CN115505070A - High-temperature-resistant expansion fiber resin plugging material, preparation method thereof and application thereof in leak prevention and plugging of well cementation cement slurry - Google Patents
High-temperature-resistant expansion fiber resin plugging material, preparation method thereof and application thereof in leak prevention and plugging of well cementation cement slurry Download PDFInfo
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- 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
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- 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
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- E21B33/00—Sealing or packing boreholes or wells
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- C09K2208/00—Aspects relating to compositions of drilling or well treatment fluids
- C09K2208/18—Bridging agents, i.e. particles for temporarily filling the pores of a formation; Graded salts
Abstract
The invention discloses a high-temperature-resistant expansion fiber resin plugging material, a preparation method thereof and application thereof in leak prevention and plugging of well cementation cement slurry. The preparation method of the high-temperature-resistant expansion fiber resin plugging material comprises the following steps: s1, adding sodium hydroxide into an acrylic acid solution, and then sequentially adding a chitosan solution, acrylamide, 2-acrylamido-2-methylpropanesulfonic acid and fibers; sequentially adding an initiator and a cross-linking agent, and carrying out polymerization reaction to obtain polymer gel; the solvent adopted by the chitosan solution is glacial acetic acid solution; and drying the polymer gel and then crushing to obtain the granular resin. By using the high temperature resistant expanded fiber resin plugging material, the problem of malignant leakage of the cementing slurry of the fractured stratum can be effectively solved, the processing time and cost for leakage of the cementing slurry of the fractured stratum are greatly reduced, the cementing quality of the fractured stratum is improved, and a new way is opened for solving the problem of leakage stoppage of the cementing slurry of the fractured stratum.
Description
Technical Field
The invention relates to a high-temperature-resistant expansion fiber resin plugging material, a preparation method thereof and application thereof in leak prevention and plugging of well cementation cement slurry, belonging to the technical field of well drilling and well cementation of oil and gas fields.
Background
Along with the expansion of oil gas exploration and development to the fields of deep layers, ultra-deep layers, ocean deep water and the like, the malignant leakage of fractured strata is one of the major engineering technical problems of oil gas wells. Nearly one-fourth of the oil and gas wells around the world have the problem of malignant loss during drilling, which seriously affects the exploration and development process. The fractured formation loss can be divided into micro fracture loss, extended fracture loss and induced fracture loss, and the fractured loss encountered in the actual drilling process is generally the mutual combination of the three types of loss. The leakage degree of the fractured formation mainly depends on the pressure difference between the wellbore pressure and the formation pore pressure, the development degree and the communication condition of a fracture leakage channel, the width and the length of a fracture, the size of a space in the leakage channel and the like.
In the process of well cementation construction, as the density of cement slurry far exceeds the density of drilling fluid, the problem of malignant lost circulation of well cementation cement slurry is more serious, and the vicious loss in the well cementation of fractured stratums often causes insufficient upward return of the cement slurry, so that the upper-layer well section is difficult to be effectively sealed. Meanwhile, due to leakage of fractured strata, displacement capacity of drilling fluid circulation and well cementation displacement is limited, displacement efficiency is low, rock debris in drilling is difficult to remove in time, and the mud cake cleaning effect of flushing fluid is poor, so that the well cementation quality is seriously influenced.
At present, the pressure bearing capacity of the stratum is generally improved by adopting a proper leakage stopping technical measure at home and abroad so as to meet the requirements of well cementation construction operation. Plugging materials such as bridging plugging materials, high-water-loss plugging materials, imbibition swelling plugging materials, flexible gel plugging materials, curable plugging materials, intelligent plugging materials and the like are commonly used for the malignant well leakage plugging of fractured strata. Compared with other plugging materials, the expandable resin plugging material has the advantages of good adaptability to crack channels, good filling and bearing effects and the like.
At present, the leakage prevention and stopping technology of fractured formations at home and abroad is well developed in many aspects, and meanwhile, the combination of field practice results shows that the liquid-absorbing expansion type leakage stopping material has high success rate in treating the leakage problem of drilling fluid of fractured formations, but is still insufficient in treating the leakage problem of well cementing cement slurry of fractured formations. The density of the well cementing cement slurry is greater than that of the drilling fluid, so that the well cementing cement slurry has more serious leakage risk in a fractured stratum. The development of a novel plugging material which can be applied to leak protection and plugging of the cementing slurry of the fractured stratum is urgently needed.
Disclosure of Invention
The invention aims to provide a pressure-bearing, leakage-proof and leakage-stopping material applied to a fractured formation well cementation cement slurry, which can ensure the smooth operation of fractured formation well cementation and solve the problem of leakage prevention and stopping of the fractured formation well cementation cement slurry.
The preparation method of the high-temperature-resistant expansion fiber resin plugging material provided by the invention comprises the following steps of:
s1, adding sodium hydroxide into an acrylic acid solution, and then sequentially adding a chitosan solution, acrylamide, 2-acrylamido-2-methylpropanesulfonic acid and fibers; sequentially adding an initiator and a cross-linking agent, and carrying out polymerization reaction to obtain polymer gel;
the solvent adopted by the chitosan solution is glacial acetic acid solution;
and S2, drying the polymer gel and then crushing to obtain granular resin, namely the high-temperature-resistant expansion fiber resin plugging material.
In the above-mentioned production method, sodium hydroxide reacts with acrylic acid to form sodium carboxylate, which forms internal and external osmotic pressures in the three-dimensional network structure of the resin, and is a main cause of liquid absorption and expansion of the resin.
In the preparation method, the added chitosan has the capability of complexing metal ions and can be combined with heavy metal ions in the stratum to achieve the effects of reducing the content of heavy metals in the stratum, improving the environmental quality of the stratum and protecting an oil gas reservoir, and the chitosan grafted water-absorbent resin has more excellent thermal stability and a loose and porous structure on the surface. The composite material is combined with the original expandable performance of the resin, is beneficial to improving the performances of the expanded resin such as liquid absorption performance, temperature resistance, mechanical strength, stretchability and the like, and has very important significance for the application of the expanded resin in leak protection and leak stoppage of fractured formation cement slurry.
In addition, the chitosan molecular structure has a large number of active groups, and can be subjected to graft copolymerization with various monomers, the chitosan graft expanded resin is mainly prepared by grafting hydrophilic monomers onto the chitosan skeleton through free radical initiated graft copolymerization, and the persulfate initiator is decomposed under the heating condition to generate sulfate radical anion free radicals, and the free radicals extract hydrogen from the active groups on the chitosan, so that alkoxy free radicals are formed on the chitosan skeleton, and the alkoxy is used as an active center to initiate the graft copolymerization.
In the above preparation method, in step S1, the mass concentration of the glacial acetic acid solution is 1 to 3%, preferably 2%;
the fiber is basalt fiber, glass fiber and the like, the diameter of a monofilament is 11-15 mu m, and the length of the monofilament is 2-6 mm;
the basalt fiber has various excellent performances of high strength, corrosion resistance, high temperature resistance and the like, and is suitable for plugging fractured strata;
the fiber can be physically crosslinked with the expansion resin, and the fiber is embedded into the expansion resin gel in the form of irregular needles, so that part of holes are filled. The expansion resin gel added with the fiber strengthens the polymer molecules to form a three-dimensional space network structure, enhances the acting force between the fiber and the polymer molecules, improves the strength and toughness of the resin, and is not easy to break under extrusion. Meanwhile, the fibers and the expansion resin can be extruded together to enter the crack channel, the fibers can be bridged in the crack channel, the resin is expanded to fill small holes after the fiber is bridged, the particles are extruded and stacked, the whole crack channel is compacted and filled, and the technical requirements of well cementation cement slurry leakage stoppage of various complex fractured stratums can be met.
In the preparation method, in step S1, the following raw materials are used, based on 100 parts by weight of water in the polymerization reaction system:
0.5 to 3 weight portions of fiber, 1 to 5 weight portions of chitosan, 0.6 to 3 weight portions of glacial acetic acid, 10 to 15 weight portions of acrylic acid, 1.5 to 2.0 weight portions of acrylamide, 6 to 10 parts of 2-acrylamide-2-methylpropanesulfonic acid, 4 to 8 parts of NaOH, 0.6 to 0.8 part of initiator and 0.05 to 0.08 part of cross-linking agent.
Because the sulfonic acid group has excellent hydrophilic performance and better tolerance to salt and reacts with the vinyl monomer containing sulfonic group which is easy to generate copolymerization reaction, the invention takes 2-acrylamide-2-methyl propanesulfonic acid as comonomer and introduces the sulfonic acid group into the high temperature resistant expansion fiber resin plugging material, thereby improving the expansibility and the salt tolerance of the high temperature resistant expansion fiber resin plugging material.
In addition, when Acrylamide (AM) has-CONH in the molecular chain 2 and-COOH has better water swelling effect than single hydrophilic group. However, experiments show that the expansion ratio of the polymer is in a descending trend along with the further increase of the addition of the Acrylamide (AM), because the crosslinking density of the expanded resin is increased, the pores in the three-dimensional network structure of the polymer are reduced, the molecular chain is in a curled state, and the expansion ratio is reduced, but the strength is improved, so that the expanded resin is more suitable for being added into a well cementing cement slurry system. Therefore, the addition of Acrylamide (AM) is properly increased, the effect is better, the prepared high-temperature-resistant expanded fiber resin plugging material has stable structure, higher strength and good expansibility, is not easy to denature in a high-temperature and high-pressure environment, and is suitable for plugging fractured stratum well cementation cement slurry.
In the above preparation method, the initiator is an oxidation-reduction system, wherein the oxidant is ammonium persulfate, and the reductant is sodium bisulfite or sodium sulfite;
the mass ratio of the oxidant to the reducing agent is 1:1;
the cross-linking agent is N, N-methylene bisacrylamide.
In the preparation method, in the step S1, the temperature of the polymerization reaction is 60-70 ℃, the reaction is stopped when the stirring speed is 500-1000 r/min for 3-5 hours, namely, polymer gel is formed;
in the step S2, the polymer gel is sequentially soaked in ethanol and water, and then dried to constant weight at the temperature of 80-90 ℃ to obtain a solid product.
The high-temperature-resistant expansion fiber resin plugging material provided by the invention has the maximum expansion multiple of 10-21 times, the expansion time of 49-55 min, the salt resistance of 69-80%, the water retention rate of 80-93%, and the strength of 351-448 g/cm when reaching the maximum expansion multiple 2 。
The gel particles formed by the high-temperature-resistant expansion fiber resin plugging material after imbibition expansion have high temperature resistance and elastic toughness, can be extruded into a crack channel together with the bridge plugging fibers under the action of a certain external force, are compacted and filled, and are extruded and stacked along with the continuous imbibition expansion of the gel particles, so that a stacked body is finally formed and the whole crack channel is filled, thereby solving the problem of malignant leakage of well cementation cement slurry in a fractured stratum.
On the basis of the high-temperature-resistant expansion fiber resin plugging material, the invention further provides well cementation cement slurry which comprises the following components in parts by mass:
100 parts of oil well cement, 15-20 parts of coarse silica sand, 10-15 parts of fine silica sand, 0.5-3 parts of the high temperature resistant expansion fiber resin plugging material, 2-5 parts of nano silicon dioxide, 1-10 parts of calcium carbonate, 0-5 parts of fluid loss additive, 0-5 parts of drag reducer, 0.5-2 parts of retarder, 0.2-0.8 part of defoaming agent and 30-100 parts of water;
the particle size of the high-temperature-resistant expansion fiber resin plugging material is 0.01-0.2 mm.
Wherein the oil well cement is API oil well G-grade cement;
the particle size of the coarse silica sand is 50-150 mu m, the coarse silica sand is amorphous white solid powder, and the mass content of silicon dioxide is more than 99 percent;
the particle size of the fine silica sand is 5-15 mu m, the fine silica sand is amorphous white solid powder, and the mass content of silicon dioxide is more than 99 percent;
the nano silicon dioxide is nano silicon dioxide hydrosol and is transparent liquid, wherein the mass content of the silicon dioxide is 20-50%;
the particle size of the calcium carbonate is 0.1-0.3 mm, and the calcium carbonate is white hexagonal crystal solid particles;
the fluid loss agent is a butadiene-styrene latex fluid loss agent;
the drag reducer is sulfonated formaldehyde-acetone polycondensate or polynaphthalene sulfonate drag reducer;
the defoaming agent is a silicon ether copolymerization defoaming agent, an organic siloxane defoaming agent or a polyether defoaming agent;
the retarder is at least one of lignosulfonate retarder, hydroxycarboxylic acid retarder and AMPS polymer retarder;
the well cementation cement slurry is suitable for plugging a 0-3 mm fractured stratum at the temperature of 120-180 ℃;
the pressure-bearing capacity of the high-temperature-resistant expansion fiber resin plugging material or the well cementation cement slurry to a crack with the thickness of 0-3 mm is more than 3.5MPa, the pressure-bearing time can reach more than 10 minutes, and the maximum leakage can be controlled within 86 mL.
The high-temperature-resistant expansion fiber resin plugging material can effectively solve the problem of malignant leakage of the cementing slurry of the fractured stratum well cementation, has simple implementation and low cost, can meet the technical requirement of modern well cementation pressure bearing, greatly reduces the processing time and cost of the leakage of the cementing slurry of the fractured stratum well cementation and improves the well cementation quality of the fractured stratum well cementation, and opens up a new way for solving the problem of leakage plugging of the cementing slurry of the fractured stratum well cementation.
Drawings
FIG. 1 is a graph showing the comparison of the bearing strength of the well cementation and leakage stoppage cement slurry prepared in the examples 1 to 6 to fractures of different widths at 150 ℃.
Detailed Description
The experimental procedures used in the following examples are all conventional procedures unless otherwise specified.
Materials, reagents and the like used in the following examples are commercially available unless otherwise specified.
The invention provides a high-temperature-resistant expansion fiber resin plugging material in a first aspect, which is prepared from the following raw materials:
based on 100 weight portions of deionized water, 0.5 to 3 weight portions of fiber, 1 to 5 weight portions of chitosan, 0.6 to 3 weight portions of glacial acetic acid, 10 to 15 weight portions of acrylic acid, 1.5 to 2.0 weight portions of acrylamide, 6 to 10 weight portions of 2-acrylamide-2-methyl propanesulfonic acid, 4 to 8 weight portions of NaOH, 0.6 to 0.8 weight portion of initiator and 0.05 to 0.08 weight portion of cross-linking agent.
The fiber is preferably basalt fiber, the basalt fiber has various excellent performances such as high strength, corrosion resistance and high temperature resistance, and is suitable for plugging fractured strata, the diameter of a monofilament is 11-15 mu m, and the length of the monofilament is 2-6 mm;
further, the initiator comprises an oxidizing agent and a reducing agent, wherein the oxidizing agent is ammonium persulfate, and the reducing agent is one of sodium bisulfite and sodium sulfite; the mass ratio of oxidant to reductant is 1:1.
Further, the glacial acetic acid is required to be prepared into a dilute solution with the concentration of 2% for dissolving the chitosan, and 30mL of glacial acetic acid with the concentration of 2% is required for dissolving each gram of chitosan.
Further, the cross-linking agent is N, N-methylene bisacrylamide.
The second aspect of the invention provides a preparation method of the high-temperature-resistant expansion fiber resin plugging material, which is prepared by aqueous solution copolymerization, and the preparation method specifically comprises the following steps:
(1) Weighing a certain amount of chitosan, adding the chitosan into a beaker, adding a certain amount of glacial acetic acid solution with the concentration of 2% into the beaker, starting stirring, and stopping stirring until the chitosan is completely dissolved;
(2) Adding a certain amount of deionized water into a three-neck flask, starting stirring, introducing nitrogen, adding a certain amount of Acrylic Acid (AA), and uniformly stirring;
(3) Dissolving a small amount of NaOH particles into the solution obtained in the step (2) for multiple times, sequentially adding the solution obtained in the step (1), acrylamide, 2-acrylamido-2-methylpropanesulfonic acid and fibers after the solution is cooled, uniformly stirring, slowly dropwise adding the solution dissolved with a proper amount of initiator and cross-linking agent into a three-neck flask through a dropping funnel, placing the three-neck flask into a constant-temperature water bath box, stirring, and obtaining polymer gel after the reaction is finished;
(4) Transferring the polymer gel reaction product into a beaker, soaking and washing the polymer gel reaction product with ethanol and pure water in sequence, chopping and drying the product to obtain a solid product, and crushing the solid product to obtain granular resin which is the high-temperature-resistant expansion fiber resin plugging material;
wherein the reaction condition is water bath heating, the temperature is 60-70 ℃, the stirring speed is 500-1000 r/min, when the polymerization reaction forms polymer gel, the stirring is stopped, and the reaction time is 3-5 hours.
Further, after the polymer gel is cooled, the polymer gel is soaked in ethanol and pure water successively and washed repeatedly, the synthesized product can be cut into blocks by scissors or a cutter and the like, and the blocks are placed into a drying box and continuously dried to constant weight at the temperature of 80-90 ℃. After being crushed by a powder particle machine, the obtained granular resin is the high-temperature-resistant expanded fiber resin plugging material, and is suitable for plugging 0-3 mm fractured strata at the temperature of 120-180 ℃.
The third aspect of the invention provides a well cementation leakage prevention and leakage stoppage cement slurry system, wherein the high temperature resistant expansion fiber resin leakage stoppage material can be used in the well cementation cement slurry system and is suitable for leakage prevention and leakage stoppage of 0-3 mm fractured strata at the temperature of 120-180 ℃.
The high-temperature-resistant expansion fiber resin plugging material can be used in a well cementation cement slurry system, and the well cementation cement slurry system comprises the following components in percentage by weight: 100 portions of oil well cement, 15 to 20 portions of coarse silica sand, 10 to 15 portions of fine silica sand, 0.5 to 3 portions of high temperature resistant expansion fiber resin plugging material, 2 to 5 portions of nano silicon dioxide, 1 to 10 portions of calcium carbonate, 0 to 5 portions of fluid loss additive, 0 to 5 portions of drag reducer, 0.5 to 2 portions of retarder, 0.2 to 0.8 portion of defoaming agent and 30 to 100 portions of water.
Wherein the particle size of the high-temperature-resistant expansion fiber resin plugging material is 0.01-0.2 mm.
Further, the coarse silica sand is amorphous white solid powder, the mass content of silicon dioxide is more than 99%, and the particle size is 50-150 μm; the fine silica sand is amorphous white solid powder, the mass content of silicon dioxide is more than 99%, and the particle size is 5-15 mu m.
Further, the well cement is an API well G grade cement.
Further, the defoaming agent is one of a silicon ether copolymerization defoaming agent, an organic siloxane defoaming agent and a polyether defoaming agent.
Further, the nano silicon dioxide is nano silicon dioxide hydrosol which is transparent liquid, and the mass content of the silicon dioxide is 20-50%.
Further, the calcium carbonate is white hexagonal crystal solid particles, and the particle size is 0.1-0.3 mm.
Further, the drag reducer is one of sulfonated formaldehyde-acetone polycondensate and polynaphthalene sulfonate drag reducer.
Further, the fluid loss agent is a butadiene-styrene latex fluid loss agent.
Furthermore, the retarder is one or more than two of lignosulfonate retarder, hydroxycarboxylic acid retarder and AMPS polymer retarder.
The sources of the raw materials used in the following examples and comparative examples are specifically as follows:
acrylic Acid (AA) (grade, analytical grade), acrylamide (AM) (grade, analytical grade), N-methylenebisacrylamide (grade, analytical grade), ammonium persulfate (grade, analytical grade), glacial acetic acid (grade, analytical grade), chitosan (grade, analytical grade), sodium bisulfite (grade, analytical grade), sodium hydroxide (NaOH) (grade, analytical grade) were purchased from national pharmaceutical group chemical agents, inc.
2-acrylamido-2-methylpropanesulfonic Acid (AMPS) (grade, analytically pure) and absolute ethanol (grade, analytically pure) were purchased from Shanghai Allantin Biotech Co., ltd.
Coarse and fine silica sand: purchased from Kathon quartz sand works in Jianping county, liaoning.
Basalt fiber: from smithd engineering materials ltd, tin free.
Calcium carbonate: purchased from Guangzhou Tuoyi trade company Limited.
Defoaming agent: commercially available from Ohio America Petroleum science, inc. under the type DF-E (polyether defoamer).
Drag reducer: commercially available from Olympic Petroleum science, inc. under the type HX-21L (sulfonated formaldehyde-acetone polycondensate).
Fluid loss agent: purchased from Oneka Petroleum science Co., ltd, as model HX-11L (butadiene-styrene latex fluid loss additive).
Retarder: purchased from Kyoto Europe, america, petro-technology, inc. model HX-31L (AMPS polymer retarder).
Nano silicon dioxide: purchased from the island technologies, ltd, beijing, german.
G-grade oil well cement: g-grade oil well cement purchased from Shandong Linji384vici Special Cement Ltd.
Testing the performance of the high-temperature-resistant expansion fiber resin plugging material:
1. maximum expansion multiple test:
taking one 500mL beaker, and taking the mass as M 0 (about 0.3 g) placing the high-temperature-resistant expansion fiber resin plugging material in a beaker, adding 200mL of deionized water at room temperature, filtering excessive water by using a 100-mesh screen after the imbibition expansion reaches the maximum value, standing and draining for 10min, wiping off surface water, weighing the expanded high-temperature-resistant expansion fiber resin plugging material, wherein the mass of the expanded high-temperature-resistant expansion fiber resin plugging material is M 1 The maximum expansion multiple formula of the high-temperature-resistant expansion fiber resin plugging material is as follows:
Q s ＝(M 1 -M 0 )/M 0 (1)
in the formula Q s The maximum expansion factor is expressed in g/g.
2. And (3) testing the swelling time:
and in unit time, the time for the high-temperature expansion resistant fiber resin plugging material to reach the maximum expansion multiple. Weighing mass M 0 (about 0.3 g) of high-temperature-resistant expansion fiber resin plugging material particles are put into a 500mL beaker, 200mL of deionized water is added at room temperature, after a certain time interval, redundant water is filtered out by a screen, the surface water is wiped off, the mass of the expanded gel is weighed, and when the mass is stable, the liquid absorption time T is s The unit is min.
3. And (3) testing salt resistance:
the salt resistance refers to the salinity of water in an oil field or NaCl and CaCl with different concentrations 2 In the saline water, the expansion capacity of the high-temperature expansion resistant fiber resin plugging material is measured, and the high-temperature expansion resistant fiber resin plugging material is generally considered to have better salt resistance when the expansion capacity reaches 50 times or more.
Weighing mass M 0 (about 1 g) placing the high-temperature expansion resistant fiber resin plugging material particles into a 500mL beaker, adding 200mL of NaCl solution with the concentration of 1000mg/L at room temperature, filtering excessive water by using a screen at regular intervals, wiping off surface water, weighing the mass of the gel after expansion, and weighing the mass M of the expanded high-temperature expansion resistant fiber resin plugging material when the mass is stable 1 . The formula of the salt resistance of the high-temperature-resistant expansion fiber resin plugging material is as follows:
K＝(M 1 -M 0 )/(M 0 +Q s )×100％ (2)
wherein K is the salt resistance,%.
4. Testing the water retention rate:
weighing a certain amount of high-temperature-resistant expansion fiber resin plugging material reaching the maximum expansion multiple, and under the same environmental condition, the quality of the high-temperature-resistant expansion fiber resin plugging material in a certain time, wherein the formula of the water retention rate of the high-temperature-resistant expansion fiber resin plugging material is as follows:
B＝(M 1 /M 2 )×100％ (3)
in the formula: b-high temperature resistant expansion fiber resinWater retention of the lost circulation material,%; m 1 The mass g of the high-temperature-resistant expanded fiber resin plugging material in a certain time and under the same environmental conditions; m 2 The mass g of the high temperature expansion resistant fiber resin lost circulation material which reaches the maximum expansion factor.
5. And (3) testing the strength:
after the high-temperature-resistant expansion fiber resin plugging material is fully imbibed and expanded, a cuboid gel sample with the upper surface area of S and the height of 0.9-1.1 cm is taken and placed on an electronic balance, a glass slide with a proper size is placed on the sample, weights are added on the glass slide to uniformly apply pressure until the gel is broken, and the mass M of the weights when the gel is broken is recorded, wherein the unit is g. The larger the E value is, the larger the gel strength of the high-temperature expansion resistant fiber resin plugging material is.
E＝M/S，(4)
In the formula: e-is gel strength, g/cm 2 (ii) a M-is the weight mass, g; s is the upper surface area of the gel in cm 2 。
Example 1 preparation of high temperature resistant expanded fiber resin lost circulation Material
(1) Weighing 2g of chitosan, adding the chitosan into a beaker, adding 60mL of 2% glacial acetic acid solution into the beaker, starting stirring, and stopping stirring after the chitosan is completely dissolved;
(2) Adding 90 g of deionized water into a three-neck flask, starting stirring, introducing nitrogen, adding 18 g of Acrylic Acid (AA), and uniformly stirring;
(3) Dissolving 8g of NaOH particles into the solution obtained in the step 2 for a plurality of times in a small amount, adding the solution obtained in the step 1 after the solution is cooled, sequentially adding 2.2 g of acrylamide, 10 g of 2-acrylamido-2-methylpropanesulfonic acid and 1.5 g of fibers, uniformly stirring, slowly dropwise adding the solution dissolved with 1g of initiator (the oxidant is ammonium persulfate, the reducing agent is sodium bisulfite) and 0.12 g of cross-linking agent (N, N-methylene bisacrylamide) into a three-neck flask through a dropping funnel, stirring the three-neck flask in a constant-temperature water bath at 60 ℃, and obtaining polymer gel after the reaction is finished;
(4) Transferring the polymer gel reaction product into a beaker, soaking and washing the polymer gel reaction product by using ethanol and pure water in sequence, cutting the polymer gel reaction product, drying the product at 90 ℃ to obtain a solid product, and crushing the solid product to obtain granular resin, namely the high-temperature-resistant expansion fiber resin plugging material P1 (the particle size is 0.01-0.2 mm).
The properties of the prepared high temperature resistant expanded fiber resin plugging material P1 are shown in Table 1.
Example 2 preparation of high temperature resistant expanded fiber resin lost circulation material
(1) Weighing 3g of chitosan, adding the chitosan into a beaker, adding 90mL of 2% glacial acetic acid solution into the beaker, starting stirring, and stopping stirring after the chitosan is completely dissolved;
(2) Adding 60 g of deionized water into a three-neck flask, starting stirring, introducing nitrogen, adding 18 g of Acrylic Acid (AA), and uniformly stirring;
(3) Dissolving 8g of NaOH particles into the solution obtained in the step 2 for a plurality of times in a small amount, adding the solution obtained in the step 1 after the solution is cooled, sequentially adding 2.2 g of acrylamide, 10 g of 2-acrylamido-2-methylpropanesulfonic acid and 1.5 g of fibers, uniformly stirring, slowly dropwise adding the solution dissolved with 1g of initiator (the oxidant is ammonium persulfate, the reducing agent is sodium bisulfite) and 0.12 g of cross-linking agent (N, N-methylene bisacrylamide) into a three-neck flask through a dropping funnel, stirring the three-neck flask in a constant-temperature water bath at 60 ℃, and obtaining polymer gel after the reaction is finished;
(4) And transferring the polymer gel reaction product into a beaker, sequentially soaking and washing the polymer gel reaction product by using ethanol and pure water, cutting the polymer gel reaction product, drying the cut product at 90 ℃ to obtain a solid product, and crushing the solid product to obtain granular resin, namely the high-temperature-resistant expanded fiber resin plugging material P2 (the grain diameter is 0.01-0.2 mm).
The properties of the obtained high temperature resistant expanded fiber resin plugging material P2 are shown in Table 1.
Example 3 preparation of high temperature resistant expanded fiber resin lost circulation Material
The high temperature resistant expanded fiber resin lost circulation material was prepared in the same manner as in example 2, except that: 20 g of acrylic acid were added in step (2) and 9 g of NaOH pellets were added in step (3). The properties of the prepared high temperature resistant expanded fiber resin plugging material P3 are shown in Table 1 (the particle size is 0.01-0.2 mm).
Example 4 preparation of high temperature resistant expanded fiber resin lost circulation Material
The high temperature resistant expanded fiber resin lost circulation material was prepared in the same manner as in example 2, except that: in step (3), 2.5 g of acrylamide and 15 g of 2-acrylamido-2-methylpropanesulfonic acid are added. The properties of the obtained high temperature resistant expanded fiber resin plugging material P4 are shown in Table 1.
Example 5 preparation of high temperature resistant expanded fiber resin lost circulation Material
The high temperature resistant expanded fiber resin lost circulation material was prepared in the same manner as in example 2, except that: in step (3) 2.5 grams of basalt fibers are added. The properties of the prepared high temperature resistant expanded fiber resin plugging material P5 are shown in Table 1 (the particle size is 0.01-0.2 mm).
Example 6 preparation of high temperature resistant expanded fiber resin lost circulation Material
The high temperature resistant expanded fiber resin lost circulation material was prepared in the same manner as in example 2, except that: in step (3) 0.075 g of crosslinker was added. The properties of the prepared high temperature resistant expanded fiber resin plugging material P6 are shown in Table 1 (the particle size is 0.01-0.2 mm).
Comparative examples 1,
The high temperature resistant expanded fiber resin lost circulation material was prepared in the same manner as in example 2, except that: in the step (1), no chitosan or glacial acetic acid solution is added, and in the step (2), the deionized water is 150 g. The properties of the obtained high temperature resistant expanded fiber resin lost circulation material DP1 are shown in Table 1.
Comparative examples 2,
The high temperature resistant expanded fiber resin lost circulation material was prepared in the same manner as in example 2, except that: no Acrylamide (AM) was added. The properties of the high temperature resistant expanded fiber resin lost circulation material DP2 are shown in Table 1.
Comparative examples 3,
The high temperature resistant expanded fiber resin lost circulation material was prepared in the same manner as in example 2, except that: 2-acrylamido-2-methylpropanesulfonic Acid (AMPS) was not added. The properties of the high temperature resistant expanded fiber resin lost circulation material DP3 are shown in Table 1.
Comparative examples 4,
The high temperature resistant expanded fiber resin lost circulation material was prepared in the same manner as in example 2, except that: acrylamide (AM) and 2-acrylamido-2-methylpropanesulfonic Acid (AMPS) were not added. The properties of the high temperature resistant expanded fiber resin lost circulation material DX4 are shown in Table 1.
Comparative examples 5,
The high temperature resistant expanded fiber resin lost circulation material was prepared in the same manner as in example 2, except that: basalt fibers were not added. The properties of the high temperature resistant expanded fiber resin lost circulation material DX5 are shown in Table 1.
Comparative examples 6,
The high temperature resistant expanded fiber resin lost circulation material was prepared in the same manner as in example 1, except that: the temperature of the polymerization water bath was 70 ℃. The properties of the high temperature resistant expanded fiber resin lost circulation material DX6 are shown in Table 1.
Table 1 shows the properties of different high temperature resistant expanded fiber resin lost circulation materials:
as can be seen from the results in Table 1, the high temperature expansion resistant fiber resin plugging materials of examples P1 to P5 of the invention have the maximum expansion times of 10 to 21 times, the expansion time of 49 to 55min, the salt resistance of 69 to 80 percent and the water retention of 80 to 93 percent, and the strength of the plugging material is 351 to 448g/cm when the maximum expansion times are reached 2 The expansion capacity of the sodium chloride solution with the mineralization degree of 1000mg/L is reduced, but the strength of the sodium chloride solution is improved, and the maximum expansion multiple can reach more than 62 percent of the maximum expansion multiple in deionized water. The gel strength of the plugging material is 351g/cm 2 The above shows that the plugging material of the invention has good liquid absorption and expansion capacity, liquid retention capacity, good salt resistance, and higher strength, and is suitable for plugging fractured stratum well cementation cement slurry. It can be seen from comparative examples 1 to 6 that the addition of chitosan slightly reduces the swelling capacity of the resin, the addition of basalt fiber can significantly improve the strength and toughness of the resin, the amide group in Acrylamide (AM) can improve the swelling capacity of the resin, the sulfonic acid group in 2-acrylamido-2-methylpropanesulfonic Acid (AMPS) can improve the salt resistance of the resin, and the liquid-absorbing swelling capacity is better when the polymerization temperature is 60 ℃.
Testing the plugging performance of cement paste:
installing a crack die with a crack width of 0-3 mm in a rock core dynamic simulation experiment device, fixing, applying stratum confining pressure by a pressure pump, filling cement slurry into a slurry barrel with the capacity of 2000mL, screwing a barrel cover and sealing, turning on a stirrer to select the revolution number of 200rmp/min, setting the temperature and turning on a heating switch. After the container is sealed, the pressure is increased to 7.5MPa at the rate of 0.10MPa/s until the loss of the cement slurry in the container is finished, and the volume of the leaked cement slurry and the maximum pressure value reached are recorded when the pressure is 0.5, 1.0, 1.5, 2.0, 2.5, 3.0, 3.5, 4.0, 4.5, 5.0, 5.5, 6.0, 6.5, 7.0 and 7.5MPa respectively. If plugging is successful, maintaining the pressure for 10min, and recording the leakage.
The plugging performance of the high temperature resistant expanded fiber resin plugging material in the well cementation cement slurry is further described by the application examples and application comparative examples, but the invention is not limited to the application examples and application comparative examples.
The experimental method comprises the following steps: preparing well cementation cement slurry according to a standard GB/T19139-2012 oil well cement test method, and testing the performance of a well cementation cement slurry system according to a standard SY/T6544-2017 oil well cement slurry performance requirement.
The "parts" described in the application examples and comparative examples are "parts by mass".
Application example 1 for preparing well cementation and leakage stoppage cement slurry
The significance of the application example is to explain the application of the high-temperature-resistant fiber water-absorbent resin plugging material in the leakage prevention and plugging of the well cementation cement slurry.
The well cementation leaking stoppage cement slurry is prepared from the following raw materials in parts by mass: 100 parts of oil well cement (API oil well G-grade cement), 15 parts of coarse silica sand (the particle size is 50-150 mu m, the coarse silica sand is amorphous white solid powder, the mass content of silicon dioxide is more than 99%), 15 parts of fine silica sand (the particle size is 5-15 mu m, the amorphous white solid powder, the mass content of silicon dioxide is more than 99%), 1 part of high temperature expansion resistant fiber resin plugging material (the particle size is 0.01-0.2 mm), 3 parts of nano silica (nano silica hydrosol which is transparent liquid, wherein the mass content of silicon dioxide is 20-50%), 4 parts of calcium carbonate (the particle size is 0.1-0.3 mm, the white hexagonal crystal solid particles), 1 part of dewatering agent, 2 parts of drag reducer, 1 part of retarder and 0.3 part of defoaming agent, the plugging agent is prepared by using the water-cement ratio of 0.38, the solid phase material is continuously and uniformly poured into a stirring cup to be mixed with the liquid phase material in 15s at the rotating speed of 4000rmp, then the rotating speed is adjusted to 120rm00 p, and the plugging cement slurry is prepared by stirring, and the G1 is obtained.
Application example 2 preparation of well cementation leaking stoppage cement slurry
The well cementation leaking stoppage cement slurry is prepared from the following raw materials in parts by mass: 100 parts of oil well cement, 15 parts of coarse silica sand, 15 parts of fine silica sand, 2 parts of high temperature resistant expanded fiber resin plugging material, 3 parts of nano silicon dioxide, 4 parts of calcium carbonate, 1 part of fluid loss additive, 2 parts of drag reducer, 1 part of retarder and 0.3 part of defoaming agent, and cement slurry is prepared by taking the water-cement ratio as 0.38 to prepare the well cementation plugging cement slurry G2.
The preparation method is the same as that of application example 1.
Application example 3 preparation of well cementation and leakage stoppage cement slurry
The well cementation and leakage stoppage cement slurry is prepared from the following raw materials in parts by mass: 100 parts of oil well cement, 15 parts of coarse silica sand, 15 parts of fine silica sand, 3 parts of high temperature resistant expanded fiber resin plugging material, 3 parts of nano silicon dioxide, 4 parts of calcium carbonate, 1 part of fluid loss additive, 2 parts of drag reducer, 1 part of retarder and 0.3 part of defoaming agent, and cement slurry is prepared with the water cement ratio of 0.38 to prepare the well cementation and plugging cement slurry G3.
The preparation method is the same as that of application example 1.
Application example 4 preparation of well cementation and leakage stoppage cement slurry
The well cementation and leakage stoppage cement slurry is prepared from the following raw materials in parts by mass: 100 parts of oil well cement, 15 parts of coarse silica sand, 15 parts of fine silica sand, 2 parts of high-temperature-resistant expanded fiber resin plugging material, 3 parts of nano-silica, 8 parts of calcium carbonate, 1 part of fluid loss additive, 2 parts of drag reducer, 1 part of retarder and 0.3 part of defoamer, and cement slurry is prepared according to the water-cement ratio of 0.38 to prepare the well cementation and plugging cement slurry G4.
The preparation method is the same as that of application example 1.
Application example 5 preparation of well cementation and leakage stoppage cement slurry
The well cementation and leakage stoppage cement slurry is prepared from the following raw materials in parts by mass: 100 parts of oil well cement, 20 parts of coarse silica sand, 10 parts of fine silica sand, 2 parts of high temperature resistant expanded fiber resin plugging material, 3 parts of nano silicon dioxide, 4 parts of calcium carbonate, 1 part of fluid loss additive, 2 parts of drag reducer, 1 part of retarder and 0.3 part of defoaming agent, and cement slurry is prepared by taking the water-cement ratio as 0.38 to prepare the well cementation plugging cement slurry G5.
The preparation method is the same as that of application example 1.
Application example 6 preparation of well cementation and leakage stoppage cement slurry
The well cementation and leakage stoppage cement slurry is prepared from the following raw materials in parts by mass: 100 parts of oil well cement, 15 parts of coarse silica sand, 15 parts of fine silica sand, 2 parts of high temperature resistant expanded fiber resin plugging material, 5 parts of nano silicon dioxide, 4 parts of calcium carbonate, 1 part of fluid loss additive, 2 parts of drag reducer, 1 part of retarder and 0.3 part of defoaming agent, and cement slurry is prepared by taking the water-cement ratio as 0.38 to prepare the well cementation plugging cement slurry G6.
The preparation method is the same as that of application example 1.
Application comparative example 1,
Wherein, the well cementation leakage stoppage cement slurry system is prepared according to the method corresponding to the application example 2, and the difference is that: high temperature resistant expansion fiber resin plugging material is not used. Thereby preparing the well cementation leaking stoppage cement slurry DG1.
Comparative example 2 was used,
Wherein, the well cementation leakage stoppage cement slurry system is prepared according to the method corresponding to the application example 2, and the difference is that: calcium carbonate is not used. Thereby preparing the well cementation leaking stoppage cement slurry DG2.
Application comparative example 3,
Wherein, the well cementation leakage stoppage cement slurry system is prepared according to the method corresponding to the application example 2, and the difference is that: coarse and fine silica sand is not added. Thereby preparing the well cementation leaking stoppage cement slurry DG3.
Application comparative example 4,
Wherein, the well cementation leakage stoppage cement slurry system is prepared according to the method corresponding to the application example 2, and the difference is that: no nanosilica was added. Thereby preparing the well cementation leaking stoppage cement slurry DG4.
Application comparative example 5,
Wherein, prepare the well cementation leaking stoppage cement slurry system according to the method corresponding to application example 2 separately, the difference lies in: 5 parts of fluid loss agent. Thereby preparing the well cementation leaking stoppage cement slurry DG5.
Comparative example 6 was used,
Wherein, the well cementation leakage stoppage cement slurry system is prepared according to the method corresponding to the application example 2, and the difference is that: and 5 parts of drag reducer. Thereby preparing the well cementation leaking stoppage cement slurry DG6.
Comparative application example 7,
Wherein, the well cementation leakage stoppage cement slurry system is prepared according to the method corresponding to the application example 2, and the difference is that: and 2 parts of a retarder. Thereby preparing the well cementation leaking stoppage cement slurry DG7.
Comparative application example 8,
Wherein, the well cementation leakage stoppage cement slurry system is prepared according to the method corresponding to the application example 2, and the difference is that: 0.8 part of defoaming agent. Thereby preparing the well cementation leaking stoppage cement slurry DG8.
Test examples 1,
The results of measuring the compressive strength and elastic modulus of the cement slurry G1-G6 and DG 1-DG 8 for the plugging performance at 150 ℃ for a 0.25mm crack and the cement slurry after curing for 5 days are shown in Table 2.
TABLE 2 leak-stopping performance and cement slurry performance of different well cementation and leak-stopping cement slurries for 0.25mm cracks at 150 DEG C
According to the data in the table 2, it can be seen from G1 to G3 and DG1 that the addition of the high temperature expansion resistant fiber resin plugging material can make the cement paste have good plugging performance for 0.25mm cracks under the condition of 150 ℃, but the compressive strength and the elastic modulus after the cement stone is cured for 5 days are reduced by too much addition. The comparison of G4-G6 and DG 2-DG 4 can discover that calcium carbonate can improve the leakage stoppage performance and compressive strength of cement paste, reduce the elastic modulus of set cement, and nano-silica not only can effectively improve the compressive strength of set cement, but also can effectively reduce the elastic modulus of set cement, slightly promotes the leakage stoppage performance, and the added silica sand can effectively further optimize the compressive strength and toughness of set cement to a cement paste system, and promotes the leakage stoppage performance of cement paste. DG 5-DG 8 show that the addition of various additives of the cement paste has great influence on the performance of the cement paste, and the proper addition does not have great influence on the plugging performance of the cement paste. In conclusion, the high-temperature-resistant expansion fiber resin plugging material can enable the pressure-bearing capacity of cement paste to 0.25mm cracks to reach more than 7MPa at the temperature of 150 ℃, the pressure-bearing time to be longer than 10min, the leakage loss to be less than 26mL, and the plugging performance to be good.
Test examples 2,
The results of measuring the compressive strength and elastic modulus of the well cementation and leaking stoppage cement slurries G1 to G6 for the leak stoppage performance of the well cementation and leaking stoppage cement slurries to 1.5mm cracks under the temperature condition of 120 ℃ to 180 ℃ and the cement stones for 5 days are shown in Table 3.
TABLE 3 plugging Properties and grout Properties of different cementing and plugging grouts at 120-180 deg.C for 1.5mm crack
According to the data in the table 3, the well cementation and leaking stoppage cement slurries G1 to G6 can effectively block 1.5mm cracks at the temperature of 120-180 ℃, the pressure bearing capacity is more than 5.0MPa, the leakage amount can be controlled within 56mL, and the pressure bearing time can reach more than 10 minutes. Along with the rise of the temperature, the plugging pressure-bearing capacity is slightly reduced after being firstly improved to 180 ℃, because the liquid absorption speed and the liquid absorption capacity of the resin are improved due to the fact that molecular thermal motion is accelerated after the temperature is increased, but the gel strength is reduced after expansion when the temperature is increased to 180 ℃, and the maximum pressure-bearing capacity of the gel particle stacking and plugging layer is reduced. Through comparison, the compressive strength of the set cement can be gradually increased and the elastic modulus gradually decreases after the temperature is increased, which shows that the plugging cement slurry system has good high-temperature resistance. The test example shows that the addition of the high temperature resistant expansion fiber resin plugging material can lead the cement slurry to have good plugging performance on 1.5mm cracks under the temperature condition of 120-180 ℃.
Test examples 3,
The results of the plugging performance of the well cementation plugging cement slurries G1 to G6 on 3mm cracks at the temperature of 120 ℃ to 180 ℃ are shown in Table 4.
TABLE 4 plugging Properties of different cementing and plugging slurries at 120-180 deg.C for 3mm cracks
| Plugging cement slurry | Crack width/mm | Temperature/. Degree.C | Bearing capacity/MPa | Bearing time/min | leakage/mL |
| G1 | 3 | 120 | 3.5 | >10 | 86 |
| G2 | 3 | 120 | 4.5 | >10 | 64 |
| G3 | 3 | 120 | 5.0 | >10 | 54 |
| G4 | 3 | 120 | 5.0 | >10 | 57 |
| G5 | 3 | 120 | 4.5 | >10 | 67 |
| G6 | 3 | 120 | 4.5 | >10 | 68 |
| G1 | 3 | 150 | 4.0 | >10 | 73 |
| G2 | 3 | 150 | 5.5 | >10 | 47 |
| G3 | 3 | 150 | 5.5 | >10 | 44 |
| G4 | 3 | 150 | 6.0 | >10 | 38 |
| G5 | 3 | 150 | 5.0 | >10 | 55 |
| G6 | 3 | 150 | 5.5 | >10 | 45 |
| G1 | 3 | 180 | 4.0 | >10 | 71 |
| G2 | 3 | 180 | 5.5 | >10 | 48 |
| G3 | 3 | 180 | 5.0 | >10 | 58 |
| G4 | 3 | 180 | 5.5 | >10 | 49 |
| G5 | 3 | 180 | 5.0 | >10 | 59 |
| G6 | 3 | 180 | 5.5 | >10 | 47 |
According to the data in the table 4, the well cementation and leaking stoppage cement slurries G1 to G6 can effectively block 3mm cracks at the temperature of 120-180 ℃, the pressure bearing capacity is more than 3.5MPa, the leakage amount can be controlled within 86mL, and the pressure bearing time can reach more than 10 minutes. Compared with a 1.5mm crack, the pressure bearing capacity is reduced, but the pressure bearing can be carried out for more than 10 min. The test example can prove that the high-temperature-resistant expanded fiber resin plugging material provided by the invention has good plugging performance on 3mm cracks at 120-180 ℃ when added into a well cementation cement slurry system.
FIG. 1 is a comparison graph of the pressure-bearing strength of the well cementation leaking stoppage cement slurry of the embodiment 1-6 applied to fractures with different widths at 150 ℃, and according to the comparison graph, the well cementation cement slurry added with the high temperature resistant expansion fiber resin leaking stoppage material can effectively block the fractures with 0-3 mm, and has good stability resistance and strong pressure-bearing capacity, which shows that the invention has good practical application effect.
Test example 4: influence of addition of high-temperature-resistant expansion fiber resin plugging material on cement paste performance
The well cementation cement slurry in the application example 1 is used as a test object, slurry is prepared according to the oil well cement test method in the standard GB/T19139-2012, the high temperature expansion resistant fiber resin plugging material and the cement slurry are uniformly stirred in different mixing ratios, the rheological property of the mixture is measured by using a ZNN-D6 type rotary viscometer, and the thickening time of the mixture is measured by using a high temperature and high pressure thickener.
TABLE 5 compatibility test of high temperature resistant expanded fiber resin plugging material with well cementation cement slurry
According to the data in the table 5, the rheological mode of the cement slurry added with the high-temperature-resistant expansion fiber resin plugging material conforms to the power law mode, the influence on the rheological property of the well cementation cement slurry is small, and the thickening time and the compressive strength can meet the relevant requirements of field well cementation construction.
In conclusion, the high-temperature-resistant expanded fiber resin plugging material provided by the invention can better solve the problem of leakage prevention and plugging of the existing fractured formation well cementation cement slurry, can effectively improve the fractured formation well cementation quality, and has a better application prospect.
Claims (10)
1. A preparation method of a high-temperature-resistant expansion fiber resin plugging material comprises the following steps:
s1, adding sodium hydroxide into an acrylic acid solution, and then sequentially adding a chitosan solution, acrylamide, 2-acrylamido-2-methylpropanesulfonic acid and fibers; sequentially adding an initiator and a cross-linking agent, and carrying out polymerization reaction to obtain polymer gel;
the solvent adopted by the chitosan solution is glacial acetic acid solution;
and S2, drying the polymer gel and then crushing to obtain granular resin, namely the high-temperature-resistant expansion fiber resin plugging material.
2. The method of claim 1, wherein: in the step S1, the mass concentration of the glacial acetic acid solution is 1-3%;
the fiber is basalt fiber or glass fiber, the diameter of the monofilament is 11-15 mu m, and the length of the monofilament is 2-6 mm.
3. The production method according to claim 1 or 2, characterized in that: in the step S1, the amount of each raw material is as follows, based on 100 parts by weight of water in the polymerization reaction system:
0.5 to 3 portions of fiber, 1 to 5 portions of chitosan, 0.6 to 3 portions of glacial acetic acid, 10 to 15 portions of acrylic acid, 1.5 to 2.0 portions of acrylamide, 6 to 10 portions of 2-acrylamide-2-methylpropanesulfonic acid, 4 to 8 portions of NaOH, 0.6 to 0.8 portion of initiator and 0.05 to 0.08 portion of cross-linking agent.
4. The production method according to any one of claims 1 to 3, characterized in that: the initiator is an oxidation-reduction system, wherein the oxidant is ammonium persulfate, and the reducing agent is sodium bisulfite or sodium sulfite;
the mass ratio of the oxidant to the reducing agent is 1:1;
the cross-linking agent is N, N-methylene bisacrylamide.
5. The production method according to any one of claims 1 to 4, characterized in that: in the step S1, the temperature of the polymerization reaction is 60-70 ℃, and the reaction is carried out for 3-5 hours under the condition that the stirring speed is 500-1000 r/min;
in the step S2, the polymer gel is sequentially soaked in ethanol and water, and then dried to constant weight at the temperature of 80-90 ℃ to obtain a solid product.
6. The high-temperature expansion resistant fiber resin plugging material obtained by the preparation method of any one of claims 1 to 5;
the high-temperature-resistant expansion fiber resin plugging material has the maximum expansion multiple of 10-21 times, the expansion time of 49-55 min, the salt resistance of 69-80 percent, the water retention rate of 80-93 percent and the strength of 351-448 g/cm when reaching the maximum expansion multiple 2 。
7. A well cementation cement slurry comprises the following components by mass:
100 parts of oil well cement, 15-20 parts of coarse silica sand, 10-15 parts of fine silica sand, 0.5-3 parts of the high temperature resistant expanded fiber resin plugging material of claim 6, 2-5 parts of nano silica, 1-10 parts of calcium carbonate, 0-5 parts of a fluid loss agent, 0-5 parts of a drag reducer, 0.5-2 parts of a retarder, 0.2-0.8 part of a defoaming agent and 30-100 parts of water;
the particle size of the high-temperature-resistant expansion fiber resin plugging material is 0.01-0.2 mm.
8. A cementing slurry according to claim 7, characterized in that: the oil well cement is API oil well G-grade cement;
the grain size of the coarse silica sand is 50-150 mu m;
the particle size of the fine silica sand is 5-15 mu m;
the nano silicon dioxide is nano silicon dioxide hydrosol, wherein the mass content of the silicon dioxide is 20-50%;
the particle size of the calcium carbonate is 0.1-0.3 mm;
the fluid loss agent is a butadiene-styrene latex fluid loss agent;
the drag reducer is sulfonated formaldehyde-acetone polycondensate or polynaphthalene sulfonate drag reducer;
the defoaming agent is a silicon ether copolymerization defoaming agent, an organic siloxane defoaming agent or a polyether defoaming agent;
the retarder is at least one of lignosulfonate retarder, hydroxycarboxylic acid retarder and AMPS polymer retarder.
9. The high temperature resistant expansion fiber resin plugging material as defined in claim 6 and the application of the well cementation cement slurry as defined in claim 7 or 8 in the leak prevention and plugging of the well cementation cement slurry in fractured strata.
10. Use according to claim 9, characterized in that: the high-temperature-resistant expansion fiber resin plugging material or the well cementation cement slurry is suitable for plugging a 0-3 mm fractured stratum at the temperature of 120-180 ℃;
the pressure-bearing capacity of the high-temperature-resistant expansion fiber resin plugging material or the well cementation cement slurry to a crack with the thickness of 0-3 mm is more than 3.5MPa, the pressure-bearing time can reach more than 10 minutes, and the maximum leakage can be controlled within 86 mL.
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| CN202211259382.0A CN115505070A (en) | 2022-10-14 | 2022-10-14 | High-temperature-resistant expansion fiber resin plugging material, preparation method thereof and application thereof in leak prevention and plugging of well cementation cement slurry |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116333701A (en) * | 2023-04-12 | 2023-06-27 | 中国石油大学(华东) | Leak stopping agent and cement slurry system suitable for leak prevention and stopping of hard and brittle stratum |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116333701A (en) * | 2023-04-12 | 2023-06-27 | 中国石油大学(华东) | Leak stopping agent and cement slurry system suitable for leak prevention and stopping of hard and brittle stratum |
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