pressure-bearing effect of the plugging agent are well achieved, the plugging effect of the plugging agent is greatly enhanced, the pressure-bearing capacity of the plugging agent is improved, the production cost of the plugging agent raw materials is saved, and the purposes of saving energy and protecting environment are well achieved.
Disclosure of Invention
Aiming at the defects of the prior art, the invention mainly aims to provide a composite plugging material, a preparation method and application thereof, and the composite plugging material has the advantages of good high temperature resistance, high pressure bearing capacity, environmental protection in production and application and the like.
The first aspect of the invention provides a composite plugging material, which comprises a crosslinked polymer, fibers and elastic particle materials; the crosslinked polymer comprises a structural unit A, a structural unit B, a structural unit D and a structural unit E; the structural unit B and the structural unit E are connected through a structural unit D; the structural unit A is starch; the structural unit B is a vinyl monomer-containing structural unit; the structural unit D is a silane coupling agent structural unit; the structural unit E is a clay mineral unit;
the crosslinked polymer has the following structural formula:
wherein R is H or CH 3 ；R 1 Si may be used to represent a vinylsilane monomer; may also beRepresents a gamma-methacryloxypropyl silane monomer; si in the structure forms a covalent bond Si-O-Si with HO-Si in the clay mineral;
the structural formula of the structural unit B isOr->The method comprises the steps of carrying out a first treatment on the surface of the Wherein R is 2 And R is 4 Is the side chain structure of the vinyl polymer except the vinyl structure, m is the polymerization degree of the starch structural unit, x is the polymerization degree of the vinyl monomer, y is the vinyl silane monomerM+x+y=800 to 1800.
Further, based on the total weight of the composite plugging material, the cross-linked polymer accounts for 30-60 wt%, the fiber accounts for 20-40 wt% and the elastic particle material accounts for 20-40 wt%.
Further, in the above composite plugging agent, the fiber may be one or more of crop straw extracted fiber, polyester fiber, cellulose acetate, glass fiber, asbestos fiber, cotton-hemp plant fiber, etc., preferably polyester fiber and glass fiber. The diameter of the fiber is 0.05-1 mm, and the length is 0.5-10 mm.
Further, in the composite plugging agent, the elastic particle material may be one or more selected from rubber particles, resin particles and the like, and the particle size of the elastic particles is 20-40 mesh. The rubber particles are mainly produced by processing various waste rubber, including waste rubber, leftover materials, cable jackets, automobile tires and other waste rubber raw materials, and comprise natural rubber, butyl rubber, nitrile rubber, ethylene propylene rubber, styrene butadiene rubber, butadiene rubber and the like. The resin particles are produced by processing various waste resins including polyethylene, polyvinyl chloride, polystyrene, polypropylene, ABS resin and other waste raw materials.
Further, based on the total weight of the crosslinked polymer, the content of the structural unit A in the crosslinked polymer is 20 to 65wt%, the content of the structural unit B is 10 to 45wt%, the content of the structural unit D is 8 to 35wt%, and the content of the structural unit E is 8 to 35wt%.
Furthermore, in the composite plugging material, the starch can be one or more of mung bean starch, tapioca starch, sweet potato starch, wheat starch, water chestnut starch, lotus root starch and corn starch, and preferably corn starch and/or potato starch.
Further, in the composite plugging material, the vinyl-containing monomer is a water-soluble vinyl monomer and can be one or more of a cationic monomer, an anionic monomer, a nonionic monomer and a zwitterionic monomer. Further, the zwitterionic monomer is one or more of methacryloxyethyl-N, N-dimethyl propane sulfonate (DMAPS), N-dimethyl allyl amine propane sulfonate (DAPS), 4-Vinyl Pyridine Propane Sulfonate (VPPS), N-methyl diallyl propane sulfonate (MAPS) and N-methyl diallyl butane sulfonate (MABS), and is preferably N-methyl diallyl propane sulfonate. The cationic monomer is one or more of methacryloxyethyl trimethyl ammonium chloride (DMC), acryloxyethyl trimethyl ammonium chloride (DAC), acryloxyethyl dimethyl benzyl ammonium chloride (DBC), dimethyl diallyl ammonium chloride (DMDAAC) and diethyl diallyl ammonium chloride (DEDAAC), preferably dimethyl diallyl ammonium chloride. The anionic monomer is one or more of AA (acrylic acid), 2-methyl-2-acrylamidopropane sulfonic Acid (AMPS), fumaric Acid (FA), sodium allylsulfonate (SSS) and sodium 2-acryloyloxyisopentene sulfonate (AOIAS), and preferably 2-methyl-2-acrylamidopropane sulfonic acid. The nonionic monomer is one or more of N-vinyl pyrrolidone (NVP), acrylonitrile (AN), vinyl formamide (NVF) and vinyl acetamide (NVA), preferably N-vinyl pyrrolidone.
Further, in the composite plugging material, the silane coupling agent is a silane coupling agent containing vinyl or gamma-methacryloxypropyl; more specifically, the silane coupling agent in the method of the present invention is one or more of vinyltrichlorosilane, vinyltriethoxysilane, vinyltrimethoxysilane, vinyl (2-methoxyethoxy) silane, vinyltriacetoxysilane, vinylt-butylperoxy silane, vinylmethyldichlorosilane, gamma-methacryloxypropyl trichlorosilane, gamma-methacryloxypropyl trimethoxysilane, gamma-methacryloxypropyl methyldiethoxysilane, gamma-methacryloxypropyl methyldimethoxy silane, preferably one or more of vinyltrichlorosilane, vinyltriethoxysilane, vinyltrimethoxysilane, gamma-methacryloxypropyl trichlorosilane, gamma-methacryloxypropyl trimethoxysilane, and more preferably one or more of vinyltrichlorosilane and gamma-methacryloxypropyl trimethoxysilane.
Further, in the composite plugging material, the clay mineral is one or more of kaolinite, montmorillonite, illite, sepiolite and attapulgite, preferably one or more of kaolinite, montmorillonite and illite, and more preferably montmorillonite.
The second aspect of the invention provides a preparation method of the composite plugging material, wherein the composite plugging material is obtained by uniformly mixing the crosslinked polymer, the fiber and the elastic particle material.
The third aspect of the invention provides a drilling fluid, which comprises the composite plugging material, wherein the content of the composite plugging material is 0.5-20wt%, preferably 2-10wt%, and more preferably 3-7wt% based on the total weight of the drilling fluid. The drilling fluid added with the composite plugging material has good plugging capability, can effectively plug pores or micro-cracks, prevent filtrate from penetrating into stratum in a large amount, reduce filtrate loss and play a good role in plugging.
The fourth aspect of the invention provides the use of the composite lost circulation material described above in a drilling process.
When the composite plugging material is used in the drilling process, the addition amount is 0.1-5 wt%, preferably 0.5-5 wt%, and more preferably 1-5 wt%.
Compared with the prior art, the composite plugging material provided by the invention and the preparation method and application thereof have the following advantages:
1. the composite plugging material is formed by compounding high-temperature-resistant crosslinked polymers, high-temperature-resistant fibers and elastic particle materials, wherein the high-temperature-resistant fibers are long rods, the elastic particle materials are spherical, the elastic particle materials have good viscoelasticity at high temperature, multiple layers of irregular accumulation can be formed with the high-temperature-resistant fibers, the reinforcing consolidation of the high-temperature-resistant crosslinked polymers is assisted, and the pressure bearing capacity of the plugging material is greatly improved.
2. The plugging material provided by the invention uses the vinyl polymerization monomer grafted modified starch, so that the starch has functionality, and the temperature resistance, salt resistance and calcium resistance of the plugging agent in drilling fluid are improved besides the plugging property of the plugging agent.
3. In the preparation method of the plugging material, the silane coupling agent is used for combining the organic starch and the inorganic clay mineral, so that on one hand, the structural rigidity of the material is improved, and the pressure bearing capacity of the plugging material is improved. On the other hand, the viscosity of the grafted starch part in the plugging material is high after the grafted starch part is dissolved in water, so that clay minerals of inert parts can be tightly connected with a stratum, the interface effect is enhanced, and the bearing capacity is further improved. The clay mineral has the same lithology as the stratum, and the structure containing silicon and oxygen is further condensed under high temperature and high pressure to form a bonding structure, so that the plugging and bearing capacity under high temperature and high pressure is greatly improved.
4. In the preparation method of the plugging material, the clay mineral structure is subjected to graft copolymerization with starch through the vinyl silane coupling agent, and the clay mineral structure is not subjected to cross-linking reaction with the starch directly. The clay mineral content ratio is adjustable, and even under the condition of high temperature higher than 180 ℃, the clay mineral side chain is still reserved due to the decomposition of the starch structure and the fracture of the main chain of the polymer, and the plugging material always keeps better bearing capacity. The temperature resistance of the plugging material can reach more than 180 ℃.
Detailed Description
The composite plugging material, the preparation method and the application thereof are further described below by specific examples, but the invention is not limited thereto.
The preparation method of the cross-linked polymer comprises the following steps:
(1) Preparation of Material A
Uniformly mixing a silane coupling agent, an organic solvent and a clay mineral, reacting for 1-5 hours at 30-90 ℃, separating, and drying for 8-16 hours at 60-120 ℃ to obtain a material A; the dosage of the organic solvent is 2-8 times of the weight of the clay mineral, and the dosage of the silane coupling agent is 25-400 wt% of the weight of the clay mineral. The organic solvent can be one or more of methanol, ethanol, propanol, butanol, methyl formate, ethyl acetate, ethyl formate, methyl acetate, butyl acetate and the like, and preferably one or more of methyl formate, ethyl acetate, ethyl formate and methyl acetate.
(2) Preparation of gelatinized starch
Mixing starch and water at 50-100 ℃, preferably 80-95 ℃, and uniformly mixing to obtain gelatinized starch; the mass fraction of starch in the gelatinized starch is 5-20wt%.
(3) Preparation of emulsion B
Uniformly mixing the material A obtained in the step (1), the gelatinized starch obtained in the step (2), the vinyl-containing monomer, the surfactant and the water to obtain emulsion B; the weight ratio of the material A to the gelatinized starch to the vinyl-containing monomer is 1: 1-20: 1 to 15; the weight of the water is 1 to 5 times of the total weight of the material A, the gelatinized starch and the vinyl monomer, and the mass of the surfactant is 0.1 to 5 percent of the mass of the water.
The surfactant is an anionic surfactant or a nonionic surfactant; wherein the anionic surfactant can be one or more of sodium dodecyl benzene sulfonate, sodium dodecyl sulfate, sodium alkyl polyoxyethylene ether sulfate and sodium alkyl polyoxyethylene ether carboxylate, preferably sodium dodecyl benzene sulfonate and/or sodium dodecyl sulfate; the nonionic surfactant can be one or more of long-chain fatty alcohol polyoxyethylene ether, alkylphenol polyoxyethylene ether, fatty acid polyoxyethylene ester, polyoxyethylene alkylamine, polyoxyethylene alkylamide and polyether, and is preferably alkylphenol polyoxyethylene ether and/or fatty acid polyoxyethylene ester.
(4) Preparation of crosslinked polymers
And (3) contacting the emulsion B with an initiator to react for 2-6 hours at 40-90 ℃, and washing and drying after the reaction is finished to obtain the plugging material.
The initiator is one or more of potassium persulfate, sodium persulfate and ammonium persulfate; the initiator is used in an amount of 0.5 to 1.5 weight percent based on the total mass of the material A, the gelatinized starch and the vinyl-containing monomer.
The washing is generally carried out by washing with water for several times, and the drying is carried out for 8-16 h at 80-120 ℃.
In the above method for producing a crosslinked polymer, the separation in step (1) is a liquid-solid separation, and the solvent is separated. Any one of the existing liquid-solid separation means in the art can be adopted, and a person skilled in the art can select the liquid-solid separation means according to the actual needs according to routine knowledge. Specifically, one or more of the modes of standing, layering, filtering, centrifugal separation and the like can be adopted.
Example 1
20g of vinyltriethoxysilane and 30g of kaolin are weighed, added into 300ml of ethanol, fully stirred and dispersed, heated to 60 ℃ for reaction for 3 hours to obtain a material A, and then centrifuged to separate, and the solid is dried for 12 hours at 90 ℃ for standby. 30g of corn starch was prepared as a suspension of 20wt% water and reacted at 90℃for 2 hours to give gelatinized starch. 25g of methacryloyloxyethyl-N, N-dimethylpropanesulfonate was taken and prepared as a 45wt% aqueous solution. The material A, gelatinized starch and monomer solution are added into 220g of water which is used for dissolving 3g of sodium dodecyl benzene sulfonate, and the mixture is fully stirred, emulsified and dispersed. After the temperature was raised to 65 ℃, 1.5g of ammonium persulfate was added and the reaction was carried out for 3 hours. Washing with deionized water for 2 times after the reaction is finished, drying at 110 ℃ for 8 hours, and crushing to finally obtain the crosslinked polymer. And uniformly mixing the crosslinked polymer with 45g of glass fiber and 45g of resin particles to obtain the final composite plugging material.
Example 2
7.5g of vinyl trichlorosilane and 30g of kaolin are weighed, added into 300ml of ethanol, fully stirred and dispersed, heated to 90 ℃ for reaction for 1h, material A is obtained, centrifugal separation is carried out, and the solid is dried for 12h at 90 ℃ for standby. 30g of corn starch is prepared into a suspension of 20% water, and the suspension is reacted for 1h at 95 ℃ to obtain gelatinized starch. 25g of N, N-dimethylallylamine propanesulfonate was taken and formulated as a 60% aqueous solution. The material A, gelatinized starch and monomer solution are added into 200g of water which is dissolved with 10g of sodium dodecyl benzene sulfonate, and the mixture is fully stirred, emulsified and dispersed. After the temperature was raised to 90 ℃, 1.3g of ammonium persulfate was added and reacted for 2 hours. Washing with deionized water for 2 times after the reaction is finished, drying at 120 ℃ for 10 hours, and crushing to finally obtain the crosslinked polymer. And uniformly mixing the crosslinked polymer with 40g of glass fiber and 40g of rubber particles to obtain the final composite plugging material.
Example 3
30g of vinyltrimethoxysilane and 30g of montmorillonite are weighed, added into 300ml of methanol, fully stirred and dispersed, heated to 80 ℃ for reaction for 2 hours to obtain a material A, and then centrifuged to separate, and the solid is dried for 8 hours at 120 ℃ for standby. 30g of potato starch is prepared into a suspension of 15% water, and the suspension is reacted for 2 hours at 90 ℃ to obtain gelatinized starch. 25g of methacryloyloxyethyl trimethylammonium chloride was prepared as a 40% aqueous solution. The material A, gelatinized starch and monomer solution are added into 230g of water which is dissolved with 0.23g of sodium dodecyl sulfate, and the mixture is fully stirred, emulsified and dispersed. After heating to 60 ℃, 1.6g of sodium persulfate was added and the reaction was carried out for 4 hours. Washing with deionized water for 2 times after the reaction is finished, drying at 100 ℃ for 8 hours, and crushing to finally obtain the crosslinked polymer. And uniformly mixing the crosslinked polymer, 60g of polyester fiber and 60g of resin particles together to obtain the final composite plugging material.
Example 4
100g of vinyl (2-methoxyethoxy) silane and 30g of montmorillonite are weighed, added into 300ml of methyl formate, fully stirred and dispersed, heated to 60 ℃ for reaction for 3 hours, material A is obtained, centrifugal separation is carried out, and the solid is dried for 8 hours at 120 ℃ for standby. 30g of potato starch is prepared into a suspension of 5% water, and the suspension is reacted for 1h at 95 ℃ to obtain gelatinized starch. 40g of acryloyloxyethyl trimethylammonium chloride was prepared as a 30% aqueous solution. The material A, gelatinized starch and monomer solution are added into 300g of water which is dissolved with 5g of sodium alkyl polyoxyethylene ether sulfate, and the mixture is fully stirred, emulsified and dispersed. After heating to 65 ℃, 2.5g of sodium persulfate was added and the reaction was carried out for 3 hours. Washing with deionized water for 2 times after the reaction is finished, drying at 90 ℃ for 15 hours, and crushing to finally obtain the crosslinked polymer. And uniformly mixing the crosslinked polymer, 70g of polyester fiber and 70g of rubber particles to obtain the final composite plugging material.
Example 5
50g of vinyl tertiary butyl silane triperoxide and 30g of illite are weighed, added into 300ml of ethyl acetate, fully stirred and dispersed, heated to 60 ℃ for reaction for 3 hours to obtain a material A, and then centrifuged to separate, and the solid is dried at 60 ℃ for 16 hours for standby. 30g of mung bean starch is prepared into a suspension of 20% water, and the suspension is reacted for 5 hours at 85 ℃ to obtain gelatinized starch. 40g of 2-methyl-2-acrylamidopropane sulfonic acid was taken and prepared as a 45% aqueous solution. The material A, gelatinized starch and monomer solution are added into 280g of water which is used for dissolving 4g of alkylphenol ethoxylate, and the mixture is fully stirred, emulsified and dispersed. After the temperature is raised to 90 ℃, 2g of potassium persulfate is added for reaction for 2 hours. Washing with deionized water for 2 times after the reaction is finished, drying at 80 ℃ for 16 hours, and crushing to finally obtain the crosslinked polymer. And uniformly mixing the crosslinked polymer with 75g of asbestos fiber and 75g of resin particles to obtain the final composite plugging material.
Example 6
30g of vinylmethyldichlorosilane and 30g of illite are weighed, added into 300ml of ethyl formate, fully stirred and dispersed, heated to 30 ℃ for reaction for 5 hours to obtain a material A, and then centrifuged to separate, and the solid is dried at 90 ℃ for 12 hours for standby. 30g of tapioca starch is prepared into a suspension of 20% water, and the suspension is reacted for 3 hours at 85 ℃ to obtain gelatinized starch. 20g of fumaric acid was prepared as a 30% aqueous solution. The material A, gelatinized starch and monomer solution are added into 230g of water which is used for dissolving 2.5g of fatty acid polyoxyethylene ester, and the mixture is fully stirred, emulsified and dispersed. After heating to 40 ℃, 1.5g of potassium persulfate is added for reaction for 6 hours. Washing with deionized water for 2 times after the reaction is finished, drying at 95 ℃ for 12 hours, and crushing to finally obtain the crosslinked polymer. And uniformly mixing the crosslinked polymer with 50g of asbestos fiber and 50g of rubber particles to obtain the final composite plugging material.
Example 7
60g of gamma-methacryloxypropyl trichlorosilane and 30g of sepiolite are weighed, added into 300ml of methyl acetate, fully stirred and dispersed, heated to 50 ℃ for reaction for 3 hours to obtain a material A, and then centrifuged to separate, and the solid is dried for 12 hours at 90 ℃ for standby. 30g of water chestnut starch is prepared into a suspension of 15% water, and the suspension is reacted for 2 hours at 90 ℃ to obtain gelatinized starch. 40g of N-vinylpyrrolidone was taken and prepared into a 50% aqueous solution. The material A, gelatinized starch and monomer solution are added into 250g of water for dissolving 3g of polyoxyethylene alkylamine, and the mixture is fully stirred, emulsified and dispersed. After heating to 50 ℃, 2g of potassium persulfate is added for reaction for 4 hours. Washing with deionized water for 2 times after the reaction is finished, drying for 14h at 90 ℃, and crushing to finally obtain the crosslinked polymer. And uniformly mixing the crosslinked polymer with 65g of cellulose acetate and 65g of resin particles to obtain the final composite plugging material.
Example 8
70g of vinyltriethoxysilane and 30g of montmorillonite are weighed, added into 300ml of ethanol, fully stirred and dispersed, heated to 60 ℃ for reaction for 3 hours, material A is obtained, and then the material A is centrifugally separated, and the solid is dried for 10 hours at 120 ℃ for standby. 30g of corn starch is prepared into a suspension of 10% water, and the suspension is reacted for 2 hours at 95 ℃ to obtain gelatinized starch. 40g of acrylonitrile was prepared as a 40% aqueous solution. The material A, gelatinized starch and monomer solution are added into 300g of water for dissolving 6g of polyoxyethylene alkylamide, and the mixture is fully stirred, emulsified and dispersed. After the temperature was raised to 70 ℃, 2g of ammonium persulfate was added and the reaction was carried out for 3 hours. Washing with deionized water for 2 times after the reaction is finished, drying at 80 ℃ for 10 hours, and crushing to finally obtain the crosslinked polymer. And uniformly mixing the crosslinked polymer with 85g of polyester fiber and 85g of rubber particles to obtain the final composite plugging material.
Comparative example 1
Substantially the same as in example 1, except that vinyltriethoxysilane was not added.
Comparative example 2
Substantially the same as in example 1, except that methacryloyloxyethyl-N, N-dimethylpropanesulfonate was not added.
Samples of the examples and the comparative examples were taken, and under the condition of an addition of 5wt%, the pressure bearing capacity test was performed by using a QD-2 type plugging instrument and selecting different slit plates. The test results are shown in tables 1 and 2. The test slurry is mixed salt water-based slurry, and the preparation method comprises the following steps: 40g of test soil is weighed and added into 1000mL of water, 1.4g of anhydrous sodium carbonate is added, and 100g of NaCl and 50g of CaCl are added after stirring for 20min 2 And (5) sealing and curing for 24 hours at room temperature for standby. Before testing the bearing capacity, 350mL of base slurry is added with 5wt% of plugging material, stirred for 20min, then added into an aging kettle, rolled and aged for 16h at 180 ℃, cooled, taken out and stirred for 20min, and then tested for the bearing capacity.
Table 1 results of test of pressure bearing ability of sample on 1mm slit plate
Sequence number Sample of Pressure bearing capacity/MPa
1 Example 1 7.3
2 Example 2 6.9
3 Example 3 7.2
4 Example 4 7.0
5 Example 5 7.6
6 Example 6 7.5
7 Example 7 7.4
8 Example 8 7.6
9 Comparative example 1 4.6
10 Comparative example 2 3.6
Table 2 results of test of the bearing ability of the sample in the 3mm slit plate
Sequence number Sample of Pressure bearing capacity/MPa
1 Example 1 6.5
2 Example 2 6.6
3 Example 3 6.7
4 Example 4 6.4
5 Example 5 6.8
6 Example 6 6.6
7 Example 7 6.7
8 Example 8 6.9
9 Comparative example 1 3.5
10 Comparative example 2 3.0

Claims (19)

1. A composite plugging material, which comprises a cross-linked polymer, fibers and elastic particle materials; the crosslinked polymer comprises a structural unit A, a structural unit B, a structural unit D and a structural unit E;
the structural unit B and the structural unit E are connected through a structural unit D; the structural unit A is connected with the structural unit B;
the structural unit A is a starch structural unit; the structural unit B is a vinyl monomer-containing structural unit; the structural unit D is a silane coupling agent structural unit; the structural unit E is a clay mineral unit;
wherein the vinyl-containing monomer is a water-soluble vinyl monomer and comprises one or more of a cationic monomer, an anionic monomer, a nonionic monomer and a zwitterionic monomer; the zwitterionic monomer is one or more of methacryloxyethyl-N, N-dimethyl propane sulfonate (DMAPS), N-Dimethyl Allylamine Propane Sulfonate (DAPS), 4-Vinyl Pyridine Propane Sulfonate (VPPS), N-methyl diallyl propane sulfonate (MAPS) and N-methyl diallyl butane sulfonate (MABS); the cationic monomer is one or more of methacryloxyethyl trimethyl ammonium chloride (DMC), acryloxyethyl trimethyl ammonium chloride (DAC), acryloxyethyl dimethyl benzyl ammonium chloride (DBC), dimethyl diallyl ammonium chloride (DMDAAC) and diethyl diallyl ammonium chloride (DEDAAC); the anionic monomer is one or more of AA (acrylic acid), 2-methyl-2-acrylamidopropane sulfonic Acid (AMPS), fumaric Acid (FA), sodium allylsulfonate (SSS) and sodium 2-acryloyloxyisopentene sulfonate (AOIAS); the nonionic monomer is one or more of N-vinyl pyrrolidone (NVP), acrylonitrile (AN), vinyl formamide (NVF) and vinyl acetamide (NVA);
the silane coupling agent structural unit is one or more of vinyl trichlorosilane, vinyl triethoxysilane, vinyl trimethoxysilane, vinyl (2-methoxyethoxy) silane, vinyl triacetoxy silane, vinyl tert-butylperoxy silane, vinyl methyldichlorosilane, gamma-methacryloxypropyl trichlorosilane, gamma-methacryloxypropyl trimethoxysilane, gamma-methacryloxypropyl methyl diethoxy silane and gamma-methacryloxypropyl methyl dimethoxy silane;
the sum of the polymerization degree of the starch structural unit, the polymerization degree of the vinyl monomer and the polymerization degree of the vinyl silane monomer is 800-1800;
the fibers comprise one or more of crop straw extracted fibers, polyester fibers, cellulose acetate, glass fibers, asbestos fibers and cotton numbness plant fibers; the diameter of the fiber is 0.05-1 mm, and the length is 0.5-10 mm;
the elastic particle material comprises one or two of rubber particles and resin particles, and the particle size is 20-40 meshes;
the preparation method of the crosslinked polymer comprises the following steps:
(1) Preparation of Material A
Uniformly mixing a silane coupling agent, an organic solvent and a clay mineral, reacting for 1-5 hours at 30-90 ℃, separating, and drying for 8-16 hours at 60-120 ℃ to obtain a material A; the dosage of the organic solvent is 2-8 times of the weight of the clay mineral, and the dosage of the silane coupling agent is 25-400 wt% of the weight of the clay mineral; the organic solvent is one or more of methanol, ethanol, propanol, butanol, methyl formate, ethyl acetate, ethyl formate, methyl acetate and butyl acetate;
(2) Preparation of gelatinized starch
Mixing starch and water at 50-100 ℃ uniformly to obtain gelatinized starch; the mass fraction of starch in the gelatinized starch is 5-20wt%;
(3) Preparation of emulsion B
Uniformly mixing the material A obtained in the step (1), the gelatinized starch obtained in the step (2), the vinyl-containing monomer, the surfactant and the water to obtain emulsion B; the weight ratio of the material A to the gelatinized starch to the vinyl-containing monomer is 1: 1-20: 1 to 15; the weight of the water is 1 to 5 times of the total weight of the material A, the gelatinized starch and the vinyl monomer, and the mass of the surfactant is 0.1 to 5 percent of the mass of the water;
the surfactant is an anionic surfactant or a nonionic surfactant; wherein the anionic surfactant is one or more of sodium dodecyl benzene sulfonate, sodium dodecyl sulfate, sodium alkyl polyoxyethylene ether sulfate and sodium alkyl polyoxyethylene ether carboxylate; the nonionic surfactant is one or more of long-chain fatty alcohol polyoxyethylene ether, alkylphenol polyoxyethylene ether, fatty acid polyoxyethylene ester, polyoxyethylene alkylamine, polyoxyethylene alkylamide and polyether;
(4) Preparation of crosslinked polymers
And (3) contacting the emulsion B with an initiator to react for 2-6 hours at 40-90 ℃, and washing and drying after the reaction is finished to obtain the crosslinked polymer.
2. The composite lost circulation material of claim 1, wherein: based on the total weight of the composite plugging material, the cross-linked polymer accounts for 30-60 wt%, the fiber accounts for 20-40 wt% and the elastic particle material accounts for 20-40 wt%.
3. The composite lost circulation material of claim 1, wherein: based on the total weight of the crosslinked polymer, the content of the structural unit A in the crosslinked polymer is 20-65 wt%, the content of the structural unit B is 10-45 wt%, the content of the structural unit D is 8-35 wt%, and the content of the structural unit E is 8-35 wt%.
4. The composite lost circulation material of claim 1, wherein: the starch is one or more of mung bean starch, tapioca starch, sweet potato starch, wheat starch, water chestnut starch, lotus root starch and corn starch.
5. The composite lost circulation material of claim 4, wherein: the starch is corn starch and/or potato starch.
6. The composite lost circulation material of claim 1, wherein: the zwitterionic monomer is N-methyl diallyl propane sulfonate.
7. The composite lost circulation material of claim 1, wherein: the cationic monomer is dimethyl diallyl ammonium chloride.
8. The composite lost circulation material of claim 1, wherein: the anionic monomer is 2-methyl-2-acrylamidopropane sulfonic acid.
9. The composite lost circulation material of claim 1, wherein: the nonionic monomer is N-vinyl pyrrolidone.
10. The composite lost circulation material of claim 1, wherein: the clay mineral is one or more of kaolinite, montmorillonite, illite, sepiolite and attapulgite.
11. The composite lost circulation material of claim 10, wherein: the clay mineral is one or more of kaolinite, montmorillonite and illite.
12. The composite lost circulation material of claim 10, wherein: the clay mineral is montmorillonite.
13. The method for preparing the composite plugging material according to any one of claims 1 to 12, wherein the crosslinked polymer, the fiber and the elastic particle material are uniformly mixed to obtain the composite plugging material.
14. A drilling fluid comprising the composite lost circulation material of any one of claims 1-12, wherein the composite lost circulation material comprises 0.5-20 wt% based on the total weight of the drilling fluid.
15. The drilling fluid of claim 14, wherein: the content of the composite plugging material is 2-10wt% based on the total weight of the drilling fluid.
16. The drilling fluid of claim 14, wherein: the content of the composite plugging material is 3-7wt% based on the total weight of the drilling fluid.
17. Use of a composite lost circulation material according to any of claims 1-12 in a drilling process, said composite lost circulation material being added in an amount of 0.1-5 wt% when used in a drilling process.
18. The use according to claim 17, characterized in that: when the composite plugging material is used in the drilling process, the addition amount is 0.5-5 wt%.
19. The use according to claim 17, characterized in that: when the composite plugging material is used in the drilling process, the addition amount is 1-5 wt%.
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