CN110746948A - High-strength composite plugging agent - Google Patents
High-strength composite plugging agent Download PDFInfo
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- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/42—Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells
- C09K8/46—Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells containing inorganic binders, e.g. Portland cement
- C09K8/467—Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells containing inorganic binders, e.g. Portland cement containing additives for specific purposes
- C09K8/487—Fluid loss control additives; Additives for reducing or preventing circulation loss
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Abstract
The invention discloses a high-strength composite plugging agent, and belongs to the technical field of oilfield development. According to the invention, bentonite, iron powder and the like are used as raw materials, and an organic-inorganic phase-linked high-stability composite system is constructed by multiple water absorption and dehydration effects accompanied with oxidation effects and combination of activated yeast, so that the problem of precipitation and filtration loss is not easy to occur; macromolecular components such as 2-acrylamide-2-methylbenzenesulfonic acid, allyl polyoxyethylene ether and the like are used as raw materials to prepare a composite reinforcing material, and the composite reinforcing material is matched with micromolecular amphiphilic components under the action of space and charges to improve the stability of a system. The invention solves the problems that the common plugging agent is easy to precipitate and lose leakage and has poor plugging strength.
Description
Technical Field
The invention relates to the technical field of oilfield development, in particular to a high-strength composite plugging agent.
Background
The lost circulation is a complex underground condition that working fluids (including drilling fluid, cement slurry, completion fluid and other working fluids) are leaked into a stratum under the action of pressure difference in various underground operation processes of drilling, cementing, testing or repairing and the like of petroleum and natural gas exploration and development, and is one of the most common technical problems in drilling engineering. It is called a downhole complication because it occurs mostly not artificially, not at human will, and of course, this statement is not accurate enough. If a lost circulation path is encountered which is capable of producing lost circulation, but a corresponding effective measure is taken, it is possible that lost circulation will not occur, at least to a much reduced extent. Secondly, even if the fine pores of the stratum do not cause the well leakage, when some measures taken by the stratum are not suitable for actual conditions, such as construction pressure exceeds the fracture pressure of the stratum, the serious well leakage can be caused, which is directly shown in that the liquid level of a mud tank on the ground is reduced, or the return amount of drilling fluid at a well head is less than the normal discharge amount of a pump, or no drilling fluid at the well head returns.
The research of the lost circulation prevention and control technology is emphasized in the early 40 s abroad; in the 50 s, researches on a well leakage mechanism and a leakage prevention and stopping mechanism, a leakage layer testing method and a leakage stopping process technology are greatly developed; in the 60-70 s, research on a leaking stoppage simulation test device and a leaking stoppage mechanism is developed, the characteristics and the leaking stoppage rule of leaking layers in various leaking areas are gradually mastered, various leaking stoppage methods and leaking stoppage processes are gradually mature, and the leaking stoppage success rate is obviously improved; in the 80-90 s, a series of composite plugging agents with a reservoir protection effect are developed, and the plugging success rate is improved again; the theoretical research on the well leakage is emphasized, and the research on leakage stoppage test equipment and leakage stoppage tools is developed to a high level. In order to improve the working efficiency of drilling, reduce the loss of working fluid such as operating time and mud, reduce the damage to a reservoir and the like to obtain the maximum economic benefit, the leakage stoppage process while drilling provides a method for solving the problem, and the leakage stoppage process is a leakage stoppage technology along with the drilling in the drilling engineering. The leak stopping agent while drilling is a novel leak stopping agent which is developed recently at home and abroad and has good use effect. At present, 801 plugging agent while drilling is a powdery product prepared by scientifically compounding and processing a plurality of high molecular compounds such as wood powder (a wood containing vegetable gum and containing cellulose, lignin, pentosan and the like), humate, carboxymethyl cellulose and the like. The NFU leakage stopping agent is a powdery or granular product prepared by compounding a plurality of high molecular compounds such as nanmu root powder (a root of a bushy shrub containing plant gum and formed by crushing), humic acid high-valence metal salt, starch carboxymethyl sodium, polyacrylamide and the like by a scientific method and matching with inert materials with different varieties, different granularities and different addition amounts. The NFDF8012 plugging agent is a powdery or granular product which is compounded by a plurality of macromolecular compounds such as nanmu root powder, humic acid high-valence metal salt or derivatives thereof, ammonium methyl cellulose, polyacrylamide, leather powder and the like through scientific formula and scientific method and added with inert materials with different amounts, different granularities and different varieties. These plugging agents while drilling have been used in more than 300 units in coal fields, metallurgy, nonferrous, nuclear industry, petroleum, chemical industry, building materials and other industries.
The leak-proof plugging agent while drilling has unique advantages in the aspect of preventing permeability and fractured leakage. The method has the advantages of less investment, simple method, no need of stopping drilling, great reduction of the processing time and cost of oil and gas lost circulation, great significance for improving the drilling speed of a lost stratum and reducing the drilling cost, but the common plugging agent is easy to precipitate and lose during use at present, has poor plugging strength and needs to be enhanced.
Disclosure of Invention
The technical problems to be solved by the invention are as follows: aiming at the problems that the common plugging agent is easy to precipitate and lose leakage and the plugging strength is poor when the common plugging agent is used at present, the high-strength composite plugging agent is provided.
In order to solve the technical problems, the invention adopts the following technical scheme:
a high-strength composite plugging agent comprises the following components in parts by weight: 40-60 parts of oil well cement, 8-13 parts of sepiolite, 10-15 parts of quartz sand, 4-8 parts of epoxy resin and 1-3 parts of foaming agent, and further comprises: 35-50 parts of composite plugging base material and 18-30 parts of composite reinforcing material.
The preparation method of the composite plugging base material comprises the following steps:
(1) washing bentonite, adding calcium oxide accounting for 20-35% of the mass of the bentonite and iron powder accounting for 12-18% of the mass of the bentonite, mixing and ball-milling to obtain a ball grinding material, drying the ball grinding material, calcining at 400-550 ℃, cooling to obtain a calcined material, crushing and sieving the calcined material, collecting sieved particles according to a mass ratio of 1: 5-8, adding a reagent, mixing and stirring, standing at room temperature, filtering, taking filter residues, and drying to obtain a magnetic material, wherein the mass ratio of the magnetic material to the filter residues is 1: 30-50 taking yeast powder and active bacterial liquid, mixing and stirring, standing and activating at 24-27 ℃ to obtain yeast liquid, wherein the mass ratio of the yeast liquid to the active bacterial liquid is 10-15: 3: 0.2 taking the magnetic material, the pretreated fiber and the yeast liquid, mixing and stirring to obtain a base material;
(2) according to the weight parts, 30-50 parts of base material, 3-7 parts of calcium carbonate, 2-5 parts of acrylamide, 0.1-0.4 part of cerium sulfate, 3-7 parts of silicon-containing material, 1-4 parts of β -D-mannuronic acid, 0.4-0.8 part of ammonium dihydrogen phosphate, 6-10 parts of talcum powder and 15-25 parts of acetic acid solution are taken, the base material, the calcium carbonate, the cerium sulfate and the talcum powder are mixed and stirred at 20-30 ℃, the acrylamide, the β -D-mannuronic acid, the ammonium dihydrogen phosphate and the acetic acid solution are added and mixed, the temperature is increased to 35-50 ℃, the mixture is stirred and evaporated under reduced pressure to obtain concentrated material, the concentrated material is taken, sealed and kept stand, sterilized and evaporated in a rotating mode to obtain the composite plugging base material.
The reagent in the step (1): according to the mass ratio of 1: and 10-15, mixing hydrogen peroxide and HCl solution to obtain the reagent.
The pretreatment of the fiber material in the step (1): crushing and sieving the cucurbituril pith to obtain a sieved substance, and weighing the sieved substance according to a mass ratio of 5: 0.3-0.7: 1: and 25, adding polyethyleneimine, glutaraldehyde and NaOH solution, mixing and stirring, cooling, carrying out suction filtration, and drying a filter cake to obtain the pretreated fiber.
The active solution in the step (2): according to the mass parts, 2-5 parts of guar gum, 3-7 parts of casein, 2-5 parts of yeast extract, 1-3 parts of potassium chloride, 1-4 parts of tartaric acid and 300-500 parts of wort are mixed to obtain the active liquid.
The silicon-containing material in the step (2): according to the mass ratio of 5-8: 3: 10 mixing mercaptopropyltriethoxysilane, ethyl orthosilicate and polyvinyl alcohol to obtain the silicon-containing material.
The preparation of the composite reinforcing material comprises the following steps: under the nitrogen atmosphere, according to parts by weight, taking 25-35 parts of 2-acrylamide-2-methylbenzene sulfonic acid, 7-12 parts of allyl polyoxyethylene ether, 7-12 parts of acrylamide, 1-3 parts of dodecyl mercaptan and 60-80 parts of NaOH solution, mixing and stirring at 30-45 ℃ to obtain a mixed material, heating to 60-75 ℃, adding an initiator accounting for 1-3% of the mixed material, mixing and stirring, keeping the temperature, standing, cooling, adding acetone accounting for 40-55% of the mixed material, mixing and stirring, filtering, taking a filter cake, drying, crushing and sieving, and taking sieved particles according to the mass ratio of 7-12: 1, adding auxiliary materials, mixing and grinding to obtain the composite reinforcing material.
The initiator is as follows: according to the mass ratio of 5: and 1-2, mixing sodium bisulfite and sodium persulfate to obtain the initiator.
The auxiliary materials are as follows: according to the mass ratio of 3-7: 1: 1 mixing polyethylene wax, castor oil and magnesium stearate to obtain the auxiliary material.
The foaming agent is as follows: according to the mass ratio of 3: 1: and 2-5, mixing sodium silicate, sodium bicarbonate and sodium laureth sulfate to obtain the foaming agent.
Compared with other methods, the method has the beneficial technical effects that:
(1) the invention washes the bentonite, which can make the bentonite have water, then mixes with calcium oxide and iron powder for ball milling, generates calcium hydroxide to generate heat, makes the iron powder be oxidized partially and partially, and the calcium hydroxide is converted into calcium oxide in the high temperature calcining process, the iron powder is completely converted into ferroferric oxide, the dispersion effect is promoted by multi-layer action from inside to outside, then the calcium oxide is mixed and activated by a reagent with oxidation and acidification effects to generate heat and provide more active sites, the quantity of surface functional groups is increased, the invention combines with the pretreated fiber material which adopts polyethyleneimine and glutaraldehyde cross-linking treatment to the silk melon net, carries out immobilization treatment to the yeast, and covalently combines with amino, hydroxyl, sulfhydryl, imidazolyl and other groups on the surface of the yeast, so as to form a biological net structure between cells, thereby forming tiny magnetic particles, bacteria, The fiber component and the yeast cell-lined high mechanical strength are integrated to form an organic-inorganic high-stability composite system, the stability of the internal performance can be obviously improved, the added silicon-containing material can also provide an additional adsorption site for the immobilization of yeast, wherein hydroxyl carried by polyvinyl alcohol and silanol groups of organoalkoxysilane form strong hydrogen bonds, so that the integral mechanical strength is further increased, and the plugging agent is not easy to precipitate and filter out and has the problem of influencing the plugging strength;
(2) according to the invention, macromolecular components such as 2-acrylamide-2-methyl benzene sulfonic acid and allyl polyoxyethylene ether are used as raw materials to prepare the composite reinforcing material, the branched chain of the composite reinforcing material has volume and electrical repulsion characteristics, so that the polymer is not easy to curl and wind, comb-type shear resistance and good dispersion characteristics can be formed in the application process, the precipitation filtration loss and the reduction of leaking stoppage strength are avoided, castor oil and polyethylene wax added in auxiliary materials can also play a role in adjusting the viscosity of a system, the contact leaking stoppage is convenient to carry out, and the castor oil has amphipathy, so that the internal compatibility can be well provided, and the application effect is improved;
(3) according to the invention, bentonite, iron powder and the like are used as raw materials, a high-stability composite system with organic-inorganic phase connection is constructed by multiple water absorption and dehydration effects accompanied with oxidation effects and activated saccharomycetes, the problem of precipitation and filtration loss is not easy to occur, a comb-shaped polymer is polymerized from macromolecular components, and the stability of the system is improved by matching with micromolecular amphiphilic components under the effects of space and charges.
Detailed Description
Pretreating fiber materials: crushing the cucurbita pepo seeds in a crusher, sieving the crushed cucurbita pepo seeds with a 100-mesh sieve to obtain a sieved substance, and sieving the sieved substance in a water bath at 35-55 ℃ according to a mass ratio of 5: 0.3-0.7: 1: and 25, adding polyethyleneimine, glutaraldehyde and a 12% NaOH solution by mass, mixing and stirring for 30-55 min, naturally cooling to room temperature, carrying out suction filtration, taking a filter cake, and drying in an oven at 65-80 ℃ to obtain the pretreated fiber.
Active liquid: according to the mass parts, 2-5 parts of guar gum, 3-7 parts of casein, 2-5 parts of yeast extract, 1-3 parts of potassium chloride, 1-4 parts of tartaric acid and 300-500 parts of wort with the mass fraction of 15% are mixed to obtain the active liquid.
Silicon-containing material: according to the mass ratio of 5-8: 3: 10 mixing mercaptopropyltriethoxysilane, ethyl orthosilicate and polyvinyl alcohol to obtain the silicon-containing material.
Reagent: according to the mass ratio of 1: and (3) mixing 55% of hydrogen peroxide by volume fraction and 16% of HCl solution by mass fraction to obtain the reagent.
Initiator: according to the mass ratio of 5: and 1-2, mixing sodium bisulfite and sodium persulfate to obtain the initiator.
Auxiliary materials: according to the mass ratio of 3-7: 1: 1 mixing polyethylene wax, castor oil and magnesium stearate to obtain the auxiliary material.
Foaming agent: according to the mass ratio of 3: 1: and 2-5, mixing sodium silicate, sodium bicarbonate and sodium laureth sulfate to obtain the foaming agent.
The preparation method of the composite plugging base material comprises the following steps:
(1) washing bentonite with water for 2-4 times, adding calcium oxide accounting for 20-35% of the mass of the bentonite and iron powder accounting for 12-18% of the mass of the bentonite, mixing the mixture in a ball milling tank, ball milling the mixture for 1-3 hours at a speed of 350-550 r/min to obtain a ball milling material, drying the ball milling material in an oven at a temperature of 90-100 ℃ for 10-13 hours, transferring the ball milling material to a muffle furnace, calcining the ball milling material for 3-5 hours at a temperature of 400-550 ℃, cooling the ball milling material to room temperature along with the furnace to obtain a calcined material, crushing the calcined material in a crusher, sieving the crushed calcined material with an 80-mesh sieve, and collecting sieved particles: 5-8, adding a reagent, mixing and stirring for 20-35 min, standing at room temperature for 1-3 h, filtering, taking filter residues, and drying to obtain a magnetic material, wherein the mass ratio of the magnetic material to the filter residues is 1: 30-50 taking yeast powder and active bacterial liquid, mixing and stirring for 25-45 min, standing and activating for 20-24 h at 24-27 ℃ to obtain yeast liquid, wherein the mass ratio of the yeast liquid to the active bacterial liquid is 10-15: 3: 0.2, mixing and stirring the magnetic material, the pretreated fiber and the yeast liquid for 30-50 min to obtain a base material;
(2) according to the weight parts, 30-50 parts of base material, 3-7 parts of calcium carbonate with the particle size of 150-200 mu m, 2-5 parts of acrylamide, 0.1-0.4 part of cerium sulfate, 3-7 parts of silicon-containing material, 1-4 parts of β -D-mannuronic acid, 0.4-0.8 part of ammonium dihydrogen phosphate, 6-10 parts of talcum powder and 15-25 parts of acetic acid solution with the mass fraction of 15% are taken, the base material, the calcium carbonate, the cerium sulfate and the talcum powder are mixed in a reaction kettle, the mixture is magnetically stirred for 40-60 min at the speed of 350-550 r/min, the acrylamide, the β -D-mannuronic acid, the ammonium dihydrogen phosphate and the acetic acid solution are added and mixed, the temperature is increased to 35-50 ℃, the mixture is magnetically stirred for 25-45 min at the speed of 500-800 r/min, the concentrated material is subjected to reduced pressure evaporation to 30-45% of the original volume to obtain the concentrated material, the concentrated material is taken and is sealed and stands for 3-5 days, the temperature is kept for 10-15 min at the temperature of.
Preparing a composite reinforcing material: under the nitrogen atmosphere, according to parts by weight, taking 25-35 parts of 2-acrylamide-2-methylbenzene sulfonic acid, 7-12 parts of allyl polyoxyethylene ether, 7-12 parts of acrylamide, 1-3 parts of dodecyl mercaptan and 60-80 parts of a 12% NaOH solution in terms of mass fraction, mixing in a 30-45 ℃ reaction kettle, magnetically stirring for 25-50 min at a speed of 400-700 r/min to obtain a mixed material, heating to 60-75 ℃, adding an initiator accounting for 1-3% of the mixed material, mixing and stirring for 30-45 min, keeping the temperature and standing for 1-3 h, naturally cooling to room temperature, adding acetone accounting for 40-55% of the mixed material, mixing and stirring for 20-35 min, filtering, taking a filter cake, drying for 1-3 h in a 65-80 ℃ oven, crushing and sieving with a 100-mesh sieve, taking sieved particles according to a mass ratio of 7-12: 1, adding auxiliary materials, mixing and grinding for 1-3 hours to obtain the composite reinforcing material.
A high-strength composite plugging agent comprises the following components in parts by weight: 40-60 parts of oil well cement, 8-13 parts of sepiolite, 10-15 parts of quartz sand, 4-8 parts of epoxy resin, 1-3 parts of foaming agent, 35-50 parts of composite plugging base material and 18-30 parts of composite reinforcing material.
Example 1
Pretreating fiber materials: crushing the cucurbita pepo seeds in a crusher, sieving the crushed cucurbita pepo seeds with a 100-mesh sieve to obtain a sieved substance, and sieving the sieved substance at 35 ℃ in a water bath according to a mass ratio of 5: 0.3: 1: 25, adding polyethyleneimine, glutaraldehyde and a 12% NaOH solution by mass, mixing and stirring for 30min, naturally cooling to room temperature, carrying out suction filtration, taking a filter cake, and drying in a 65 ℃ oven to obtain the pretreated fiber.
Active liquid: according to the mass parts, 2 parts of guar gum, 3 parts of casein, 2 parts of yeast extract, 1 part of potassium chloride, 1 part of tartaric acid and 300 parts of wort with the mass fraction of 15% are mixed to obtain the active liquid.
Silicon-containing material: according to the mass ratio of 5: 3: 10 mixing mercaptopropyltriethoxysilane, ethyl orthosilicate and polyvinyl alcohol to obtain the silicon-containing material.
Reagent: according to the mass ratio of 1: and 10, mixing 55% of hydrogen peroxide by volume fraction and 16% of HCl solution by mass fraction to obtain the reagent.
Initiator: according to the mass ratio of 5: 1, mixing sodium bisulfite and sodium persulfate to obtain the initiator.
Auxiliary materials: according to the mass ratio of 3: 1: 1 mixing polyethylene wax, castor oil and magnesium stearate to obtain the auxiliary material.
Foaming agent: according to the mass ratio of 3: 1: 2 mixing sodium silicate, sodium bicarbonate and sodium laureth sulfate to obtain the foaming agent.
The preparation method of the composite plugging base material comprises the following steps:
(1) washing bentonite with water for 2 times, adding calcium oxide accounting for 20% of the mass of the bentonite and iron powder accounting for 12% of the mass of the bentonite, mixing the mixture in a ball milling tank, ball milling the mixture for 1h at 350r/min to obtain ball grinding materials, drying the ball grinding materials in a 90 ℃ oven for 10h, transferring the ball grinding materials to a muffle furnace, calcining the ball grinding materials at 400 ℃ for 3h, cooling the ball grinding materials to room temperature along with the furnace to obtain calcined materials, crushing the calcined materials in a crusher, sieving the calcined materials with a 80-mesh sieve, collecting sieved particles according to a mass ratio of 1: and 5, adding a reagent, mixing and stirring for 20min, standing at room temperature for 1h, filtering, taking filter residues, and drying to obtain a magnetic material, wherein the mass ratio of the magnetic material to the filter residues is 1: 30, mixing and stirring the yeast powder and the active bacterial liquid for 25min, standing and activating at 24 ℃ for 20h to obtain yeast liquid, wherein the mass ratio of the yeast liquid to the active bacterial liquid is 10: 3: 0.2 taking the magnetic material, the pretreated fiber and the yeast liquid, mixing and stirring for 30min to obtain a base material;
(2) according to the weight portion, 30 portions of base material, 3 portions of calcium carbonate with the grain diameter of 150 mu m, 2 portions of acrylamide, 0.1 portion of cerium sulfate, 3 portions of silicon-containing material, 1 portion of β -D-mannuronic acid, 0.4 portion of ammonium dihydrogen phosphate, 6 portions of talcum powder and 15 portions of acetic acid solution with the mass fraction of 15 percent are taken, the base material, the calcium carbonate, the cerium sulfate and the talcum powder are taken to be mixed in a reaction kettle at the temperature of 20 ℃, the mixture is magnetically stirred for 40min at the speed of 350r/min, the acrylamide, β -D-mannuronic acid, the ammonium dihydrogen phosphate and the acetic acid solution are added to be mixed, the temperature is increased to 35 ℃, the mixture is magnetically stirred for 25min at the speed of 500r/min, the concentrated material is obtained after being decompressed and evaporated to 30min of the original volume, the concentrated material is taken to be sealed and kept stand for 3 days, the temperature.
Preparing a composite reinforcing material: under the nitrogen atmosphere, according to the weight portion, 25 portions of 2-acrylamide-2-methyl benzene sulfonic acid, 7 portions of allyl polyoxyethylene ether, 7 portions of acrylamide, 1 portion of dodecyl mercaptan and 60 portions of NaOH solution with the mass fraction of 12% are mixed in a 30 ℃ reaction kettle, magnetic stirring is carried out for 25min at the speed of 400r/min to obtain a mixed material, the temperature is raised to 60 ℃, an initiator with the mass of 1% of the mixed material is added to be mixed and stirred for 30min, the mixed material is kept warm and kept stand for 1h, the mixed material is naturally cooled to the room temperature, acetone with the mass of 40% of the mixed material is added to be mixed and stirred for 20min, filtering is carried out, a filter cake is taken out, dried in a 65 ℃ oven for 1h, and: 1, adding auxiliary materials, mixing and grinding for 1 hour to obtain the composite reinforcing material.
A high-strength composite plugging agent comprises the following components in parts by weight: 40 parts of oil well cement, 8 parts of sepiolite, 10 parts of quartz sand, 4 parts of epoxy resin, 1 part of foaming agent, 35 parts of composite plugging base material and 18 parts of composite reinforcing material.
Example 2
Pretreating fiber materials: crushing the cucurbita pepo seeds in a crusher, sieving the crushed cucurbita pepo seeds with a 100-mesh sieve to obtain a sieved substance, and sieving the sieved substance in a water bath at 55 ℃ according to a mass ratio of 5: 0.7: 1: 25, adding polyethyleneimine, glutaraldehyde and a 12% NaOH solution by mass, mixing and stirring for 55min, naturally cooling to room temperature, carrying out suction filtration, taking a filter cake, and drying in an oven at 80 ℃ to obtain the pretreated fiber.
Active liquid: according to the mass parts, 5 parts of guar gum, 7 parts of casein, 5 parts of yeast extract, 3 parts of potassium chloride, 4 parts of tartaric acid and 500 parts of wort with the mass fraction of 15% are mixed to obtain the active liquid.
Silicon-containing material: according to the mass ratio of 8: 3: 10 mixing mercaptopropyltriethoxysilane, ethyl orthosilicate and polyvinyl alcohol to obtain the silicon-containing material.
Reagent: according to the mass ratio of 1: 15, mixing 55% of hydrogen peroxide by volume fraction and 16% of HCl solution by mass fraction to obtain the reagent.
Initiator: according to the mass ratio of 5: and 2, mixing sodium bisulfite and sodium persulfate to obtain the initiator.
Auxiliary materials: according to the mass ratio of 7: 1: 1 mixing polyethylene wax, castor oil and magnesium stearate to obtain the auxiliary material.
Foaming agent: according to the mass ratio of 3: 1: 5 mixing sodium silicate, sodium bicarbonate and sodium laureth sulfate to obtain the foaming agent.
The preparation method of the composite plugging base material comprises the following steps:
(1) washing bentonite with water for 4 times, adding calcium oxide accounting for 35% of the mass of the bentonite and iron powder accounting for 18% of the mass of the bentonite, mixing the mixture in a ball milling tank, ball milling the mixture for 3 hours at 550r/min to obtain a ball milling material, drying the ball milling material in a 100 ℃ oven for 13 hours, transferring the ball milling material to a muffle furnace, calcining the ball milling material at 550 ℃ for 5 hours, cooling the ball milling material to room temperature along with the furnace to obtain a calcined material, crushing the calcined material in a crusher, sieving the calcined material with an 80-mesh sieve, and collecting sieved particles according to a mass ratio of 1: 8, adding a reagent, mixing and stirring for 35min, standing at room temperature for 3h, filtering, taking filter residues, and drying to obtain a magnetic material, wherein the mass ratio of the magnetic material to the filter residues is 1: 50, mixing and stirring the yeast powder and the active bacterial liquid for 45min, standing and activating at 27 ℃ for 24h to obtain yeast liquid, wherein the mass ratio of the yeast liquid to the active bacterial liquid is 15: 3: 0.2 taking the magnetic material, the pretreated fiber and the yeast liquid, mixing and stirring for 50min to obtain a base material;
(2) according to the weight portion, 50 portions of base material, 7 portions of calcium carbonate with the grain diameter of 200 mu m, 5 portions of acrylamide, 0.4 portion of cerous sulfate, 7 portions of silicon-containing material, 4 portions of β -D-mannuronic acid, 0.8 portion of ammonium dihydrogen phosphate, 10 portions of talcum powder and 25 portions of acetic acid solution with the mass fraction of 15% are taken, the base material, the calcium carbonate, the cerous sulfate and the talcum powder are taken to be mixed in a reaction kettle at the temperature of 30 ℃, the mixture is magnetically stirred for 60min at the speed of 550r/min, the acrylamide, β -D-mannuronic acid, the ammonium dihydrogen phosphate and the acetic acid solution are added to be mixed, the temperature is increased to 50 ℃, the mixture is magnetically stirred for 45min at the speed of 800r/min, the concentrated material is obtained by decompression and evaporation, the concentrated material is taken to be sealed and kept stand for 5 days, the temperature is kept and sterilized for 15.
Preparing a composite reinforcing material: under the nitrogen atmosphere, according to the weight portion, 35 portions of 2-acrylamide-2-methyl benzene sulfonic acid, 12 portions of allyl polyoxyethylene ether, 12 portions of acrylamide, 3 portions of dodecyl mercaptan and 80 portions of NaOH solution with the mass fraction of 12% are mixed in a 45 ℃ reaction kettle, magnetic stirring is carried out for 50min at the speed of 700r/min to obtain a mixed material, the temperature is increased to 75 ℃, an initiator with the mass of 3% of the mixed material is added to be mixed and stirred for 45min, the mixed material is kept warm and kept stand for 3h, the mixed material is naturally cooled to the room temperature, acetone with the mass of 55% of the mixed material is added to be mixed and stirred for 35min, filtering is carried out, a filter cake is taken out, dried in an 80 ℃ oven for 3h, and: 1, adding auxiliary materials, mixing and grinding for 3 hours to obtain the composite reinforcing material.
A high-strength composite plugging agent comprises the following components in parts by weight: 60 parts of oil well cement, 13 parts of sepiolite, 15 parts of quartz sand, 8 parts of epoxy resin, 3 parts of foaming agent, 50 parts of composite plugging base material and 30 parts of composite reinforcing material.
Example 3
Pretreating fiber materials: crushing the cucurbita pepo seeds in a crusher, sieving the crushed cucurbita pepo seeds with a 100-mesh sieve to obtain a sieved substance, and sieving the sieved substance in a mass ratio of 5: 0.5: 1: 25, adding polyethyleneimine, glutaraldehyde and a 12% NaOH solution by mass, mixing and stirring for 45min, naturally cooling to room temperature, carrying out suction filtration, taking a filter cake, and drying in an oven at 70 ℃ to obtain the pretreated fiber.
Active liquid: according to the mass parts, 3 parts of guar gum, 5 parts of casein, 3 parts of yeast extract, 2 parts of potassium chloride, 2 parts of tartaric acid and 400 parts of wort with the mass fraction of 15% are mixed to obtain the active liquid.
Silicon-containing material: according to the mass ratio of 6: 3: 10 mixing mercaptopropyltriethoxysilane, ethyl orthosilicate and polyvinyl alcohol to obtain the silicon-containing material.
Reagent: according to the mass ratio of 1: and 12, mixing 55% of hydrogen peroxide by volume fraction and 16% of HCl solution by mass fraction to obtain the reagent.
Initiator: according to the mass ratio of 5: 1.5 mixing sodium bisulfite and sodium persulfate to obtain the initiator.
Auxiliary materials: according to the mass ratio of 5: 1: 1 mixing polyethylene wax, castor oil and magnesium stearate to obtain the auxiliary material.
Foaming agent: according to the mass ratio of 3: 1: and 3, mixing sodium silicate, sodium bicarbonate and sodium laureth sulfate to obtain the foaming agent.
The preparation method of the composite plugging base material comprises the following steps:
(1) washing bentonite with water for 3 times, adding calcium oxide accounting for 25% of the mass of the bentonite and iron powder accounting for 15% of the mass of the bentonite, mixing the mixture in a ball milling tank, ball milling for 2 hours at 450r/min to obtain a ball milling material, drying the ball milling material in a 95 ℃ oven for 12 hours, transferring the ball milling material to a muffle furnace, calcining for 4 hours at 450 ℃, cooling the ball milling material to room temperature along with the furnace to obtain a calcined material, crushing the calcined material in a crusher, sieving the calcined material with an 80-mesh sieve, and collecting sieved particles according to a mass ratio of 1: 7, adding a reagent, mixing and stirring for 25min, standing for 2h at room temperature, filtering, taking filter residues, and drying to obtain a magnetic material, wherein the mass ratio of the magnetic material to the filter residues is 1: and 40, mixing and stirring the yeast powder and the active bacterial liquid for 35min, standing and activating at 25 ℃ for 22h to obtain yeast liquid, wherein the mass ratio of the yeast liquid to the active bacterial liquid is 13: 3: 0.2 taking the magnetic material, the pretreated fiber and the yeast liquid, mixing and stirring for 40min to obtain a base material;
(2) according to the weight portion, 40 portions of base material, 5 portions of calcium carbonate with the grain diameter of 190 mu m, 3 portions of acrylamide, 0.2 portion of cerous sulfate, 5 portions of silicon-containing material, 3 portions of β -D-mannuronic acid, 0.6 portion of ammonium dihydrogen phosphate, 8 portions of talcum powder and 20 portions of acetic acid solution with the mass fraction of 15% are taken, the base material, the calcium carbonate, the cerous sulfate and the talcum powder are taken to be mixed in a reaction kettle at 25 ℃, the mixture is magnetically stirred for 50min at 450r/min, the acrylamide, β -D-mannuronic acid, the ammonium dihydrogen phosphate and the acetic acid solution are added to be mixed, the temperature is increased to 40 ℃, the mixture is magnetically stirred for 35min at 600r/min, the concentrated material is obtained after being decompressed and evaporated to 35min of the original volume, the concentrated material is taken to be sealed and kept stand for 4 days, the temperature is kept and the sterilization is carried.
Preparing a composite reinforcing material: under the nitrogen atmosphere, according to the weight portion, 30 portions of 2-acrylamide-2-methyl benzene sulfonic acid, 10 portions of allyl polyoxyethylene ether, 11 portions of acrylamide, 2 portions of dodecyl mercaptan and 70 portions of NaOH solution with the mass fraction of 12% are mixed in a reaction kettle at 35 ℃, magnetic stirring is carried out for 30min at the speed of 600r/min to obtain a mixed material, the temperature is increased to 65 ℃, an initiator with the mass of 2% of the mixed material is added to be mixed and stirred for 35min, the mixed material is kept warm and kept stand for 2h, the mixed material is naturally cooled to the room temperature, acetone with the mass of 45% of the mixed material is added to be mixed and stirred for 25min, filtering is carried out, a filter cake is taken out, dried in an oven at the temperature of 70 ℃ for: 1, adding auxiliary materials, mixing and grinding for 2 hours to obtain the composite reinforcing material.
A high-strength composite plugging agent comprises the following components in parts by weight: 50 parts of oil well cement, 10 parts of sepiolite, 12 parts of quartz sand, 6 parts of epoxy resin, 2 parts of foaming agent, 40 parts of composite plugging base material and 20 parts of composite reinforcing material.
Comparative example 1: the preparation was essentially the same as in example 1 except that the composite lost circulation base was absent.
Comparative example 2: essentially the same procedure as in example 1 was followed except that the composite reinforcement was absent.
Comparative example 3: the high-strength composite plugging agent is produced by a certain company in Shanghai city.
The high-strength composite plugging agent obtained in the above examples and comparative examples is carried out according to SY/T5840-2007 indoor test method for bridging plugging material for drilling fluid of oil and gas industry standard of the people's republic of China. Heating to 100 ℃ by using a DLM-01 type leaking stoppage simulation device produced by Bohai sea drilling engineering institute. A vertical seam template with the thickness of 5mm, the seam height of 50mm and the seam width of 3mm is selected for detection, and the obtained results are shown in Table 1.
Table 1:
| detecting items | Example 1 | Example 2 | Example 3 | Comparative example 1 | Comparative example 2 | Comparative example 3 |
| Plugging time/s | 170 | 176 | 173 | 201 | 210 | 280 |
| Bearing pressure/MPa | 7.0 | 6.5 | 6.3 | 5.2 | 5.3 | 3.5 |
| Loss of fluid condition | Is not lost | Is not lost | Is not lost | Micro leakage | Micro leakage | Loss of fluid |
| Plugging effect | Success of the method | Success of the method | Success of the method | 10min15ml | 10min15ml | 10min25ml |
In summary, it can be seen from table 1 that the high strength composite plugging agent of the present invention is more effective and is worth popularizing, and the above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A high-strength composite plugging agent comprises the following components in parts by weight: 40-60 parts of oil well cement, 8-13 parts of sepiolite, 10-15 parts of quartz sand, 4-8 parts of epoxy resin and 1-3 parts of foaming agent, and is characterized by further comprising: 35-50 parts of composite plugging base material and 18-30 parts of composite reinforcing material.
2. The high-strength composite plugging agent as claimed in claim 1, wherein the preparation method of the composite plugging base material comprises the following steps:
(1) washing bentonite, adding calcium oxide accounting for 20-35% of the mass of the bentonite and iron powder accounting for 12-18% of the mass of the bentonite, mixing and ball-milling to obtain a ball grinding material, drying the ball grinding material, calcining at 400-550 ℃, cooling to obtain a calcined material, crushing and sieving the calcined material, collecting sieved particles according to a mass ratio of 1: 5-8, adding a reagent, mixing and stirring, standing at room temperature, filtering, taking filter residues, and drying to obtain a magnetic material, wherein the mass ratio of the magnetic material to the filter residues is 1: 30-50 taking yeast powder and active bacterial liquid, mixing and stirring, standing and activating at 24-27 ℃ to obtain yeast liquid, wherein the mass ratio of the yeast liquid to the active bacterial liquid is 10-15: 3: 0.2 taking the magnetic material, the pretreated fiber and the yeast liquid, mixing and stirring to obtain a base material;
(2) according to the weight parts, 30-50 parts of base material, 3-7 parts of calcium carbonate, 2-5 parts of acrylamide, 0.1-0.4 part of cerium sulfate, 3-7 parts of silicon-containing material, 1-4 parts of β -D-mannuronic acid, 0.4-0.8 part of ammonium dihydrogen phosphate, 6-10 parts of talcum powder and 15-25 parts of acetic acid solution are taken, the base material, the calcium carbonate, the cerium sulfate and the talcum powder are mixed and stirred at 20-30 ℃, the acrylamide, the β -D-mannuronic acid, the ammonium dihydrogen phosphate and the acetic acid solution are added and mixed, the temperature is increased to 35-50 ℃, the mixture is stirred and evaporated under reduced pressure to obtain concentrated material, the concentrated material is taken, sealed and kept stand, sterilized and evaporated in a rotating mode to obtain the composite plugging base material.
3. The high-strength composite plugging agent according to claim 2, wherein the reagents in the step (1): according to the mass ratio of 1: and 10-15, mixing hydrogen peroxide and HCl solution to obtain the reagent.
4. The high-strength composite plugging agent according to claim 2, wherein the pre-treated fiber material in the step (1): crushing and sieving the cucurbituril pith to obtain a sieved substance, and weighing the sieved substance according to a mass ratio of 5: 0.3-0.7: 1: and 25, adding polyethyleneimine, glutaraldehyde and NaOH solution, mixing and stirring, cooling, carrying out suction filtration, and drying a filter cake to obtain the pretreated fiber.
5. The high-strength composite plugging agent as claimed in claim 2, wherein the active liquid in the step (2): according to the mass parts, 2-5 parts of guar gum, 3-7 parts of casein, 2-5 parts of yeast extract, 1-3 parts of potassium chloride, 1-4 parts of tartaric acid and 300-500 parts of wort are mixed to obtain the active liquid.
6. The high-strength composite plugging agent as claimed in claim 2, wherein the silicon-containing material in the step (2): according to the mass ratio of 5-8: 3: 10 mixing mercaptopropyltriethoxysilane, ethyl orthosilicate and polyvinyl alcohol to obtain the silicon-containing material.
7. The high-strength composite plugging agent as claimed in claim 1, wherein the preparation of the composite reinforcing material comprises the following steps: under the nitrogen atmosphere, according to parts by weight, taking 25-35 parts of 2-acrylamide-2-methylbenzene sulfonic acid, 7-12 parts of allyl polyoxyethylene ether, 7-12 parts of acrylamide, 1-3 parts of dodecyl mercaptan and 60-80 parts of NaOH solution, mixing and stirring at 30-45 ℃ to obtain a mixed material, heating to 60-75 ℃, adding an initiator accounting for 1-3% of the mixed material, mixing and stirring, keeping the temperature, standing, cooling, adding acetone accounting for 40-55% of the mixed material, mixing and stirring, filtering, taking a filter cake, drying, crushing and sieving, and taking sieved particles according to the mass ratio of 7-12: 1, adding auxiliary materials, mixing and grinding to obtain the composite reinforcing material.
8. The high-strength composite plugging agent as claimed in claim 7, wherein the initiator: according to the mass ratio of 5: and 1-2, mixing sodium bisulfite and sodium persulfate to obtain the initiator.
9. The high-strength composite plugging agent as claimed in claim 7, wherein the auxiliary materials are: according to the mass ratio of 3-7: 1: 1 mixing polyethylene wax, castor oil and magnesium stearate to obtain the auxiliary material.
10. The high-strength composite plugging agent as claimed in claim 1, wherein the foaming agent: according to the mass ratio of 3: 1: and 2-5, mixing sodium silicate, sodium bicarbonate and sodium laureth sulfate to obtain the foaming agent.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111560240A (en) * | 2020-07-16 | 2020-08-21 | 海塔石油科技有限公司 | Ultramicro-grade channeling and plugging agent as well as preparation method and application thereof |
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| CN115321918A (en) * | 2022-08-29 | 2022-11-11 | 贵州大学 | Mine water inrush channel plugging material and preparation method thereof |
| CN117070202A (en) * | 2023-10-17 | 2023-11-17 | 西南石油大学 | Acid-soluble high-strength consolidation plugging agent and preparation method thereof |
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