CN115093164B - Adhesive agent and its preparation method - Google Patents

Adhesive agent and its preparation method Download PDF

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CN115093164B
CN115093164B CN202210431623.9A CN202210431623A CN115093164B CN 115093164 B CN115093164 B CN 115093164B CN 202210431623 A CN202210431623 A CN 202210431623A CN 115093164 B CN115093164 B CN 115093164B
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parts
agent
water
cement
reaction
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CN115093164A (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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    • C04B18/04—Waste materials; Refuse
    • C04B18/14—Waste materials; Refuse from metallurgical processes
    • C04B18/146—Silica fume
    • C—CHEMISTRY; METALLURGY
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    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
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    • C04B22/06—Oxides, Hydroxides
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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
    • C04B24/12—Nitrogen containing compounds organic derivatives of hydrazine
    • 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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    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • 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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    • C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
    • C09K8/42—Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells
    • C09K8/46—Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells containing inorganic binders, e.g. Portland cement
    • C09K8/467—Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells containing inorganic binders, e.g. Portland cement containing additives for specific purposes
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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 comprises the following components in parts by weight: 46-50 parts of superfine cement; 41-46 of mineral powder; 1-3 parts of superfine silica fume; sepiolite powder 1-3; 0.2 to 0.8 percent of magnetic high molecular polymer; 3-5 parts of an expanding agent; 1-2 parts of amino phosphonic acid chelate resin; 0.2 to 0.5 of drag reducing 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 the sleeve breaking section and the crack inlet.

Description

Adhesive agent and its preparation method
Technical Field
The invention relates to the technical field of oil field operation well repair, in particular to a well cementation plugging agent for treating casing leakage and a preparation method thereof.
Background
Along with the extension of the development time of the oil field, due to the factors of plastic flow, ground stress, mineralization degree and the like of a salt bearing layer, and the implementation of severe corrosion and frequent fracturing and acidification measures of produced water, the service life of the oil layer casing is too long, and the phenomena of perforation, casing deformation, breakage and the like occur in the free section and the sealing section of the casing due to corrosion, so that the water and leakage of the stratum are caused, the normal production of an oil well is seriously influenced, and even the normal production cannot be carried out and the oil layer casing is scrapped. The well is an ineffective water injection. The number of newly increased casing damage wells is increased every year, the casing damage trend is continuously worsened, and serious threat is brought to normal production of the oil field. Therefore, 4 inch semi-coupling-free casing plugging is carried out in 5 inch semi-casing to realize shaft reconstruction, and the technical principle is that the microcrystalline mineral chemical plugging and casing reinforcing technology are organically combined. And (3) placing the plugging pipe at a preset position, injecting a plugging agent into the annular space and stratum of the sleeve and the plugging pipe at high pressure, and constructing a double-layer plugging barrier of the plugging agent and the plugging pipe to realize plugging and reinforcing of a plugging layer and a sleeve leakage section.
Under the condition that corrosion products such as iron scale exist on the inner wall of the old well casing, the conventional cement well cementation fluid cannot form firm interface cementation with the old well casing due to high system density, system shrinkage, higher water absorption rate under low density conditions and the like, so that plugging is invalid under the action of injection and production pressure, and the plugging effective period is shortened. The requirement of cementing a short well section (less than 450 m) of a narrow-gap annular space cannot be met.
In the ground pipeline plugging, a positive injection process is adopted, and no environment is lost outside the pipeline, so that the requirements on flow velocity and circulating pressure are relatively low. Different from the ground pipeline plugging, the plugging is carried out on the outer annular space of the underground 5-inch half casing pipe and the 4-inch half casing pipe, the interval between the plugging and the plugging is only 10mm, the annular space is smaller, the circulating upward annular space construction process is adopted, the annular space return speed of a small well hole is larger, the well cementation circulating pressure is higher, if the displacement control is unreasonable, the phenomenon of uncongealed beancurd is easily formed, and the leaking blocking stratum or the annular well cementation accident is caused.
Therefore, a low-density, low-water-absorption and high-strength well cementing plugging agent needs to be studied. The apparent viscosity of the patch is required to be less than 50mPa.s, the water separation rate is required to be less than 2%, and the cementing strength (50 ℃) with the sleeve is required to be more than 25MPa.
Disclosure of Invention
The invention provides a plugging agent for well cementation and a preparation method thereof, and the plugging agent for well cementation can realize smooth circulation in a short well section of a narrow-gap annular space, and can form compact, impermeable, thin-wall and net-shaped 'cement cakes' at a sleeve breaking section and a crack inlet.
The technical scheme provided by the invention is as follows:
the patch comprises the following components in parts by weight: 46-50 parts of superfine cement; 41-46 of mineral powder; 1-3 parts of superfine silica fume; sepiolite powder 1-3; 0.2 to 0.8 percent of magnetic high molecular polymer; 3-5 parts of an expanding agent; 1-2 parts of amino phosphonic acid chelate resin; 0.2 to 0.5 of drag reducing 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 amino phosphonic acid chelating resin; and 0.3 of drag reducing retarder.
Preferably, the average grain diameter 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 expanding agent is a lattice type expanding agent.
Preferably, the preparation method of the magnetic high molecular polymer comprises the following steps,
1) Preparation of iron oxide magnetic nanoparticles: 300mL of deionized water was added to the flask, nitrogen was purged, and 3g of FeCl was added after nitrogen protection 3 And FeCl 2 Wherein FeCl 3 And FeCl 2 The molar ratio of (2) to (1) is 2:1, 30ml of ammonia water with the concentration of 25-30% is quickly dripped when the temperature is raised to 50 ℃, after the ammonia water is dripped, the temperature is kept at 50 ℃, the reaction time is 4.5 hours, the reaction time is reduced to room temperature, the reaction time is poured into a beaker, deionized water is used for washing, and magnet separation is carried out, so that the washed iron oxide magnetic nano particles are finally obtained;
2) Preparation of KH570 modified magnetic nanoparticles: adding 300mL of deionized water and 150mL of ethanol into a flask, introducing nitrogen, performing nitrogen protection, adding 2g of iron oxide magnetic nanoparticles, heating to 50 ℃, adding 25mL of ammonia water with mass concentration of 25-30%, slowly dropwise adding 6mL of silane coupling agent KH570, after dropwise adding, preserving heat 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: 150mL of deionized water, 2.5g of modified magnetic nano particles, 0.64g of acrylamide, 0.03g of N, N-methylene bisacrylamide, 1.2g of polyvinylpyrrolidone and 0.96g of acrylic acid with the neutralization degree of 70% are respectively added into a flask, uniformly stirred, finally 0.8g of ammonium persulfate-sodium bisulfate initiator is slowly and uniformly dripped into the reaction system, after all materials are added, stirring is continued, polymerization is carried out for 3-5 h, polymer gel is poured out, the polymer gel is soaked in absolute ethyl alcohol for 24 h, unreacted substances and other soluble substances are removed, and then the mixture is dried in an oven at 80 ℃ for 5-6 h, and crushed, thus obtaining the magnetic high polymer.
Preferably, 0.8g of ammonium persulfate-sodium bisulfite initiator is prepared into a solution with the mass percent of 10 percent, and then slowly dripped into a reaction system.
Preferably, the synthesis method of the amino phosphonic acid chelate resin comprises the following steps:
1) Synthesis of crosslinked polyacrylamide: adding 40g acrylamide and 0.75g N, N' -methylenebisacrylamide into water phase, stirring to dissolve completely, introducing nitrogen to remove air, heating to 50deg.C, and dripping 0.15g K 2 S 2 0 8 And 0.15g KHS0 3 Maintaining the temperature of 50 ℃ for reaction under the protection of nitrogen, stopping the reaction when gel is generated, washing the generated gel with water and methanol in sequence, drying in a vacuum drying oven at 70 ℃, grinding and sieving after drying to obtain white powdery crosslinked polyacrylamide;
2) Synthesis of aminophosphonic acid chelate resin: 1.42g of crosslinked polyacrylamide is weighed, after the crosslinked polyacrylamide is swelled for 12 hours by distilled water at room temperature, the pH value of the solution is regulated to be ll by Na0H solution, then 0.6g of paraformaldehyde dry powder is added, the mixture is uniformly mixed and stirred, the crosslinked polyacrylamide and the paraformaldehyde are subjected to methylolation reaction at 25 ℃ and react for 3 hours by maintaining the temperature, phosphorous acid is added into a reaction system, the molar ratio of the phosphorous acid to the paraformaldehyde is 1.4:1, the temperature is increased to 90 ℃, the reflux and stirring are carried out for 8 hours, after the reaction is finished, the product is washed to be neutral, the product is washed by 1mol/L of NaOH solution for a plurality of times, the product is washed by 1mol/L of hydrochloric acid for a plurality of times to be converted to be hydrogen form, the product is washed by the 1mol/L of hydrochloric acid again to be neutral, and finally the product is washed by methanol for 3 to 4 times, and the product is dried to be constant in vacuum to obtain the amino phosphonic acid chelate resin.
Preferably, the drag reduction retarder is composed of polyacrylamide drag reduction agent and sodium lignin sulfonate retarder according to a weight ratio of 1:1.
Preferably, the superfine cement is superfine G-grade cement, the median particle diameter is 9.2 μm, and the specific surface area is 6540m 2 /g。
The invention also provides a preparation method of the patch,
adding superfine cement, mineral powder, superfine silica fume and sepiolite powder in a container in a specified weight part, and uniformly stirring;
and secondly, adding the swelling 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 the finished product of the blocking agent.
In the drilling process, in order to prevent formation fluid from entering the well, the pressure of a drilling fluid column is generally controlled to be higher than the formation pressure, free water in the drilling fluid permeates into a rock crack or a gap of a well wall under the action of the pressure difference between the drilling fluid column and the formation pressure, and the process is called the fluid loss effect of the drilling fluid. During the fluid loss process, some solid particles in the drilling fluid adhere to the well wall to form a mud cake. The process of forming mud cakes by attaching solid particles to the well wall is called wall forming property of drilling fluid. After a mud cake is formed on the well wall, free water in the drilling fluid can be prevented or slowed down to continuously invade the stratum.
The development of the plugging agent formula system adopts the drilling fluid wall-making concept, and a compact, impermeable, thin-wall and net-shaped 'cement cake' is formed in near-wellbore zones, hollow walls, large pore canals and crack inlets rapidly. After the large-size material forms the bridge, the smaller-size material is embedded and blocked on the small pore canal formed by the bridge material. By means of the elasticity and plasticity of the active material of the plugging agent, powerful lacing wire net-shaped effect occurs, and a firm plug-shaped cushion layer which is difficult to move is formed, so that the purpose of plugging is achieved.
The narrow-gap annular short well Duan Gujing requires good pumping performance of the well cementation plugging agent, and excellent water loss reduction performance, and the slurry prepared by the well cementation plugging agent has relatively low viscosity and water separation rate of less than 2 percent.
The magnetic high molecular polymer in the formula is formed by the reaction of acrylic acid, acrylamide, N-methylene bisacrylamide, polyvinylpyrrolidone, iron oxide and the like, and a polymer system with weak magnetism on the surface is formed by introducing a 'molecular bridge' between the interfaces of inorganic substances and organic substances which are chemically connected with the base frame. The magnetic high molecular polymer contains COO - To make its surface negatively charged, and iron oxide (Fe 2 O 3 Or Fe 3 O 4 ) Under acidic conditionsThe lower surface has positive charges, and the iron oxide ions of the lower surface are wrapped 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 through polymerization.
Through experiments, the water absorption of the plugging agent for well cementation is obviously improved by adding the weakly magnetic polymer, and the apparent viscosity is reduced along with the increase of the adding amount. Probably due to the addition of iron oxides, in particular Fe 2 O 3 The intermolecular acting force is reduced, the relative sliding among 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 plugging agent for well cementation.
The amino phosphonic acid chelating resin in the formula is synthesized by taking acrylamide as a framework and carrying out methylolation and phosphorylation on crosslinked polyacrylamide, wherein 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 coordination bonds, can form relatively stable chelates with a plurality of metal ions, and has adsorption capacity more advantageous than metal ions with high valence such as Fe, cu and the like attached on the inner wall of an old sleeve.
Sepiolite powder in the formula system belongs to fibrous clay minerals, and has main chemical compositions of silicon (Si) and magnesium (Mg), and the chemical formula is Mg 8 Si 12 O 30 (OH) 4 (OH 2 ) 4 ·8H 2 O; in the chemical formula "8H 2 O' represents adsorbed water, sepiolite powder is adsorbed on the surface of minerals and occupies part of the central channel; (OH) 2 ) 4 Represents water of crystallization combined with octahedral layer magnesium ions; (OH) 4 Represents structural water, usually in the form of hydroxyl groups. Sepiolite powder with its unique water adsorption channel and large holes contained in fiber bundle to make its theoretical specific surface area up to 900m 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 bridge and form a net, so that the consistency of the slurry is increased, and the pumping and displacement efficiency of the slurry is affected, 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 drag reduction and retarding components are sodium lignin sulfonate and acrylamide, active groups of sodium lignin sulfonate molecules are adsorbed on the surfaces of cement particles, the Z potential of the surfaces of the cement particles is improved, the purpose of drag reduction is achieved by electrostatic repulsive force, meanwhile, the steric hindrance caused by the adsorption of acrylamide molecules on the surfaces of the cement particles realizes the dispersion effect, and the slurry with plasticity and rheological property is formed under the combined action of the sodium lignin sulfonate and the acrylamide molecules.
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 of the slurry and in the early stage of hardening, and can ensure the continuity of the expansion of the drilling fluid slurry from the plastic state to the early stage of hardening, namely has double expansion effects.
The average grain size of the superfine silica fume is 0.1-0.15 mu m, which is several percent of the average grain size of the common cement, and the specific surface area is 15-27 m 2 And/g, has extremely strong surface activity and can be chemically combined with organic functional groups; meanwhile, the catalyst also contains silanol which is easy to hydrolyze and reacts with oxide or hydroxyl on the surface of inorganic substances to generate stable silicon-oxygen bond. In addition, the interface performance of different materials can be improved, and the embedding and blocking in the bridging and net-forming structure can be realized.
Drawings
FIG. 1 is a photograph of a microscopic view of the patch of example 1;
Detailed Description
The invention is further illustrated by the following specific examples, which are, however, merely exemplary and should not be construed as limiting the invention.
In the following examples, the average particle diameter of the ultrafine silica fume is 0.1 to 0.15. Mu.m, and the specific surface area is 15 to 27m 2 And/g. The expanding agent is lattice type expanding agent, and magnesium oxide is specifically selected. The drag reduction retarder is composed of polyacrylamide drag reduction agent and sodium lignin sulfonate retarder according to a weight ratio of 1:1.
The mineral powder is a byproduct of smelting pig iron in a blast furnace, and comprises magnesium oxide, silicon dioxide, aluminum oxide, a small amount of calcium oxide, ferric oxide and other compounds as main components, wherein the median particle size is 7.8 mu m, and the specific surface area is 7660m 2 /g。
To verify the beneficial effects of the examples, the ultra-fine cement was ultra-fine G-grade cement having a median particle diameter 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) Preparation of iron oxide magnetic nanoparticles: 300mL of deionized water was added to a flask equipped with a condenser, an air duct, a thermometer, a dropping funnel, and a magnetic stirrer, nitrogen was introduced to perform nitrogen protection, and 3g of FeCl was added 3 And FeCl 2 Wherein FeCl 3 And FeCl 2 The molar ratio of (2) to (1) is 2:1, 30ml of 28% ammonia water is quickly added dropwise when the temperature is raised to 50 ℃, after the ammonia water is added dropwise, the temperature is kept at 50 ℃, the reaction time is 4.5 hours, the reaction time is reduced to room temperature, the reaction time is poured into a beaker, deionized water is used for washing, and magnet separation is carried out, so that the washed iron oxide magnetic nano particles are finally obtained;
2) Preparation of KH570 modified magnetic nanoparticles: adding 300mL of deionized water and 150mL of ethanol into a flask, introducing nitrogen, performing nitrogen protection, adding 2g of iron oxide magnetic nanoparticles, heating to 50 ℃, adding 25mL of 28% ammonia water by mass concentration, slowly dropwise adding 6mL of silane coupling agent KH570, after dropwise adding, preserving heat at 50 ℃ for 4 hours, cooling to room temperature, washing with deionized water for 5 times, 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 nano particles, 0.64g of acrylamide, 0.03g of N, N-methylene bisacrylamide, 1.2g of polyvinylpyrrolidone and 0.96g of acrylic acid with the neutralization degree of 70% are respectively added into a flask, uniformly stirred, finally 0.8g of ammonium persulfate-sodium bisulfate initiator is slowly and uniformly dripped into the reaction system, after all materials are added, stirring is continued, after 4h of polymerization reaction, polymer gel is poured out, the polymer gel is soaked in absolute ethyl alcohol for 24 h, unreacted substances and other soluble substances are removed, and then the mixture is dried in an oven at 80 ℃ for 6 h, and crushed, so that the magnetic high-molecular polymer is obtained.
0.8g of ammonium persulfate-sodium bisulfite initiator is prepared into a solution with the mass percent of 10 percent, and then slowly dripped into a reaction system.
The synthesis method of the amino phosphonic acid chelate resin comprises the following steps:
1) Synthesis of crosslinked polyacrylamide: adding 40g of acrylamide and 0.75g of N, N' -methylenebisacrylamide into a water phase respectively, stirring until the acrylamide is fully dissolved, introducing nitrogen for about 20min to remove air, heating to 50 ℃, and simultaneously dropwise adding 0.15g of K respectively 2 S 2 0 8 And 0.15g KHS0 3 Maintaining the temperature of 50 ℃ for reaction under the protection of nitrogen, stopping the reaction when gel is generated, washing the generated gel with water and methanol in sequence, drying in a vacuum drying oven at 70 ℃, grinding and sieving after drying to obtain white powdery crosslinked polyacrylamide;
2) Synthesis of aminophosphonic acid chelate resin: 1.42g of crosslinked polyacrylamide is weighed, after the crosslinked polyacrylamide is swelled for 12 hours by distilled water at room temperature, the pH value of the solution is regulated to be ll by Na0H solution, then 0.6g of paraformaldehyde dry powder is added, the mixture is uniformly mixed and stirred, the crosslinked polyacrylamide and the paraformaldehyde are subjected to methylolation reaction at 25 ℃ and react for 3 hours by maintaining the temperature, phosphorous acid is added into a reaction system, the molar ratio of the phosphorous acid to the paraformaldehyde is 1.4:1, the temperature is increased to 90 ℃, the reflux and stirring are carried out for 8 hours, after the reaction is finished, the product is washed to be neutral, the product is washed by 1mol/L of NaOH solution for a plurality of times, the product is washed by 1mol/L of hydrochloric acid for a plurality of times to be converted to hydrogen form, the product is washed by the 1mol/L of hydrochloric acid again to be neutral, and finally the product is washed by methanol for 4 times, and the product is dried in vacuum to be constant weight, thus obtaining the amino phosphonic acid chelating resin.
Example 1
The patch comprises the following components in parts by weight:
ultra-fine cement 46; mineral powder 41; superfine silica fume 1; sepiolite powder 1; 0.2 of magnetic high molecular polymer; an expanding agent 3; aminophosphonic acid chelate resin 1; and 0.2 of drag reducing retarder.
The preparation method of the sticking agent comprises the following steps:
adding superfine cement, mineral powder, superfine silica fume and sepiolite powder in a container in a specified weight part, and uniformly stirring;
and secondly, adding the swelling 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 the finished product of the plugging agent for well cementation.
Example 2
The patch comprises the following components in parts by weight:
superfine cement 48; mineral powder 43; ultrafine silica fume 2; sepiolite powder 2; 0.5 parts of magnetic high molecular polymer; an expanding agent 4; 1.5 parts of amino phosphonic acid chelate resin; and 0.3 of drag reducing retarder.
The preparation method of the sticking agent comprises the following steps:
adding superfine cement, mineral powder, superfine silica fume and sepiolite powder in a container in a specified weight part, and uniformly stirring;
and secondly, adding the swelling 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 the finished product of the plugging agent for well cementation.
Example 3
The patch comprises the following components in parts by weight:
ultra-fine cement 50; mineral powder 46; superfine silica fume 3; sepiolite powder 3; 0.8 of magnetic high molecular polymer; an expanding agent 5; aminophosphonic acid chelate resin 2; and 0.5 of drag reducing retarder.
The preparation method of the sticking agent comprises the following steps:
adding superfine cement, mineral powder, superfine silica fume and sepiolite powder in a container in a specified weight part, and uniformly stirring;
and secondly, adding the swelling 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 the finished product of the plugging agent for well cementation.
Comparative example 1
The patch comprises the following components in parts by weight:
ultra-fine cement 50; mineral powder 46; superfine silica fume 3; sepiolite powder 3; an expanding agent 5; aminophosphonic acid chelate resin 2; and 0.5 of drag reducing retarder.
The preparation method of the sticking agent comprises the following steps:
adding superfine cement, mineral powder, superfine silica fume and sepiolite powder in a container in a specified weight part, and uniformly stirring;
and secondly, adding the swelling agent, 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 plugging agent for well cementation.
Comparative example 2
The patch comprises the following components in parts by weight:
ultra-fine cement 50; mineral powder 46; superfine silica fume 3; sepiolite powder 3; 0.8 of magnetic high molecular polymer; an expanding agent 5; and 0.5 of drag reducing retarder.
The preparation method of the sticking agent comprises the following steps:
adding superfine cement, mineral powder, superfine silica fume and sepiolite powder in a container in a specified weight part, and uniformly stirring;
and secondly, adding the swelling agent, the magnetic high molecular polymer and the drag reduction retarder in the specified weight parts into a container, and uniformly stirring to obtain the finished product of the well cementation plugging agent.
Slurry viscosity measurement 560 g of the prepared patch was weighed, 350 g of water was added, and after 10 minutes of stirring, the slurry was passed through a 16-hole per inch screen, and the time of filling 500ml of slurry was measured by a 1006-type slurry viscometer, reflecting the viscosity value.
Water evolution rate for 2 hours: 165g (accurate to 0.1 g) of the sample is weighed into a 250mL beaker, 100mL of water is added, the sample is stirred until the sample is completely dispersed in the water to form suspension slurry, the suspension slurry is stirred for 20min by a stirrer to prepare slurry, the slurry is added into a 500mL measuring cylinder, the rest is carried out for 2h, and the water precipitation amount is observed.
The water evolution rate is calculated according to formula (1).
Figure BDA0003611416010000121
Wherein:
s-water extraction rate,%;
v1, water precipitation, in milliliters (mL);
v 0-total amount of suspension slurry in milliliters (mL).
The test results are shown in table 1 below.
Sequence number Viscosity mPas Precipitation (ml) Slurry volume (ml) Rate of water evolution (%)
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
Compressive strength tests were also performed on the examples and comparative examples, 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 amino phosphonic acid chelate resin obtained by the invention is a cationic chelate resin, and N atoms and O atoms in the chelate group of the resin form coordination bonds with high-valence metal ions, so that the adsorption capacity of the chelate resin on the metal surface or the scaling surface of the inner wall of the sleeve is ensured.
The amino phosphonic acid chelate resin is added, and under the condition of similar strength indexes, the flexural strength and the plastic modulus are greatly improved. The yield deformation characteristics of aminophosphonic acid chelate resins result from the impediment of the expansion of individual shear bands and the induction of multiple shear bands at the site of impediment, the shear band generation and expansion process being discontinuous. Thus, the patch material breaks with a pronounced choroidal character. The interface between the blocking agent and the inner wall of the sleeve still keeps a good state when being damaged, which indicates that the blocking agent and the inner wall of the sleeve have good bonding capability.
The applicant has carried out a field practical application using the technical solution of example 3.
Positive circulation well flushing with clear water; pressing the adhesive agentIrradiating with light of 1.70-1.75g/cm 3 Adding the mixture into clear water to prepare mortar 4m 3 The initial setting time is required to be not less than 200min. Opening the sleeve gate, and replacing mortar by 4.0m 3 5.2m of clean water 3 Closing an internal rotation plug valve or a gate on a water tap connected with an oil pipe, opening a blowout preventer, placing the whole load of a tubular column, pressurizing and sitting on a sand surface, lifting the tubular column load to a point of neutralization at a positive and negative joint, removing the weight of a plugged pipe, rotating for 20-30 circles in a positive direction, and lifting the tubular column for 2-3m after success; closing the blowout preventer; the water is reversely replaced by the sleeve pipe to be controlled at 3.3m 3 Is within; slowly opening a water tap gate to release pressure, flushing the well with clean water in a large discharge capacity, and washing out redundant mortar in the well; and (5) closing the well, condensing for 48 hours, and flushing sand to the artificial well bottom by drilling plugs. And (5) opening the lower pump.
And implementing 12 times in total, completing 12 wells, and uniformly testing the pressure for 15MPa after plugging. The oil increasing effect is seen to be 12 wells, the effective rate is 100%, daily oil increasing amount is 19.8 tons, the average daily oil increasing amount of a single well is 1.65 tons, the average effective period is 154 days, the accumulated oil increasing amount is 2415.48 tons, the average single well oil increasing amount 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 understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made therein without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.

Claims (9)

1. The patch is characterized by comprising the following components in parts by weight:
46-50 parts of superfine cement; 41-46 of mineral powder; 1-3 parts of superfine silica fume; sepiolite powder 1-3; 0.2 to 0.8 percent of magnetic high molecular polymer; 3-5 parts of an expanding agent; 1-2 parts of amino phosphonic acid chelate resin; 0.2 to 0.5 of drag reduction retarder;
the synthesis method of the amino phosphonic acid chelate resin comprises the following steps:
1) Synthesis of crosslinked polyacrylamide: adding 40g of acrylamide and 0.75g of N, N' -methylenebisacrylamide into a water phase respectively, stirring until the acrylamide is fully dissolved, introducing nitrogen to remove air, and heating to 50 ℃ and 0.15gK is respectively added dropwise 2 S 2 0 8 And 0.15g KHS0 3 Maintaining the temperature of 50 ℃ for reaction under the protection of nitrogen, stopping the reaction when gel is generated, washing the generated gel with water and methanol in sequence, drying in a vacuum drying oven at 70 ℃, grinding and sieving after drying to obtain white powdery crosslinked polyacrylamide;
2) Synthesis of aminophosphonic acid chelate resin: 1.42g of crosslinked polyacrylamide is weighed, after the crosslinked polyacrylamide is swelled for 12 hours by distilled water at room temperature, the pH value of the solution is regulated to be ll by Na0H solution, then 0.6g of paraformaldehyde dry powder is added, the mixture is uniformly mixed and stirred, the crosslinked polyacrylamide and the paraformaldehyde are subjected to methylolation reaction at 25 ℃ and react for 3 hours by maintaining the temperature, phosphorous acid is added into a reaction system, the molar ratio of the phosphorous acid to the paraformaldehyde is 1.4:1, the temperature is increased to 90 ℃, the reflux and stirring are carried out for 8 hours, after the reaction is finished, the product is washed to be neutral, the product is washed by 1mol/L of NaOH solution for a plurality of times, the product is washed by 1mol/L of hydrochloric acid for a plurality of times to be converted to be hydrogen form, the product is washed by the 1mol/L of hydrochloric acid again to be neutral, and finally the product is washed by methanol for 3 to 4 times, and the product is dried to be constant in vacuum to obtain the amino phosphonic acid chelate resin.
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 amino phosphonic acid chelating resin; and 0.3 of drag reducing retarder.
3. The patch according to claim 1 or 2, wherein 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 /g。
4. The patch according to claim 1 or 2, wherein the swelling agent is a lattice type swelling agent.
5. A patch as claimed in claim 1 or claim 2, wherein,
the preparation method of the magnetic high molecular polymer comprises the following steps,
1) Preparation of iron oxide magnetic nanoparticles: 300mL of deionized water was added to the flask, nitrogen was purged, and 3g of FeCl was added after nitrogen protection 3 And FeCl 2 Wherein FeCl 3 And FeCl 2 The molar ratio of (2) to (1) is 2:1, 30ml of ammonia water with the concentration of 25-30% is quickly dripped when the temperature is raised to 50 ℃, after the ammonia water is dripped, the temperature is kept at 50 ℃, the reaction time is 4.5 hours, the reaction time is reduced to room temperature, the reaction time is poured into a beaker, deionized water is used for washing, and magnet separation is carried out, so that the washed iron oxide magnetic nano particles are finally obtained;
2) Preparation of KH570 modified magnetic nanoparticles: adding 300mL of deionized water and 150mL of ethanol into a flask, introducing nitrogen, performing nitrogen protection, adding 2g of iron oxide magnetic nanoparticles, heating to 50 ℃, adding 25mL of ammonia water with mass concentration of 25-30%, slowly dropwise adding 6mL of silane coupling agent KH570, after dropwise adding, preserving heat 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: 150mL of deionized water, 2.5g of modified magnetic nano particles, 0.64g of acrylamide, 0.03g of N, N-methylene bisacrylamide, 1.2g of polyvinylpyrrolidone and 0.96g of acrylic acid with the neutralization degree of 70% are respectively added into a flask, uniformly stirred, finally 0.8g of ammonium persulfate-sodium bisulfate initiator is slowly and uniformly dripped into the reaction system, after all materials are added, stirring is continued, polymerization is carried out for 3-5 h, polymer gel is poured out, the polymer gel is soaked in absolute ethyl alcohol for 24 h, unreacted substances and other soluble substances are removed, and then the mixture is dried in an oven at 80 ℃ for 5-6 h, and crushed, thus obtaining the magnetic high polymer.
6. The patch according to claim 5, wherein,
0.8g of ammonium persulfate-sodium bisulfite initiator is prepared into a solution with the mass percent of 10 percent, and then slowly dripped into a reaction system.
7. The patch according to claim 1 or 2, wherein the drag reducing retarder is composed of polyacrylamide drag reducing agent and sodium lignin sulfonate retarder according to a weight ratio of 1:1.
8. The method for preparing a patch according to claim 1 or 2, wherein the ultra-fine cement is ultra-fine G-grade cement, the median particle diameter is 9.2 μm, and the specific surface area is 6540m 2 /g。
9. The method for producing a patch according to claim 1 or 2, wherein,
adding superfine cement, mineral powder, superfine silica fume and sepiolite powder in a container in a specified weight part, and uniformly stirring;
and secondly, adding the swelling 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 the finished product of the blocking agent.
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