CN116478669A - Plugging material and preparation method and application thereof - Google Patents

Plugging material and preparation method and application thereof Download PDF

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Publication number
CN116478669A
CN116478669A CN202310428184.0A CN202310428184A CN116478669A CN 116478669 A CN116478669 A CN 116478669A CN 202310428184 A CN202310428184 A CN 202310428184A CN 116478669 A CN116478669 A CN 116478669A
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plugging material
water
preparation
plugging
mxene
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CN116478669B (en
Inventor
李瑞刚
孙方龙
宋元成
焦延安
叶荆
何英君
杨勇
史东军
何德波
李金锁
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Sinopec Oilfield Service Corp
Sinopec North China Petroleum Engineering Corp
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Sinopec Oilfield Service Corp
Sinopec North China Petroleum Engineering Corp
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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
    • C09K8/032—Inorganic 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
    • C09K8/02—Well-drilling compositions
    • C09K8/04—Aqueous well-drilling compositions
    • C09K8/14—Clay-containing compositions
    • C09K8/16—Clay-containing compositions characterised by the inorganic compounds other than clay
    • 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
    • C09K8/04—Aqueous well-drilling compositions
    • C09K8/14—Clay-containing compositions
    • C09K8/18—Clay-containing compositions characterised by the organic compounds
    • C09K8/22—Synthetic organic compounds
    • C09K8/24—Polymers
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
    • C09K8/42—Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells
    • C09K8/426—Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells for plugging
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
    • C09K8/42—Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells
    • C09K8/46—Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells containing inorganic binders, e.g. Portland cement
    • 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

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Dispersion Chemistry (AREA)
  • Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)

Abstract

The invention relates to a plugging material, a preparation method and application thereof, and belongs to the technical field of petrochemicals. The preparation method of the plugging material comprises the following steps: and (3) in-situ growing calcium carbonate on the MXene material to obtain a composite material, and then in-situ growing molybdenum disulfide on the composite material to obtain the plugging material. The plugging material prepared by the invention is a heterojunction self-lubricating plugging material, has lower friction coefficient, excellent self-lubricating performance, good compatibility with water-based drilling fluid, excellent high temperature resistance and stronger stability, can effectively solve the technical problems of lubrication, torque reduction and friction resistance reduction in the horizontal well drilling process, can improve the rock carrying capacity and reduce the plastic viscosity in the water-based drilling fluid, and can realize the well wall stabilization, well cleaning, friction reduction, drag reduction and leakage prevention in the well drilling process.

Description

Plugging material and preparation method and application thereof
Technical Field
The invention relates to a plugging material, a preparation method and application thereof, and belongs to the technical field of petrochemicals.
Background
Lost circulation refers to a complex downhole situation in which working fluids such as drilling fluid, cement slurry, completion fluid, etc., are lost into the formation under the action of pressure differential, and is one of the most difficult problems to deal with during drilling. Since China is at the later stage of oilfield development at present, industrial oil flow cannot be obtained by adopting a conventional development technology, and most of the wells to be drilled are complex wells, such as ultra-deep wells, horizontal wells and the like. Better development effect can be obtained by adopting an ultra-long horizontal section horizontal well. Because the length of the horizontal section is large, the contact surface of the drilling tool and the well wall is large, and the long horizontal section is difficult to carry rock, is easy to form a rock debris bed, causes the increase of friction resistance, is difficult to reduce friction and drag, and has high requirement on the lubricating property of drilling fluid. Meanwhile, the problems of serious sliding drilling underpressure, easy occurrence of borehole instability, serious formation slurry production, high plugging difficulty, large friction torque in the later construction period, difficult drilling pressurization and the like are solved in the horizontal well drilling process, and the problems of high plastic viscosity and equivalent circulating density, low cutting force, poor carrying capacity, large drilling cuttings and drilling fluid later treatment difficulty, high cost and the like of the water-based drilling fluid are considered, so that the drilling fluid is required to have stronger lubricity, better carrying capacity and lower plastic viscosity in order to reduce friction torque and ensure borehole stability when the horizontal well with the horizontal section length of more than 3000m is drilled in China, so that the requirements of guaranteeing borehole stability, cleaning the borehole, reducing friction drag and preventing leakage are met.
Lubricants commonly used in drilling processes are generally classified into liquid lubricants and solid lubricants. The liquid lubricant has limited reduction of lubrication coefficient, is easy to foam a drilling fluid system, affects normal drilling, has insufficient temperature resistance, generally fails at 120 ℃, and affects large-scale popularization and application. The solid lubricant can form an isolation lubricating film on the friction surface, so that the purposes of reducing friction and preventing abrasion are achieved. In addition, solid lubricants are particularly effective in reducing wear of tool joints with hardbanding, and also in reducing wear of tailpipe, casing and rotating casing. The solid lubricant has good thermal stability, chemical stability, corrosion resistance and the like, and is suitable for high-temperature, high-inclination well sections and long horizontal sections. The common solid lubricant has complex composition and high cost.
Molybdenum disulfide (MoS) having a layered structure 2 ) Typically formed by S-Mo-S bond bonding, similar in structure to graphene. The layers are connected by weak Van der Waals force, so that slippage is easy to occur, and MoS is caused 2 Has a low friction coefficient. Furthermore, moS 2 Has the advantages of good heat stability, low shearing strength, strong surface adhesion, and the like, so that MoS 2 Is suitable for being used as a solid lubricant. However, moS 2 When being independently used as a friction lubricating material, the friction lubricating material is easy to absorb moisture and oxidize in the atmospheric environment to lose efficacy, thereby reducing the use value. Due to MoS 2 Is less dense and has poor dispersibility in water-based drilling fluids. In addition, during drilling, moS 2 Is not easy to adhere to the well wall, so that the drag reduction performance is inhibited.
Disclosure of Invention
The invention aims to provide a preparation method of a plugging material, which can solve the problem of MoS at present 2 The anti-drag performance is poor when the anti-drag agent is used for drilling fluid.
The second object of the invention is to provide a plugging material.
The third object of the invention is to provide an application of the plugging material in oil-based drilling fluid.
In order to achieve the above purpose, the preparation method of the plugging material of the invention adopts the following technical scheme:
a preparation method of a plugging material comprises the following steps: and (3) in-situ growing calcium carbonate on the MXene material to obtain a composite material, and then in-situ growing molybdenum disulfide on the composite material to obtain the plugging material.
According to the preparation method of the plugging material, the advantages of excellent lubricating performance of the molybdenum disulfide nanosheets, good shape controllability, high temperature resistance and good dispersibility of the calcium carbonate nanoparticles in base slurry, rich surface functional groups of the MXene material and the like are utilized, and the plugging material with different shapes, sizes and contents of the calcium carbonate particles is constructed by regulating and controlling the thickness and the size of the molybdenum disulfide nanosheets. The plugging material prepared by the invention is a heterojunction self-lubricating plugging material, has lower friction coefficient, excellent self-lubricating performance, good compatibility with water-based drilling fluid, excellent high temperature resistance and stronger stability, can effectively solve the technical problems of lubrication, torque reduction and friction resistance reduction in the horizontal well drilling process, can improve the rock carrying capacity and reduce the plastic viscosity in the water-based drilling fluid, and can realize the well wall stabilization, well cleaning, friction reduction, drag reduction and leakage prevention in the well drilling process.
In the plugging material prepared by the invention, calcium carbonate particles with rigid and hard properties and MoS 2 Rigid-flexible combination can improve MoS 2 Is used for the lubricating performance of the steel sheet; the density of the calcium carbonate is high and is equal to MoS 2 The combination can increase the density of the composite lubricant and enable the composite lubricant to be better dispersed in the water-based drilling fluid. In addition, the abundant functional groups on the surface of the MXene material are beneficial to improving the adhesion capability of the plugging material on the well wall.
Preferably, the MXene material is Ti 2 C 3 MXene micron sheet, ti 2 C 3 Mxene nanoplatelets, tiCN nanoplatelets.
Preferably, the size of the MXene material is not more than 50 μm.
Preferably, the surface of the MXene material contains hydroxyl groups. The calcium ions can coordinate with hydroxyl groups through hydroxyl oxygen, which is beneficial to the in-situ synthesis of calcium carbonate.
Preferably, the MXene material is etched from MAX material.
Preferably, the MXene material is made by a method comprising the steps of: and mixing the MAX material with hydrofluoric acid, carrying out solid-liquid separation, drying, and carrying out ultrasonic treatment on the dried solid to obtain the MXene material.
Preferably, the MAX material is Ti 2 AlC 3 MAX、TiAlCNMAX。
Preferably, the concentration of the hydrofluoric acid is 0.1-0.15 mol/L. Preferably, the volume of hydrofluoric acid for each 2g of MAX material is 15-25 mL. Preferably, the mixing time is not less than 24 hours. Preferably, the power of the ultrasonic treatment is 500-1200W, and the time is not less than 30min. Preferably, the ultrasonic treatment is performed at not higher than 0 ℃.
Preferably, the method of in situ growth of calcium carbonate on an MXene material comprises the steps of: and uniformly mixing the MXene material and the solution containing calcium ions, then adding the solution containing carbonate ions, mixing, aging, carrying out solid-liquid separation, and drying to obtain the composite material.
Preferably, the solution containing calcium ions is mainly made of water-soluble calcium salt and water.
Preferably, when preparing the solution containing calcium ions, the mass ratio of the water-soluble calcium salt to water used is (1-15): 100. It is further preferable that the mass ratio of the water-soluble calcium salt to water used in the preparation of the solution containing calcium ions is (1 to 1.25): 100.
Preferably, the water-soluble calcium salt is calcium chloride.
Preferably, the solution containing calcium ions is mainly prepared from water-soluble calcium salt, morphology regulator, surfactant and water.
Preferably, the mass ratio of the MXene material to the water-soluble calcium salt is (1-10): 100. Further preferably, the mass ratio of the MXene material to the water-soluble calcium salt is (1-5): 100.
Preferably, the morphology modifier is sulfuric acid, polyacrylic acid, ethanol, trisodium citrate, glycine, sucrose, dextran. The morphology modifier is used to control the crystal form and morphology of in-situ grown calcium carbonate products to obtain calcium carbonate with larger specific surface area, and can obtain calcium carbonate with different morphologies, such as spinodal, rod-shaped, amorphous, rod-shaped, spherical, cubic, spherical. The hydroxyl groups of the alcohols and the glucan can have strong electrostatic matching effect with calcium ions to form local supersaturation degree, thereby reducing nucleation activation energy of calcium carbonate crystallization.
Preferably, the weight average molecular weight of the polyacrylic acid is 4000 to 10000.
Preferably, the mass ratio of the morphology modifier to the water-soluble calcium salt is (5-20): 100.
Preferably, the surfactant is Span-80. The surfactant can be adsorbed on the surface of the calcium carbonate crystal, so that a protective layer is formed on the surface of the calcium carbonate, and the agglomeration of the calcium carbonate is effectively prevented.
Preferably, the mass of surfactant employed is no greater than 30g per 100g of water-soluble calcium salt. It is further preferable that the mass of the surfactant used is 20 to 30g per 100g of the water-soluble calcium salt.
Preferably, the carbonate ion-containing solution is made mainly of water-soluble carbonate and water.
Preferably, the water-soluble carbonate is an alkali metal carbonate. For example, the water-soluble carbonate is sodium carbonate.
Preferably, when the water-soluble carbonate is an alkali metal carbonate, the carbonate ion-containing solution is an alkali metal carbonate solution having a concentration of 0.024 to 0.05 g/mL.
Preferably, the ratio of the amount of carbonate ion in the water-soluble carbonate salt to the amount of calcium ion in the water-soluble calcium salt is (1 to 1.5): 1.
Preferably, the temperature of mixing performed in the method of in situ growth of calcium carbonate on MXene material is not lower than 70 ℃ for not less than 1h.
Preferably, the aging time is 0.5 to 2 hours. Further preferably, the aging time is 1 to 2 hours. The carbonization degree can be controlled by different ageing times, so that the grain diameter of the obtained calcium carbonate is controlled; the longer the aging time, the finer the particle size, and the less likely the reverse reaction occurs.
Preferably, the method of growing molybdenum disulfide in situ on a composite material comprises the steps of: uniformly mixing the composite material and the water-soluble tetrathiomolybdate in an organic solvent, standing for at least 12 hours at the temperature of not lower than 200 ℃, carrying out solid-liquid separation, and drying to obtain the plugging material.
Preferably, the organic solvent is a water-soluble organic solvent.
Preferably, the organic solvent is N, N-dimethylformamide.
Preferably, the water-soluble tetrathiomolybdate is ammonium tetrathiomolybdate.
Preferably, the mass ratio of the composite material to the organic solvent is (10-30): 100. It is further preferable that the mass ratio of the composite material to the organic solvent is (20 to 30): 100.
Preferably, the mass ratio of the water-soluble tetrathiomolybdate to the organic solvent is (2-10): 100. Further preferably, the mass ratio of the water-soluble tetrathiomolybdate to the organic solvent is (5 to 10): 100.
The plugging material adopts the following technical scheme:
the plugging material prepared by the preparation method of the plugging material.
The plugging material has the functions of plugging a lost stratum and preventing drill sticking, and has good application prospect in oilfield development.
The technical scheme adopted by the application of the plugging material in drilling fluid is as follows:
the plugging material prepared by the preparation method of the plugging material is applied to drilling fluid.
When the plugging material is used for drilling fluid, the plugging material has good compatibility, excellent high temperature resistance and strong stability, can effectively solve the technical problems of lubrication, torque reduction and friction resistance reduction in the horizontal well drilling process, can improve the rock carrying capacity and reduce the plastic viscosity in the drilling fluid, and can realize stable well wall, well cleaning, friction reduction, drag reduction and leakage prevention in the drilling process.
Preferably, the drilling fluid is a water-based drilling fluid.
Drawings
FIG. 1 is a scanning electron microscope image of in-situ grown calcium carbonate on a composite material prepared in an embodiment of the present invention;
fig. 2 is a scanning electron microscope image of a plugging material prepared according to an embodiment of the present invention.
Detailed Description
The technical scheme of the invention is further described below with reference to specific embodiments.
1. The specific examples of the preparation method of the plugging material of the invention are as follows:
example 1
The preparation method of the plugging material of the embodiment specifically comprises the following steps:
(1) The mass of Ti is 2g 2 AlC 3 MAX is added into 20mL hydrofluoric acid (the concentration is 0.1 mol/L), after stirring for 24 hours, the obtained suspension is centrifuged, solids obtained by the centrifugation are respectively washed by water and alcohol in turn, then the dried solids are dried for 12 hours under the vacuum condition of 60 ℃, and then the dried solids are treated by ultrasonic treatment (the power is 1200W) in ice bath for 30 minutes, thus obtaining layered Ti in the shape of flakes 2 C 3 MXene, 50 μm in size;
(2) Dissolving 1.25g of calcium chloride in 100g of deionized water, ultrasonically stirring to obtain a calcium chloride solution, and adding 0.16g of sucrose and the Ti prepared in the step (1) 2 C 3 Mxene(Ti 2 C 3 The mass ratio of Mxene to calcium chloride is 5:100) and surfactant (Span-80, 20:100) are added into the calcium chloride solution, and mixedSlowly dripping sodium carbonate solution with the concentration of 0.024g/mL (the ratio of the amount of sodium carbonate in the sodium carbonate solution to the amount of calcium chloride in the sodium carbonate solution is 1:1) into the uniformly mixed liquid, then reacting for 1h at 70 ℃ under stirring, aging the reacted system for 1h at room temperature, filtering, and drying a filter cake to obtain a composite material, wherein the particle size of calcium carbonate growing in situ on the composite material is 40nm;
(3) 20mg of the composite material obtained in step (2) was added to 100mL of N, N-Dimethylformamide (DMF), followed by addition of 5mg of (NH) 4 ) 2 MoS 4 Ultrasonic processing for 8h, transferring the mixture after ultrasonic processing into an autoclave, preserving heat and standing for 12h at 200 ℃, filtering the system after heat preservation, washing the solid obtained by filtering by ethanol and water respectively in sequence, and drying the washed solid for 10h at 70 ℃ in a vacuum environment to obtain the plugging material.
Example 2
The preparation method of the plugging material of the present embodiment differs from the preparation method of the plugging material of embodiment 1 only in that the mass of calcium chloride is adjusted in step (2) of the preparation method of the plugging material of the present embodiment so that the mass ratio of calcium chloride to water is 10:100; the particle size of calcium carbonate grown in situ on the composite material prepared by the preparation method of the plugging material of the embodiment is 60nm.
Example 3
The preparation method of the plugging material of the embodiment differs from the preparation method of the plugging material of embodiment 1 only in that the mass of calcium chloride is adjusted in the step (2) of the preparation method of the plugging material of the embodiment so that the mass ratio of calcium chloride to water is 13:100; the particle size of calcium carbonate grown in situ on the composite material prepared by the preparation method of the plugging material of the embodiment is 55nm.
Example 4
The preparation method of the plugging material of the present embodiment differs from the preparation method of the plugging material of embodiment 1 only in that the mass of calcium chloride is adjusted in step (2) of the preparation method of the plugging material of the present embodiment so that the mass ratio of calcium chloride to water is 15:100; the particle size of calcium carbonate grown in situ on the composite material prepared by the preparation method of the plugging material of the embodiment is 36nm.
Example 5
The preparation method of the plugging material of this embodiment differs from the preparation method of the plugging material of embodiment 1 only in that the ratio of the amount of sodium carbonate substance to the amount of calcium chloride substance in the sodium carbonate solution added dropwise in step (2) of the preparation method of the plugging material of this embodiment is 1.25:1.
Example 6
The preparation method of the plugging material of this embodiment differs from the preparation method of the plugging material of embodiment 1 only in that the ratio of the amount of sodium carbonate substance to the amount of calcium chloride substance in the sodium carbonate solution added dropwise in step (2) of the preparation method of the plugging material of this embodiment is 1.5:1.
Example 7
The preparation method of the plugging material of this embodiment differs from the preparation method of the plugging material of embodiment 1 only in that in step (2) of the preparation method of the plugging material of this embodiment, sucrose is replaced with a sulfuric acid solution with a mass fraction of 20%; the calcium carbonate grown in situ on the composite material prepared by the preparation method of the plugging material of the embodiment is in a spinning cone shape.
Example 8
The preparation method of the plugging material of this embodiment differs from the preparation method of the plugging material of embodiment 1 only in that in step (2) of the preparation method of the plugging material of this embodiment, sucrose is replaced with PAA (polyacrylic acid, weight average molecular weight is 4000 to 10000); the calcium carbonate grown in situ on the composite material prepared by the preparation method of the plugging material of the embodiment is in a rod shape.
Example 9
The preparation method of the plugging material of this embodiment differs from the preparation method of the plugging material of embodiment 1 only in that in step (2) of the preparation method of the plugging material of this embodiment, sucrose is replaced with ethanol; the calcium carbonate grown in situ on the composite material prepared by the preparation method of the plugging material of the embodiment is amorphous.
Example 10
The preparation method of the plugging material of this embodiment differs from the preparation method of the plugging material of embodiment 1 only in that in step (2) of the preparation method of the plugging material of this embodiment, sucrose is replaced with trisodium citrate; the calcium carbonate grown in situ on the composite material prepared by the preparation method of the plugging material of the embodiment is cubic.
Example 11
The preparation method of the plugging material of this embodiment differs from the preparation method of the plugging material of embodiment 1 only in that in step (2) of the preparation method of the plugging material of this embodiment, sucrose is replaced with glycine; the calcium carbonate grown in situ on the composite material prepared by the preparation method of the plugging material of the embodiment is spherical.
Example 12
The preparation method of the plugging material of this embodiment differs from the preparation method of the plugging material of embodiment 1 only in that in step (2) of the preparation method of the plugging material of this embodiment, sucrose is replaced with dextran; the calcium carbonate grown in situ on the composite material prepared by the preparation method of the plugging material of the embodiment is spherical.
Example 13
The preparation method of the plugging material of the embodiment is different from the preparation method of the plugging material of the embodiment 1 only in that the sucrose usage amount is adjusted in the step (2) of the preparation method of the plugging material of the embodiment, and the mass ratio of the sucrose to the calcium chloride is 5:100; the particle size of calcium carbonate grown in situ on the composite material prepared by the preparation method of the plugging material of the embodiment is 55nm.
Example 14
The preparation method of the plugging material of the embodiment is different from the preparation method of the plugging material of the embodiment 1 only in that the sucrose usage amount is adjusted in the step (2) of the preparation method of the plugging material of the embodiment, and the mass ratio of the sucrose to the calcium chloride is 10:100; the particle size of calcium carbonate grown in situ on the composite material prepared by the preparation method of the plugging material of the embodiment is 38nm.
Example 15
The preparation method of the plugging material of the embodiment is different from the preparation method of the plugging material of the embodiment 1 only in that the sucrose usage amount is adjusted in the step (2) of the preparation method of the plugging material of the embodiment, and the mass ratio of the sucrose to the calcium chloride is 15:100; the particle size of calcium carbonate grown in situ on the composite material prepared by the preparation method of the plugging material of the embodiment is 27nm.
Example 16
The preparation method of the plugging material of the embodiment is different from the preparation method of the plugging material of the embodiment 1 only in that the sucrose usage amount is adjusted in the step (2) of the preparation method of the plugging material of the embodiment, and the mass ratio of the sucrose to the calcium chloride is 20:100; the particle size of calcium carbonate grown in situ on the composite material prepared by the preparation method of the plugging material of the embodiment is 15nm.
Example 17
The preparation method of the plugging material of this embodiment differs from the preparation method of the plugging material of embodiment 1 only in that the mass of the surfactant used in step (2) of the preparation method of the plugging material of this embodiment is 0; the particle size of calcium carbonate grown in situ on the composite material prepared by the preparation method of the plugging material of the embodiment is 8 mu m.
Example 18
The preparation method of the plugging material of the embodiment is different from the preparation method of the plugging material of embodiment 1 only in that the amount of the surfactant is adjusted in the step (2) of the preparation method of the plugging material of the embodiment, and the mass ratio of the surfactant to the calcium chloride is 5:100; the particle size of calcium carbonate grown in situ on the composite material prepared by the preparation method of the plugging material of the embodiment is 200nm.
Example 19
The preparation method of the plugging material of the embodiment is different from the preparation method of the plugging material of embodiment 1 only in that the amount of the surfactant is adjusted in the step (2) of the preparation method of the plugging material of the embodiment, and the mass ratio of the surfactant to the calcium chloride is 10:100; the particle size of calcium carbonate grown in situ on the composite material prepared by the preparation method of the plugging material of the embodiment is 78nm.
Example 20
The preparation method of the plugging material of the embodiment is different from the preparation method of the plugging material of embodiment 1 only in that the amount of the surfactant is adjusted in the step (2) of the preparation method of the plugging material of the embodiment, and the mass ratio of the surfactant to the calcium chloride is 15:100; the particle size of calcium carbonate grown in situ on the composite material prepared by the preparation method of the plugging material of the embodiment is 60nm.
Example 21
The preparation method of the plugging material of the embodiment differs from the preparation method of the plugging material of embodiment 1 only in that the amount of the surfactant is adjusted in step (2) of the preparation method of the plugging material of the embodiment, and the mass ratio of the surfactant to the calcium chloride is 23:100; the particle size of calcium carbonate grown in situ on the composite material prepared by the preparation method of the plugging material of the embodiment is 36nm.
Example 22
The preparation method of the plugging material of the embodiment is different from the preparation method of the plugging material of embodiment 1 only in that the amount of the surfactant is adjusted in the step (2) of the preparation method of the plugging material of the embodiment, and the mass ratio of the surfactant to the calcium chloride is 25:100; the particle size of calcium carbonate grown in situ on the composite material prepared by the preparation method of the plugging material in the embodiment is 20nm.
Example 23
The preparation method of the plugging material of the embodiment is different from the preparation method of the plugging material of embodiment 1 only in that the amount of the surfactant is adjusted in the step (2) of the preparation method of the plugging material of the embodiment, and the mass ratio of the surfactant to the calcium chloride is 30:100; the particle size of calcium carbonate grown in situ on the composite material prepared by the preparation method of the plugging material of the embodiment is 15nm.
Example 24
The preparation method of the plugging material of this embodiment differs from the preparation method of the plugging material of embodiment 1 only in that the aging time in step (2) of the preparation method of the plugging material of this embodiment is 0.5h; the particle size of calcium carbonate grown in situ on the composite material prepared by the preparation method of the plugging material of the embodiment is 52nm.
Example 25
The preparation method of the plugging material of this embodiment differs from the preparation method of the plugging material of embodiment 1 only in that the aging time in step (2) of the preparation method of the plugging material of this embodiment is 1.5 hours; the particle size of calcium carbonate grown in situ on the composite material prepared by the preparation method of the plugging material of the embodiment is 38nm.
Example 26
The preparation method of the plugging material of this embodiment differs from the preparation method of the plugging material of embodiment 1 only in that the aging time in step (2) of the preparation method of the plugging material of this embodiment is 2 hours; the particle size of calcium carbonate grown in situ on the composite material prepared by the preparation method of the plugging material of the embodiment is 30nm.
Example 27
The preparation method of the plugging material of the present embodiment differs from the preparation method of the plugging material of embodiment 1 only in that Ti is adjusted in step (2) of the preparation method of the plugging material of the present embodiment 2 C 3 The amount of Mxene, ti 2 C 3 The mass ratio of the Mxene to the calcium chloride is 1:100; the quality of in-situ grown calcium carbonate and Ti on the composite material prepared by the preparation method of the plugging material of the embodiment 2 C 3 The mass ratio of Mxene is 1:100.
Example 28
The preparation method of the plugging material of the present embodiment differs from the preparation method of the plugging material of embodiment 1 only in that Ti is adjusted in step (2) of the preparation method of the plugging material of the present embodiment 2 C 3 The amount of Mxene, ti 2 C 3 The mass ratio of the Mxene to the calcium chloride is 3:100; the quality of in-situ grown calcium carbonate and Ti on the composite material prepared by the preparation method of the plugging material of the embodiment 2 C 3 The mass ratio of Mxene is 3:100.
Example 29
The preparation method of the plugging material of the present embodiment differs from the preparation method of the plugging material of embodiment 1 only in that Ti is adjusted in step (2) of the preparation method of the plugging material of the present embodiment 2 C 3 The amount of Mxene, ti 2 C 3 The mass ratio of the Mxene to the calcium chloride is 7:100; the quality of in-situ grown calcium carbonate and Ti on the composite material prepared by the preparation method of the plugging material of the embodiment 2 C 3 The mass ratio of Mxene is 7:100.
Example 30
The preparation method of the plugging material of the present embodiment differs from the preparation method of the plugging material of embodiment 1 only in that Ti is adjusted in step (2) of the preparation method of the plugging material of the present embodiment 2 C 3 The amount of Mxene, ti 2 C 3 The mass ratio of the Mxene to the calcium chloride is 10:100; the quality of in-situ grown calcium carbonate and Ti on the composite material prepared by the preparation method of the plugging material of the embodiment 2 C 3 The mass ratio of Mxene is 10:100.
Example 31
The preparation method of the plugging material of this embodiment differs from the preparation method of the plugging material of embodiment 1 only in that the hydrofluoric acid used in step (1) of the preparation method of the plugging material of this embodiment is 15mL.
Example 32
The preparation method of the plugging material of this embodiment differs from the preparation method of the plugging material of embodiment 1 only in that the hydrofluoric acid used in step (1) of the preparation method of the plugging material of this embodiment is 22mL.
Example 33
The preparation method of the plugging material of this embodiment differs from the preparation method of the plugging material of embodiment 1 only in that the hydrofluoric acid used in step (1) of the preparation method of the plugging material of this embodiment is 25mL.
Example 34
The preparation method of the plugging material of this embodiment differs from the preparation method of the plugging material of embodiment 1 only in that the amount of the composite material is adjusted in step (3) of the preparation method of the plugging material of this embodiment, and the mass ratio of the composite material to N, N-dimethylformamide is 10:100.
Example 35
The preparation method of the plugging material of this embodiment differs from the preparation method of the plugging material of embodiment 1 only in that the amount of the composite material is adjusted in step (3) of the preparation method of the plugging material of this embodiment, and the mass ratio of the composite material to N, N-dimethylformamide is 20:100.
Example 36
The preparation method of the plugging material of this embodiment differs from the preparation method of the plugging material of embodiment 1 only in that the amount of the composite material is adjusted in step (3) of the preparation method of the plugging material of this embodiment, and the mass ratio of the composite material to N, N-dimethylformamide is 30:100.
Example 37
The preparation method of the plugging material of this embodiment differs from the preparation method of the plugging material of embodiment 1 only in that (NH 4 ) 2 MoS 4 The amount of (NH) 4 ) 2 MoS 4 And N, N-dimethylformamide in a mass ratio of 2:100.
Example 38
The preparation method of the plugging material of this embodiment differs from the preparation method of the plugging material of embodiment 1 only in that (NH 4 ) 2 MoS 4 The amount of (NH) 4 ) 2 MoS 4 And N, N-dimethylformamide in a mass ratio of 4:100.
Example 39
The preparation method of the plugging material of this embodiment differs from the preparation method of the plugging material of embodiment 1 only in that (NH 4 ) 2 MoS 4 The amount of (NH) 4 ) 2 MoS 4 And N, N-dimethylformamide in a mass ratio of 6:100.
Example 40
The preparation method of the plugging material of this embodiment differs from the preparation method of the plugging material of embodiment 1 only in that (NH 4 ) 2 MoS 4 The amount of (NH) 4 ) 2 MoS 4 And N, N-dimethylformamide in a mass ratio of 8:100.
Example 41
The preparation method of the plugging material of this embodiment differs from the preparation method of the plugging material of embodiment 1 only in that (NH 4 ) 2 MoS 4 The amount of (NH) 4 ) 2 MoS 4 And the mass ratio of the N, N-dimethylformamide is 10:100.
In fig. 1, fig. 1a is a scanning electron microscope image of calcium carbonate grown in situ on the composite material prepared in example 23, fig. 1b is a scanning electron microscope image of calcium carbonate grown in situ on the composite material prepared in example 18, fig. 1c is a scanning electron microscope image of calcium carbonate grown in situ on the composite material prepared in example 1, and fig. 1d is a scanning electron microscope image of calcium carbonate grown in situ on the composite material prepared in example 22.
FIG. 2A is a Scanning Electron Microscope (SEM) image of the plugging material prepared in example 15, FIG. 2b is a Ti image prepared in example 1 2 C 3 FIG. 2c is a scanning electron microscope image of the plugging material prepared in example 2, and FIG. 2d is a scanning electron microscope image of the plugging material prepared in example 13.
Comparative example 1
The preparation method of the plugging material of the comparative example specifically comprises the following steps:
(1) The mass of Ti is 2g 2 AlC 3 MAX is added into 20mL hydrofluoric acid (the concentration is 0.1 mol/L), after stirring for 24 hours, the obtained suspension is centrifuged, solids obtained by the centrifugation are respectively washed by water and alcohol in turn, then the dried solids are dried for 12 hours under the vacuum condition of 60 ℃, and then the dried solids are treated by ultrasonic treatment (the power is 1200W) in ice bath for 30 minutes, thus obtaining layered Ti in the shape of flakes 2 C 3 MXene, 50 μm in size;
(2) 20mg of Ti prepared in step (1) 2 C 3 MXene was added to 100mL of N, N-Dimethylformamide (DMF), followed by addition of 5mg of (NH) 4 ) 2 MoS 4 Ultrasonic processing for 8h, transferring the mixture after ultrasonic processing into an autoclave, preserving heat and standing for 12h at 200 ℃, filtering the system after heat preservation, washing the solid obtained by filtering by ethanol and water respectively in sequence, and drying the washed solid for 10h at 70 ℃ in a vacuum environment to obtain the plugging material.
Comparative example 2
The preparation method of the plugging material of the comparative example specifically comprises the following steps:
(1) The mass of Ti is 2g 2 AlC 3 MAX is added into 20mL hydrofluoric acid (the concentration is 0.1 mol/L), after stirring for 24 hours, the obtained suspension is centrifuged, solids obtained by the centrifugation are respectively washed by water and alcohol in turn, then the dried solids are dried for 12 hours under the vacuum condition of 60 ℃, and then the dried solids are treated by ultrasonic treatment (the power is 1200W) in ice bath for 30 minutes, thus obtaining layered Ti in the shape of flakes 2 C 3 MXene, 50 μm in size;
(2) Dissolving 1.25g of calcium chloride in 100g of deionized water, ultrasonically stirring to obtain a calcium chloride solution, and adding 0.16g of sucrose and the Ti prepared in the step (1) 2 C 3 Mxene(Ti 2 C 3 Adding a surfactant (the surfactant is Span-80, the mass ratio of the surfactant to the calcium chloride is 20:100) and a surfactant (the mass ratio of the Mxene to the calcium chloride is 5:100) into a calcium chloride solution, uniformly mixing, slowly dropwise adding a sodium carbonate solution with the concentration of 0.024g/mL into the uniformly mixed solution (the ratio of the amount of sodium carbonate in the dropwise added sodium carbonate solution to the amount of the calcium chloride is 1:1), then reacting for 1h at 70 ℃ under stirring, aging the reacted system for 1h at room temperature, filtering, and drying a filter cake to obtain the plugging material.
Comparative example 3
The preparation method of the plugging material of the comparative example specifically comprises the following steps:
(1) The mass of Ti is 2g 2 AlC 3 MAX addingAdding into 20mL hydrofluoric acid (concentration of 0.1 mol/L), stirring for 24 hr, centrifuging the obtained suspension, washing the centrifuged solid with water and ethanol respectively, drying at 60deg.C under vacuum for 12 hr, and subjecting the dried solid to ultrasonic treatment (power of 1200W) in ice bath for 30min to obtain layered Ti in sheet form 2 C 3 MXene, 50 μm in size;
(2) 20mg of Ti prepared in step (1) 2 C 3 MXene was added to 100mL of N, N-Dimethylformamide (DMF), followed by addition of 5mg of (NH) 4 ) 2 MoS 4 Ultrasonic processing for 8h, transferring the mixture after ultrasonic processing into an autoclave, preserving heat and standing for 12h at 200 ℃, filtering the system after heat preservation, washing the solid obtained by filtering by ethanol and water respectively in sequence, and drying the washed solid for 10h at 70 ℃ in a vacuum environment to obtain a composite material;
(3) Dissolving 1.25g of calcium chloride in 100g of deionized water, stirring by ultrasonic to obtain a calcium chloride solution, adding 0.16g of sucrose, the composite material (the mass ratio of the composite material to the calcium chloride is 5:100) and a surfactant (the mass ratio of the surfactant to the calcium chloride is 20:100) which are prepared in the step (2) into the calcium chloride solution, uniformly mixing, slowly dropwise adding a sodium carbonate solution with the concentration of 0.024g/mL into the uniformly mixed solution (the ratio of the amount of sodium carbonate in the dropwise added sodium carbonate solution to the amount of the calcium chloride is 1:1), reacting for 1h at 70 ℃ under the stirring condition, aging the reacted system for 1h at room temperature, filtering, and drying the filter cake to obtain the plugging material.
2. Specific examples of the plugging material of the invention are as follows:
the plugging material of this embodiment is prepared by the method of any one of embodiments 1-41.
3. Specific examples of applications of the plugging material of the present invention in drilling fluids are as follows:
the plugging material prepared by the preparation method of any one of the plugging materials in the embodiments 1 to 41 is used in drilling fluid.
Experimental example 1
To evaluate the applicability of the plugging materials prepared in examples 1 to 41 and comparative examples 1 to 3 in drilling fluids, the plugging materials were added to a water-based slurry (the mass of the plugging materials is 1% of the mass of the water-based slurry), and a drilling fluid system was obtained after mixing, and then the drilling fluid system was tested according to the standard GB/T16783.1-2006 part 1 of the field test of drilling fluids for oil and gas industry: the viscosity of the water-based slurry and the drilling fluid system is tested by a six-speed rotary viscometer in the water-based drilling fluid, and the readings of the dial stability at 600r/min, 300r/min and 100r/min are recorded, and the test results are shown in table 1.
The water-based slurry used in the experimental example consists of the following components in percentage by mass: 70.7% of water, 0.3% of multifunctional high molecular weight composite ionic polymer, 20.0% of shale inhibitor CQFY-3, 2.0% of low-viscosity polyanion cellulose, 1.0% of high-viscosity vinyl monomer multipolymer anti-collapse fluid loss agent, 4.0% of LG vegetable gum and 2.0% of bentonite; wherein the multifunctional high molecular weight composite ionic polymer consists of polydiallyl dimethyl ammonium chloride and cationic polyacrylamide in a mass ratio of 1:1.
Table 1 viscosity of drilling fluid system
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As can be seen from Table 1, the plugging materials prepared in examples 1-41 have a smaller influence on the viscosity of the water-based base slurry, and the rheological property change range basically meets the field construction requirements. Among them, the plugging materials prepared in example 1, example 12 and example 20 had minimal effect on the viscosity of the water-based slurry.
Experimental example 2
To further investigate the effect of the plugging materials prepared in examples 1-41 and comparative examples 1-3 in drilling fluids, the water-based base slurry of experimental example 1 and the drilling fluid systems prepared from the different plugging materials were subjected to rheological property tests, including plastic viscosity, dynamic shear force, dynamic plastic ratio, Φ6, Φ3, and low shear rate shear force (LSYP). Wherein, phi 6 and phi 3 represent the readings of the six-speed rotary viscometer when the dial is stable at the rotating speeds of 6r/min and 3r/min, and the testing methods of plastic viscosity, dynamic shear force, dynamic plastic ratio, phi 6, phi 3 and low shear rate shear force (LSYP) are carried out according to the specifications in the standard DB 61/T574-2013 oil-based drilling fluid performance requirement and use technical specification test. The test results are shown in Table 2.
TABLE 2 rheological Properties of drilling fluid systems prepared with Water-based slurries and different plugging materials
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As can be seen from Table 2, after the plugging materials prepared in examples 1 to 41 were added to the water-based slurry, the plastic viscosity was increased, and the dynamic shear force, dynamic-plastic ratio and low shear rate shear force (LSYP) were increased, but all of them meet the practical requirements, and from the performance point of view, the plugging material prepared in example 1 was most remarkable in terms of the performance of the slurry.
Experimental example 3
On the basis of experimental example 2, the fluid loss performance of a drilling fluid system prepared from the plugging material prepared in example 1 was tested, the plugging material prepared in example 1 was added to a water-based slurry (same as the water-based slurry used in experimental example 1) in amounts of 1%, 2% and 3% of the mass of the water-based slurry, respectively, to obtain a drilling fluid system, and then the apparent viscosity, plastic viscosity, dynamic shear force and API fluid loss of the drilling fluid system before and after aging were tested, the aging temperature was 120 ℃, 150 ℃, 180 ℃, and the aging time was 4 hours. The testing method of apparent viscosity, plastic viscosity, dynamic shear force and API fluid loss is carried out according to the specification in the standard DB 61/T574-2013 oil-based drilling fluid requirement and use technical specification test.
The plugging materials prepared in comparative examples 1 to 3 were then added to water-based slurries (the same as the water-based slurries used in experimental example 1) in an amount of 2% each, and the apparent viscosity, plastic viscosity, dynamic shear force and API fluid loss of the drilling fluid system before and after aging were then tested according to the above-described methods. The test results are shown in Table 3.
TABLE 3 fluid loss properties of drilling fluid systems prepared from the lost circulation materials prepared in example 1, comparative examples 1-3
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The drilling fluid systems prepared from the plugging materials prepared in examples 2-41 were tested for fluid loss performance according to the method described above, and the test results were similar to those of the drilling fluid systems prepared from the plugging materials prepared in example 1.

Claims (10)

1. The preparation method of the plugging material is characterized by comprising the following steps: and (3) in-situ growing calcium carbonate on the MXene material to obtain a composite material, and then in-situ growing molybdenum disulfide on the composite material to obtain the plugging material.
2. The method for producing a plugging material according to claim 1, wherein the MXene material is Ti 2 C 3 MXene micron sheet, ti 2 C 3 Mxene nanoplatelets, tiCN nanoplatelets; the surface of the MXene material contains hydroxyl groups.
3. The method of making a lost circulation material according to claim 1 or 2, wherein the MXene material is made by a process comprising the steps of: and mixing the MAX material with hydrofluoric acid, carrying out solid-liquid separation, drying, and carrying out ultrasonic treatment on the dried solid to obtain the MXene material.
4. The method for producing a plugging material according to claim 3, wherein the concentration of hydrofluoric acid is 0.1 to 0.15mol/L; the volume of hydrofluoric acid corresponding to each 2g of MAX material is 15-25 mL; the mixing time is not less than 24 hours; the power of the ultrasonic treatment is 500-1200W, and the time is not less than 30min.
5. The method of making a lost circulation material of claim 1, wherein the method of in situ growth of calcium carbonate on the MXene material comprises the steps of: and uniformly mixing the MXene material and the solution containing calcium ions, then adding the solution containing carbonate ions, mixing, aging, carrying out solid-liquid separation, and drying to obtain the composite material.
6. The method for producing a plugging material according to claim 5, wherein the calcium ion-containing solution is mainly made of a water-soluble calcium salt and water; or the solution containing calcium ions is mainly prepared from water-soluble calcium salt, a morphology regulator, a surfactant and water; the solution containing carbonate ions is mainly prepared from water-soluble carbonate and water; the ratio of the amount of carbonate ion in the water-soluble carbonate to the amount of calcium ion in the water-soluble calcium salt is (1-1.5): 1; the temperature of mixing in the method for in-situ growth of calcium carbonate on MXene material is not lower than 70 ℃ for not less than 1h; the aging time is 0.5-2 h.
7. The method for producing a plugging material according to claim 6, wherein the mass ratio of the water-soluble calcium salt to water used in the production of the calcium ion-containing solution is (1-15): 100; the mass ratio of the morphology modifier to the water-soluble calcium salt is (5-20): 100; the mass of the surfactant adopted for every 100g of water-soluble calcium salt is not more than 30g; the mass ratio of the MXene material to the water-soluble calcium salt is (1-10): 100.
8. The method of making a lost circulation material of claim 1, wherein the method of growing molybdenum disulfide in situ on the composite material comprises the steps of: uniformly mixing the composite material and the water-soluble tetrathiomolybdate in an organic solvent, standing for at least 12 hours at the temperature of not lower than 200 ℃, carrying out solid-liquid separation, and drying to obtain the plugging material; the mass ratio of the composite material to the organic solvent is (10-30) 100; the mass ratio of the water-soluble tetrathiomolybdate to the organic solvent is (2-10) 100; the organic solvent is a water-soluble organic solvent.
9. A plugging material prepared by the method of preparing a plugging material according to any one of claims 1-8.
10. Use of a plugging material prepared by the method for preparing a plugging material according to any one of claims 1-8 in a drilling fluid.
CN202310428184.0A 2023-04-20 Plugging material and preparation method and application thereof Active CN116478669B (en)

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