CN115093164A - Adhesive blocking agent and preparation method thereof - Google Patents

Adhesive blocking agent and preparation method thereof Download PDF

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CN115093164A
CN115093164A CN202210431623.9A CN202210431623A CN115093164A CN 115093164 A CN115093164 A CN 115093164A CN 202210431623 A CN202210431623 A CN 202210431623A CN 115093164 A CN115093164 A CN 115093164A
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parts
water
reaction
agent
washing
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CN115093164B (en
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姚花平
王光义
张道法
李曼平
申振坤
游家庆
李博良
刘伟
徐靖文
张恒
王小鹏
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Henan Ruitong Energy Engineering Technology Co ltd
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Puyang Huaruitong Energy Engineering Technology Co ltd
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    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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    • C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
    • C—CHEMISTRY; METALLURGY
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    • C04B14/00—Use of inorganic materials as fillers, e.g. pigments, for mortars, concrete or artificial stone; Treatment of inorganic materials specially adapted to enhance their filling properties in mortars, concrete or artificial stone
    • C04B14/02—Granular materials, e.g. microballoons
    • C04B14/04—Silica-rich materials; Silicates
    • C04B14/042—Magnesium silicates, e.g. talc, sepiolite
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    • C04B22/00—Use of inorganic materials as active ingredients for mortars, concrete or artificial stone, e.g. accelerators, shrinkage compensating agents
    • C04B22/06—Oxides, Hydroxides
    • C04B22/066—Magnesia; Magnesium hydroxide
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    • C04B24/00—Use of organic materials as active ingredients for mortars, concrete or artificial stone, e.g. plasticisers
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    • C04B24/124—Amides
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    • C04B24/00—Use of organic materials as active ingredients for mortars, concrete or artificial stone, e.g. plasticisers
    • C04B24/16—Sulfur-containing compounds
    • C04B24/18—Lignin sulfonic acid or derivatives thereof, e.g. sulfite lye
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    • C04B24/00—Use of organic materials as active ingredients for mortars, concrete or artificial stone, e.g. plasticisers
    • C04B24/24—Macromolecular compounds
    • C04B24/26—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
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    • C04B24/24—Macromolecular compounds
    • C04B24/26—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
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    • C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
    • C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
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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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Abstract

The invention relates to the technical field of oil field operation well repair, in particular to a plugging agent for well cementation for treating casing leakage and a preparation method thereof. The patch plugging agent comprises the following components in parts by weight: 46-50 parts of superfine cement; 41-46 parts of mineral powder; 1-3 parts of superfine silica fume; 1-3 parts of sepiolite powder; 0.2-0.8 of magnetic high molecular polymer; 3-5 parts of a swelling agent; 1-2 parts of aminophosphonic acid chelating resin; 0.2-0.5 of drag reduction retarder. The plugging agent for well cementation can realize smooth circulation in a narrow-gap annular short well section, and can form compact, impermeable, thin-wall and net-shaped cement cakes at a sleeve broken section and a crack inlet.

Description

Adhesive blocking agent and preparation method thereof
Technical Field
The invention relates to the technical field of workover in oilfield operation, in particular to a well cementation plugging agent for treating casing leakage and a preparation method thereof.
Background
With the extension of the development time of the oil field, due to the factors of 'plastic flow' of a salt layer, ground stress, mineralization degree and the like, and the fact that produced water is seriously corroded and frequent fracturing and acidizing measures are implemented, the service life of an oil layer casing is overlong, and formation water and leakage are caused by the phenomena of perforation, casing deformation, damage and the like caused by corrosion of a free section and a sealing section of the casing, so that the normal production of an oil well is seriously influenced, and even the oil well cannot be normally produced and discarded. The well is ineffective for water injection. The number of newly-added casing damage wells is increased every year, the casing damage trend is continuously worsened, and the serious threat is brought to the normal production of the oil field. Therefore, 4-inch semi-joint-free casing sticking plugging is carried out in a 5-inch semi-casing to realize reconstruction of a shaft, and the technical principle is that chemical plugging of microcrystalline minerals and a casing reinforcing technology are organically combined. The plugging pipe is put to a preset position, plugging agent is injected into the annular space of the sleeve and the plugging pipe and the stratum under high pressure, and a double-layer plugging barrier of the plugging agent and the plugging pipe is constructed, so that plugging and reinforcement of a blocking layer and a leakage section of the sleeve are achieved.
Under the condition that corrosion products such as iron scale exist on the inner wall of the old well casing, the conventional common cement well cementing fluid cannot form firm interface cementation with the old well casing due to high system density, system shrinkage, high water absorption rate under low density conditions and the like, so that the plugging fails under the action of injection and production pressure, and the plugging validity period is shortened. The requirement of narrow-gap annular short well section (less than 450m) well cementation cannot be met.
In the process of plugging the ground pipeline, a forward injection process is adopted, and no external leakage environment exists, so that the requirements on flow rate and circulating pressure are relatively low. Different from the plugging of a ground pipeline, the plugging method has the advantages that the distance between the outer annular space of the underground 5-inch half casing and the outer annular space of the 4-inch half casing which are attached and plugged is only 10mm, the annular space volume is small, the annular space return speed of a slim hole is large by adopting a circular upward return annular space construction process, the well cementation circulating pressure is high, and if the discharge capacity is unreasonable to control, a beancurd jelly phenomenon is easily formed, so that the formation is suppressed and leaked or an annular space well cementation accident is formed.
Therefore, a low-density, low-water-absorption and high-strength well cementing plugging agent needs to be researched. The apparent viscosity of the blocking agent is required to be less than 50mPa.s, the water precipitation rate is required to be less than 2%, and the bonding strength (50 ℃) between the blocking agent and the sleeve is required to be more than 25 MPa.
Disclosure of Invention
The invention provides a cementing plugging agent for well cementation and a preparation method thereof, wherein the cementing plugging agent can realize smooth circulation in a narrow-gap annular short well section, and can form a compact, impermeable, thin-wall and reticular cement cake at a sleeve broken section and a crack inlet.
The technical scheme provided by the invention is as follows:
the patch plugging agent comprises the following components in parts by weight: 46-50 parts of superfine cement; 41-46 parts of mineral powder; 1-3 parts of superfine silica fume; 1-3 parts of sepiolite powder; 0.2-0.8 of magnetic high molecular polymer; 3-5 parts of a swelling agent; 1-2 parts of aminophosphonic acid chelating resin; 0.2 to 0.5 of drag reduction retarder.
Preferably, the composition comprises the following components in parts by weight: 48 parts of superfine cement, 43 parts of mineral powder, 2 parts of superfine silica fume, 2 parts of sepiolite powder, 0.5 part of magnetic high polymer, 4 parts of expanding agent and 4.5 parts of aminophosphonic acid chelating resin; 0.3 of drag reduction retarder.
Preferably, the average particle size of the superfine silica fume is 0.1-0.15 mu m, and the specific surface area is 15-27 m 2 /g。
Preferably, the swelling agent is a lattice type swelling agent.
Preferably, the method for preparing the magnetic high molecular polymer comprises the following steps,
1) preparing iron oxide magnetic nanoparticles: 300mL of deionized water was added to the flask, nitrogen was introduced to the flask for nitrogen protection, and 3g of FeCl was added 3 And FeCl 2 In which FeCl 3 And FeCl 2 The molar ratio of the iron oxide to the water is 2:1, when the temperature is raised to 50 ℃, 30ml of ammonia water with the concentration of 25-30% is quickly dripped, after the ammonia water is dripped, the temperature is kept at 50 ℃, the reaction is carried out for 4.5 hours, the temperature is reduced to room temperature, the mixture is poured into a beaker, washed by deionized water and separated by a magnet, and finally, the iron oxide magnetic nanoparticles which are washed clean are obtained;
2) preparation of KH570 modified magnetic nanoparticles: adding 300mL of deionized water and 150mL of ethanol into a flask, introducing nitrogen, carrying out nitrogen protection, adding 2g of iron oxide magnetic nanoparticles, heating to 50 ℃, adding 25mL of 25-30% ammonia water, slowly adding 6mL of silane coupling agent KH570 dropwise, after dropwise addition, keeping the temperature at 50 ℃, reacting for 4 hours, cooling to room temperature, washing with deionized water, and separating with a magnet to obtain modified magnetic nanoparticles;
3) synthesis of magnetic high molecular polymer: respectively adding 150mL of deionized water, 2.5g of modified magnetic nanoparticles, 0.64g of acrylamide, 0.03g of N, N-methylene bisacrylamide, 1.2g of polyvinylpyrrolidone and 0.96g of acrylic acid with a neutralization degree of 70% into a flask, uniformly stirring, finally slowly and uniformly dropwise adding 0.8g of ammonium persulfate-sodium bisulfite initiator into the reaction system, continuously stirring after all materials are added, pouring out polymer gel after a polymerization reaction lasts for 3-5 hours, soaking the polymer gel in absolute ethyl alcohol for 24 hours, removing unreacted substances and other soluble substances, then placing the polymer gel in an oven at 80 ℃ for drying for 5-6 hours, and crushing to obtain the magnetic high molecular polymer.
Preferably, 0.8g of ammonium persulfate-sodium bisulfite initiator is prepared as a 10% solution by mass and then slowly added dropwise to the reaction system.
Preferably, the synthesis method of the aminophosphonic acid chelating resin comprises the following steps:
1) synthesis of cross-linked polyacrylamide: adding 40g of acrylamide and 0.75g of N, N '-methylene-bisacrylamide into a flask respectively, stirring until the acrylamide and the N, N' -methylene-bisacrylamide are dissolved completely, introducing nitrogen to remove air, heating to 50 ℃, and simultaneously respectively dropwise adding a solvent containing 0.15g of K 2 S 2 0 8 And 0.15g KHS0 3 The aqueous solution is kept at 50 ℃ for reaction under the protection of nitrogen, when gel is generated, the reaction is stopped, the generated gel is sequentially washed by water and methanol, dried in a vacuum drying oven at 70 ℃, and ground and sieved after drying, so that white powdery crosslinked polyacrylamide is obtained;
2) synthesis of amino phosphonic acid chelating resin: weighing 1.42g of cross-linked polyacrylamide, swelling the cross-linked polyacrylamide with distilled water at room temperature for 12h, adjusting the pH value of the solution to ll with Na0H solution, adding 0.6g of paraformaldehyde dry powder, mixing and stirring uniformly, carrying out hydroxymethylation reaction on the cross-linked polyacrylamide and paraformaldehyde at 25 ℃, maintaining the temperature for reaction for 3h, adding phosphorous acid into a reaction system, wherein the molar ratio of the phosphorous acid to the paraformaldehyde is 1.4:1, raising the temperature to 90 ℃, carrying out reflux stirring reaction for 8h, washing the product to be neutral after the reaction is finished, washing the product with 1mol/L NaOH solution for a plurality of times, washing the product with water again to be neutral, washing the product with 1mol/L hydrochloric acid for a plurality of times to be converted to a hydrogen type, washing the product again to be neutral, finally washing with methanol for 3-4 times, and drying in vacuum to be constant weight to obtain the aminophosphonic acid chelating resin.
Preferably, the drag reduction retarder is composed of polyacrylamide drag reduction agent and sodium lignosulfonate retarder according to the weight part ratio of 1: 1.
Preferably, the superfine cement is superfine G-grade cement, the median particle size is 9.2 mu m, and the specific surface area is 6540m 2 /g。
The invention also provides a preparation method of the patch plugging agent,
step one, adding the superfine cement, the mineral powder, the superfine silica fume and the sepiolite powder in a container according to the specified weight parts, and uniformly stirring;
and step two, adding the swelling agent, the magnetic high-molecular polymer, the aminophosphonic acid chelating resin and the drag reduction retarder in specified parts by weight into a container, and uniformly stirring to obtain a finished product of the blocking agent.
In the drilling process, in order to prevent formation fluid from entering the well, the pressure of the drilling fluid column is generally controlled to be higher than the formation pressure, and free water in the drilling fluid permeates into rock cracks or gaps of the well wall under the action of the pressure difference between the drilling fluid column and the formation pressure, which is called the filtration action of the drilling fluid. During the filtration process some of the solid particles in the drilling fluid adhere to the walls of the wellbore, forming a mud cake. The process of forming mud cake by attaching solid particles on the well wall is called the wall building property of the drilling fluid. The formation of mud cake on the well wall can prevent or slow down the continuous invasion of free water in the drilling fluid into the stratum.
The invention relates to the development of a plugging agent formula system, which adopts the concept of drilling fluid wall building, and quickly forms compact, impermeable, thin-walled and reticular cement cakes in a near-wellbore area, a defect wall, a large pore path and a crack inlet. After the bridging is formed by the large-size material, the small-size material is embedded and blocked on the small pore channel formed by the bridging material. By means of the elasticity and plasticity of the active material, powerful lacing and reticulation effect is produced to form firm plug cushion layer with difficult movement and to reach the aim of blocking.
The narrow-gap annular short well section well cementation requires that the well cementation plugging agent has good pumping performance and superior water loss reduction performance, and the slurry prepared by the well cementation plugging agent has relatively low viscosity and the water release rate of less than 2 percent.
The magnetic high molecular polymer in the formula is generated by reaction of acrylic acid, acrylamide, N-methylene-bisacrylamide, polyvinylpyrrolidone, iron oxide and the like, and a chemical linking group is introduced to support a molecular bridge between interfaces of inorganic substances and organic substances, so that a polymer system with weak magnetism on the surface is formed. The magnetic high molecular polymer contains COO - So that the surface thereof is negatively charged, and iron oxide (Fe) 2 O 3 Or Fe 3 O 4 ) Under the acidic condition, the surface of the copolymer emulsion is positively charged, and iron oxide ions of the copolymer emulsion are coated on the surface of the copolymer emulsion due to the attraction of the charges and the mutual operation of chemical bonds, so that a weakly magnetic polymer system is formed by polymerization.
Through tests, the water absorption of the well cementation plugging agent is obviously improved by adding the weak magnetic polymer, and the apparent viscosity is reduced along with the increase of the adding amount. Probably due to the addition of iron oxides, especially Fe 2 O 3 The intermolecular force is reduced, the relative slippage between molecular chains is facilitated, and the fluidity is improved. Therefore, the addition of the magnetic high molecular polymer can improve the flow property of the well cementing plugging agent.
The amino phosphonic acid chelating resin in the formula is synthesized by taking acrylamide as a skeleton and performing hydroxymethylation and phosphorylation on cross-linked polyacrylamide, and the chelating functional group is NHCH2PO (OH)2 or-N [ CH2PO (OH)2] 2 . The resin can selectively chelate certain metal ions through ionic bonds and coordinate bonds, can form relatively stable chelate with a plurality of metal ions, and has the adsorption capacity superior to that of high-valence metal ions such as Fe, Cu and the like attached to the inner wall of an old sleeve.
The sepiolite powder in the formula system belongs to fibrous clay minerals, and the main chemical compositions of the sepiolite powder are silicon (Si) and magnesium (Mg), and the chemical formula is Mg 8 Si 12 O 30 (OH) 4 (OH 2 ) 4 ·8H 2 O; chemical formula is shown as 8H 2 O' represents adsorbed water, and sepiolite powder is adsorbed on the surface of the mineral and occupies part of the central channel; (OH) 2 ) 4 Represents crystal water combined with octahedral layer magnesium ions; (OH) 4 Which represents structural water, is usually present in the form of hydroxyl groups. The sepiolite powder has the theoretical specific surface area of up to 900m by the unique water adsorption channel and the large holes contained in the fiber bundle 2 And/g, more water and polar substances can be adsorbed in the channels and the holes.
Sepiolite powder and mineral powder in the formula system can be bridged to form a net, so that the consistency of slurry is increased, and the pumping and displacement efficiency of the slurry is influenced, therefore, the flow property of cement slurry is improved by adding the drag reduction retarder, and the plugging agent can meet the flow state designed by extrusion and displacement. The anti-drag slow-setting components are sodium lignosulphonate and acrylamide, sodium lignosulphonate molecule active groups are adsorbed on the surfaces of cement particles, the Z potential on the surfaces of the cement particles is improved, the anti-drag purpose is achieved by electrostatic repulsion, and meanwhile, the steric hindrance caused by the adsorption of acrylamide molecules on the surfaces of the cement particles realizes the dispersion effect, and the combined action of the sodium lignosulphonate molecule active groups and the acrylamide molecules forms slurry which is plastic and rheological.
The expanding agent in the formula system is a lattice type expanding agent, such as magnesium oxide and the like, expands in the later stage of the plastic state and the early stage of hardening of the slurry, and can ensure the continuity of the expansion of the drilling fluid slurry from the plastic state to the early stage of hardening, namely, the double expansion effect is achieved.
The average grain size of the superfine silica fume is 0.1-0.15 mu m, is one percent of the average grain size of the common cement, and the specific surface area of the superfine silica fume is 15-27 m 2 The polymer has strong surface activity and can be chemically combined with organic functional groups; meanwhile, the silicon-oxygen bond also contains silicon alcohol which is easy to hydrolyze into silanol and reacts with oxide or hydroxyl on the surface of an inorganic substance to generate a stable silicon-oxygen bond. In addition, the interface performance of different materials can be improved, and bridging can be realizedEmbedment and plugging in the structure of the netting.
Drawings
FIG. 1 is a microscopic photograph of the patch of example 1;
Detailed Description
The present invention is further illustrated by the following specific examples, which are, however, merely exemplary and are not to be construed as limiting the invention.
In the following examples, the ultrafine silica fume has an average particle diameter of 0.1 to 0.15 μm and a specific surface area of 15 to 27m 2 (iv) g. The swelling agent is lattice type swelling agent, and is specifically selected from magnesium oxide. The drag reduction retarder is composed of polyacrylamide drag reduction agent and sodium lignosulfonate retarder according to the weight ratio of 1: 1.
The mineral powder is a by-product produced during smelting pig iron in a blast furnace, and mainly comprises magnesium oxide, silicon dioxide, aluminum oxide, small amount of compounds such as calcium oxide and ferric oxide, wherein the median of particle size is 7.8 μm, and the specific surface area is 7660m 2 /g。
To verify the beneficial effects of the examples, the ultra-fine cement was an ultra-fine G-grade cement with a median particle size of 9.2 μm and a specific surface area of 6540m 2 /g。
The preparation method of the magnetic high molecular polymer comprises the following steps,
1) preparing iron oxide magnetic nanoparticles: 300mL of deionized water is added into a flask with a condenser tube, an air duct, a thermometer, a dropping funnel and a magnetic stirrer, nitrogen is introduced for nitrogen protection, and 3g of FeCl is added 3 And FeCl 2 In which FeCl 3 And FeCl 2 The molar ratio of the iron oxide to the water is 2:1, 30ml of ammonia water with the concentration of 28% is quickly dripped when the temperature is raised to 50 ℃, the temperature is kept at 50 ℃ after the ammonia water is dripped, the reaction is carried out for 4.5 hours, the temperature is reduced to room temperature, the mixture is poured into a beaker, washed by deionized water and separated by a magnet, and finally, the iron oxide magnetic nanoparticles which are washed clean are obtained;
2) preparation of KH570 modified magnetic nanoparticles: adding 300mL of deionized water and 150mL of ethanol into a flask, introducing nitrogen, adding 2g of iron oxide magnetic nanoparticles after nitrogen protection, heating to 50 ℃, adding 25mL of ammonia water with the mass concentration of 28%, slowly dropwise adding 6mL of silane coupling agent KH570, keeping the temperature at 50 ℃ after dropwise adding, reacting for 4h, cooling to room temperature, washing for 5 times with deionized water, and separating with a magnet to obtain modified magnetic nanoparticles;
3) synthesis of magnetic high molecular polymer: 150mL of deionized water, 2.5g of modified magnetic nanoparticles, 0.64g of acrylamide, 0.03g of N, N-methylene bisacrylamide, 1.2g of polyvinylpyrrolidone and 0.96g of acrylic acid with a neutralization degree of 70% are respectively added into a flask, the mixture is uniformly stirred, finally 0.8g of ammonium persulfate-sodium bisulfite initiator is slowly and uniformly dripped into the reaction system, after all the materials are added, the mixture is continuously stirred, the polymer gel is poured out after 4 hours of polymerization reaction, anhydrous ethanol is placed into the polymer gel for soaking for 24 hours to remove unreacted substances and other soluble substances, then the polymer is placed into an oven at 80 ℃ for drying for 6 hours and crushed to obtain the magnetic high molecular polymer.
0.8g of ammonium persulfate-sodium bisulfite initiator is prepared into a solution with the mass percentage of 10 percent, and then the solution is slowly dripped into the reaction system.
The synthesis method of the aminophosphonic acid chelating resin comprises the following steps:
1) synthesis of cross-linked polyacrylamide: adding acrylamide 40g and N, N' -methylene bisacrylamide 0.75g into water phase, stirring to dissolve completely, introducing nitrogen gas for about 20min to remove air, heating to 50 deg.C, and adding dropwise a solution containing K0.15 g 2 S 2 0 8 And 0.15g KHS0 3 The aqueous solution is kept at 50 ℃ for reaction under the protection of nitrogen, when gel is generated, the reaction is stopped, the generated gel is sequentially washed by water and methanol, dried in a vacuum drying oven at 70 ℃, and ground and sieved after drying, so that white powdery crosslinked polyacrylamide is obtained;
2) synthesis of amino phosphonic acid chelating resin: weighing 1.42g of cross-linked polyacrylamide, swelling the cross-linked polyacrylamide with distilled water at room temperature for 12 hours, adjusting the pH value of the solution to ll with Na0H solution, adding 0.6g of paraformaldehyde dry powder, mixing and stirring uniformly, carrying out hydroxymethylation reaction on the cross-linked polyacrylamide and paraformaldehyde at 25 ℃, maintaining the temperature for reaction for 3 hours, adding phosphorous acid into a reaction system, wherein the molar ratio of the phosphorous acid to the paraformaldehyde is 1.4:1, raising the temperature to 90 ℃, carrying out reflux stirring reaction for 8 hours, washing the product to be neutral after the reaction is finished, washing the product with 1mol/L NaOH solution for a plurality of times, washing the product with water again to be neutral, washing the product with 1mol/L hydrochloric acid for a plurality of times to be converted to a hydrogen type, washing the product again to be neutral, finally washing with methanol for 4 times, and carrying out vacuum drying to be constant weight to obtain the aminophosphonic acid chelating resin.
Example 1
The patch plugging agent comprises the following components in parts by weight:
ultra-fine cement 46; 41 parts of mineral powder; 1, superfine silica fume; 1 part of sepiolite powder; 0.2 parts of magnetic high molecular polymer; a swelling agent 3; aminophosphonic acid chelate resin 1; 0.2 of drag reduction retarder.
The preparation method of the adhesive comprises the following steps:
step one, adding the superfine cement, the mineral powder, the superfine silica fume and the sepiolite powder in a container according to the specified weight parts, and uniformly stirring;
and step two, adding the expanding agent, the magnetic high-molecular polymer, the amino phosphonic acid chelating resin and the drag reduction retarder in the specified weight parts into a container, and uniformly stirring to obtain a finished product of the well cementation plugging agent.
Example 2
The adhesive blocking agent comprises the following components in parts by weight:
48 parts of superfine cement; 43 parts of mineral powder; 2, superfine silica fume; sepiolite powder 2; 0.5 parts of magnetic high molecular polymer; a swelling agent 4; 1.5 of aminophosphonic acid chelating resin; 0.3 of drag reduction retarder.
The preparation method of the adhesive comprises the following steps:
step one, adding the superfine cement, the mineral powder, the superfine silica fume and the sepiolite powder in a container according to the specified weight parts, and uniformly stirring;
and step two, adding the expanding agent, the magnetic high-molecular polymer, the amino phosphonic acid chelating resin and the drag reduction retarder in the specified weight parts into a container, and uniformly stirring to obtain a finished product of the well cementation plugging agent.
Example 3
The patch plugging agent comprises the following components in parts by weight:
50 parts of superfine cement; 46 of mineral powder; 3, superfine silica fume; sepiolite powder 3; 0.8 parts of magnetic high molecular polymer; a swelling agent 5; aminophosphonic acid chelating resin 2; 0.5 of drag reduction retarder.
The preparation method of the adhesive comprises the following steps:
step one, adding the specified parts by weight of superfine cement, mineral powder, superfine silica fume and sepiolite powder into a container and uniformly stirring;
and step two, adding the swelling agent, the magnetic high-molecular polymer, the aminophosphonic acid chelating resin and the drag reduction retarder in specified parts by weight into a container, and uniformly stirring to obtain a finished product of the well cementing and plugging agent.
Comparative example 1
The adhesive blocking agent comprises the following components in parts by weight:
50 parts of superfine cement; 46 of mineral powder; 3, superfine silica fume; sepiolite powder 3; an expanding agent 5; aminophosphonic acid chelating resin 2; 0.5 of drag reduction retarder.
The preparation method of the adhesive comprises the following steps:
step one, adding the specified parts by weight of superfine cement, mineral powder, superfine silica fume and sepiolite powder into a container and uniformly stirring;
and step two, adding the expanding agent, the aminophosphonic acid chelating resin and the resistance-reducing retarder in the specified weight parts into a container, and uniformly stirring to obtain the well cementing plugging agent finished product.
Comparative example 2
The adhesive blocking agent comprises the following components in parts by weight:
50 parts of superfine cement; 46 of mineral powder; 3, superfine silica fume; sepiolite powder 3; 0.8 parts of magnetic high molecular polymer; a swelling agent 5; 0.5 of drag reduction retarder.
The preparation method of the adhesive comprises the following steps:
step one, adding the superfine cement, the mineral powder, the superfine silica fume and the sepiolite powder in a container according to the specified weight parts, and uniformly stirring;
and step two, adding the expanding agent, the magnetic high-molecular polymer and the resistance-reducing retarder in the specified weight parts into a container, and uniformly stirring to obtain the well cementing plugging agent finished product.
And during slurry viscosity measurement, 560 g of the prepared plugging agent is weighed, 350 g of water is added, after stirring for 10 minutes, the prepared plugging agent passes through a sieve with 16 holes per inch, the time for the slurry to flow out of 500ml is measured by adopting a 1006 type slurry viscometer, and the viscosity value is reflected.
Water separation rate for 2 hours: weighing 165g (accurate to 0.1g) of sample in a 250mL beaker, adding 100mL of water, stirring until the sample is completely dispersed in the water to form suspension slurry, stirring for 20min by using a stirrer to prepare slurry, adding the slurry into a 500mL measuring cylinder, standing for 2h, and observing the water evolution amount.
The water separation rate is calculated according to the formula (1).
Figure BDA0003611416010000121
In the formula:
s-water precipitation rate,%;
v 1-water evolution in milliliters (mL);
v 0-Total amount of suspension slurry in milliliters (mL).
The test results are shown in table 1 below.
Serial number Viscosity mPa.s Precipitation amount (ml) Volume of slurry (ml) Water analysis rate (%)
Example 1 42 1.9 152 1.25
Example 2 41 1.8 153 1.18
Example 3 41 1.5 153 0.98
Comparative example 1 48 4.6 154 2.98
Comparative example 2 49 3.7 154 2.40
The examples and comparative examples were also subjected to the compression strength test, and the results are shown in Table 2.
Figure BDA0003611416010000131
From the above test data, it is found that the water absorption capacity is further improved by adding the magnetic high molecular polymer. The aminophosphonic acid chelating resin obtained by the invention is cation chelating resin, and N atoms and O atoms in resin chelating groups form coordination bonds with high-valence metal ions, so that the adsorption capacity on the metal surface or the scaling surface on the inner wall of the sleeve is ensured.
The addition of the aminophosphonic acid chelating resin can greatly improve the flexural strength and the plastic modulus under similar strength indexes. The yield deformation characteristic of the aminophosphonic acid chelating resin results from the resistance of a single shear band to propagate and the induction of multiple shear bands at the location of the resistance, the shear band generation and propagation processes being discontinuous. Therefore, the patch material breaks with a pronounced veining character. The interface between the plugging agent and the inner wall of the casing still keeps a better state when being damaged, which shows that the plugging agent and the inner wall of the casing have good binding capacity.
The applicant adopts the technical scheme of the embodiment 3 to carry out field practical application.
Washing the well with clean water in a positive circulation mode; the plugging agent is mixed according to the proportion of 1.70-1.75g/cm 3 Adding into clear water to prepare mortar with a thickness of 4m 3 The initial setting time is required to be not less than 200 min. The casing gate is opened, and mortar is replaced by 4.0m 3 Just replace 5.2m of clear water 3 Closing an internal plug valve or closing a gate on a hose connected with an oil pipe, opening a blowout preventer, lowering all loads of a pipe column, pressurizing and seating the pipe column on a sand surface, lifting the pipe column load to a neutral point at a positive and negative joint, removing the weight of a sticking pipe, rotating forward for 20-30 circles and reversely buckling, and lifting the pipe column for 2-3m after success; closing the blowout preventer; the water displacement from the casing is controlled to be 3.3m 3 The content of the compound is less than the content of the compound; slowly opening a hose gate to release pressure, washing the well with clear water at a large discharge capacity, and washing out excessive mortar in the well; closing the well and waiting for setting for 48 hours, drilling a plug and flushing sand to the bottom of the artificial well. And pumping by a lower pump.
The total time of implementing 12 wells, completing 12 wells, and uniformly testing the pressure after plugging to be qualified at 15 MPa. The oil increasing effect is 12 wells, the effective rate is 100%, the daily oil increasing level is 19.8 tons, the average daily increase of a single well is 1.65 tons, the average effective period is 154 days, the cumulative oil increasing is 2415.48 tons, the average single well oil increasing is 219.6 tons, and the average productivity recovery rate is 119.37%.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.

Claims (10)

1. The patch plugging agent is characterized by comprising the following components in parts by weight:
46-50 parts of superfine cement; 41-46 parts of mineral powder; 1-3 parts of superfine silica fume; 1-3 parts of sepiolite powder; 0.2-0.8 of magnetic high molecular polymer; 3-5 parts of a swelling agent; 1-2 parts of aminophosphonic acid chelating resin; 0.2 to 0.5 of drag reduction retarder.
2. The patch according to claim 1, characterized by comprising the following components in parts by weight: 48 parts of superfine cement, 43 parts of mineral powder, 2 parts of superfine silica fume, 2 parts of sepiolite powder, 0.5 part of magnetic high polymer, 4 parts of expanding agent and 4.5 parts of aminophosphonic acid chelating resin; 0.3 of drag reduction retarder.
3. The patch according to claim 1 or 2, wherein the ultrafine silica fume has an average particle size of 0.1 to 0.15 μm and a specific surface area of 15 to 27m 2 /g。
4. The patch according to claim 1 or 2, characterized in that the swelling agent is a lattice type swelling agent.
5. The patch according to claim 1 or 2,
the preparation method of the magnetic high molecular polymer comprises the following steps,
1) preparing iron oxide magnetic nanoparticles: 300mL of deionized water was added to the flask, nitrogen was introduced to the flask for nitrogen protection, and 3g of FeCl was added 3 And FeCl 2 In which FeCl 3 And FeCl 2 The molar ratio of the ammonia water to the ammonia water is 2:1, 30ml of ammonia water with the concentration of 25-30% is quickly dripped when the temperature is raised to 50 ℃, the temperature is kept at 50 ℃ after the ammonia water is dripped, the temperature is reduced to the room temperature after the reaction is carried out for 4.5h, and the mixture is pouredWashing in a beaker by using deionized water, and separating by using a magnet to finally obtain the cleaned iron oxide magnetic nanoparticles;
2) preparation of KH570 modified magnetic nanoparticles: adding 300mL of deionized water and 150mL of ethanol into a flask, introducing nitrogen, adding 2g of iron oxide magnetic nanoparticles after nitrogen protection, heating to 50 ℃, adding 25mL of ammonia water with the mass concentration of 25-30%, slowly dropwise adding 6mL of silane coupling agent KH570, keeping the temperature at 50 ℃ after dropwise adding, reacting for 4 hours, cooling to room temperature, washing with deionized water, and separating with a magnet to obtain modified magnetic nanoparticles;
3) synthesis of magnetic high molecular polymer: adding 150mL of deionized water, 2.5g of modified magnetic nanoparticles, 0.64g of acrylamide, 0.03g of N, N-methylene bisacrylamide, 1.2g of polyvinylpyrrolidone and 0.96g of acrylic acid with a neutralization degree of 70% into a flask respectively, uniformly stirring, finally slowly and uniformly dripping 0.8g of ammonium persulfate-sodium bisulfite initiator into the reaction system, continuously stirring after all materials are added, pouring out polymer gel after a polymerization reaction is carried out for 3-5 h, soaking the polymer gel in absolute ethyl alcohol for 24 h, removing unreacted substances and other soluble substances, then placing the polymer gel in an oven at 80 ℃ for drying for 5-6 h, and crushing to obtain the magnetic high molecular polymer.
6. The patch according to claim 5,
0.8g of ammonium persulfate-sodium bisulfite initiator is prepared into a solution with the mass percentage of 10 percent, and then the solution is slowly dripped into the reaction system.
7. The patch according to claim 1 or 2,
the synthesis method of the aminophosphonic acid chelating resin comprises the following steps:
1) synthesis of cross-linked polyacrylamide: adding acrylamide 40g and N, N' -methylene-bisacrylamide 0.75g into water phase, stirring to dissolve completely, introducing nitrogen to remove air, heating to 50 deg.C, and adding dropwiseHas a K of 0.15gK 2 S 2 0 8 And 0.15g KHS0 3 The aqueous solution is kept at 50 ℃ for reaction under the protection of nitrogen, when gel is generated, the reaction is stopped, the generated gel is sequentially washed by water and methanol, dried in a vacuum drying oven at 70 ℃, and ground and sieved after drying, so that white powdery crosslinked polyacrylamide is obtained;
2) synthesis of amino phosphonic acid chelate resin: weighing 1.42g of cross-linked polyacrylamide, swelling the cross-linked polyacrylamide with distilled water at room temperature for 12h, adjusting the pH value of the solution to ll with Na0H solution, adding 0.6g of paraformaldehyde dry powder, mixing and stirring uniformly, carrying out hydroxymethylation reaction on the cross-linked polyacrylamide and paraformaldehyde at 25 ℃, maintaining the temperature for reaction for 3h, adding phosphorous acid into a reaction system, wherein the molar ratio of the phosphorous acid to the paraformaldehyde is 1.4:1, raising the temperature to 90 ℃, carrying out reflux stirring reaction for 8h, washing the product to be neutral after the reaction is finished, washing the product with 1mol/L NaOH solution for a plurality of times, washing the product with water again to be neutral, washing the product with 1mol/L hydrochloric acid for a plurality of times to be converted to a hydrogen type, washing the product again to be neutral, finally washing with methanol for 3-4 times, and drying in vacuum to be constant weight to obtain the aminophosphonic acid chelating resin.
8. The patch of claim 1 or 2, wherein the drag reduction retarder is composed of polyacrylamide drag reducer and sodium lignosulfonate retarder in a weight ratio of 1: 1.
9. The method for preparing the patch according to claim 1 or 2, wherein the ultra-fine cement is ultra-fine G-grade cement, the median particle size is 9.2 μm, and the specific surface area is 6540m 2 /g。
10. The method for producing a patch according to claim 1 or 2,
step one, adding the specified parts by weight of superfine cement, mineral powder, superfine silica fume and sepiolite powder into a container and uniformly stirring;
and step two, adding the expanding agent, the magnetic high-molecular polymer, the amino phosphonic acid chelating resin and the drag reduction retarder in the specified weight parts into a container, and uniformly stirring to obtain a finished product of the blocking agent.
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CN117534380A (en) * 2023-11-15 2024-02-09 万特福建筑构件有限公司 Wet-mixed mortar and preparation method thereof

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EP1283939A1 (en) * 2000-05-22 2003-02-19 Shell Internationale Researchmaatschappij B.V. Method for plugging a well with a resin
CN102485830A (en) * 2010-12-02 2012-06-06 北京化工大学 Profile control oil-displacement agent for core-shell type inorganic/organic polymer composite microballoon
CN102587858A (en) * 2012-03-09 2012-07-18 中国石油化工股份有限公司 Method for blocking water for fracture and hole type reservoir
CN103045214A (en) * 2013-01-16 2013-04-17 西南石油大学 Plugging thixotropic cement paste for oil-gas well and preparation method for same

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EP1283939A1 (en) * 2000-05-22 2003-02-19 Shell Internationale Researchmaatschappij B.V. Method for plugging a well with a resin
CN102485830A (en) * 2010-12-02 2012-06-06 北京化工大学 Profile control oil-displacement agent for core-shell type inorganic/organic polymer composite microballoon
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CN117534380A (en) * 2023-11-15 2024-02-09 万特福建筑构件有限公司 Wet-mixed mortar and preparation method thereof
CN117534380B (en) * 2023-11-15 2024-05-28 万特福建筑构件有限公司 Wet-mixed mortar and preparation method thereof

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