CN111995994A - High-pressure-bearing plugging agent for oil production casing pipe and processing technology thereof - Google Patents
High-pressure-bearing plugging agent for oil production casing pipe and processing technology thereof Download PDFInfo
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- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/42—Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells
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- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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- C09K8/422—Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells specially adapted for sealing expandable pipes, e.g. of the non-hardening type
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Abstract
The invention discloses a high-pressure-bearing plugging agent for an oil production casing and a processing technology thereof, wherein the high-pressure-bearing plugging agent for the oil production casing comprises 48-60 parts of MOFs-modified epoxy resin, 23-27 parts of solid particles, 17-21 parts of curing agent, 13-17 parts of coupling agent and 0.7-1.2 parts of curing regulator; the MOFs-modified epoxy resin is prepared by multistage reaction of bisphenol A epoxy resin, nano silicon nitride, an acrylate monomer, methacrylic acid, acrylonitrile, hydroxyl-terminated butadiene-acrylonitrile rubber powder and MOFs materials, and the modified epoxy resin, a curing agent and solid particles are crosslinked to form the plugging agent, so that the plugging agent has the advantages of high mechanical strength, strong bearing capacity, high thermal stability, salt and alkali resistance, and capability of slowly expanding when meeting water to enhance the sealing property; the plugging agent acts in the oil extraction casing pipe, can effectively plug leakage layers such as pores, cracks and the like, and can prevent leakage by extrusion.
Description
Technical Field
The invention relates to the technical field of chemical plugging of oil fields, in particular to a high-pressure-bearing plugging agent for an oil extraction casing and a processing technology thereof.
Background
Along with long-term exploitation, some old wells, the service life of oil-gas well casing is too long, well cement does not completely seal the oil-gas well casing, when perforating, the cement ring of a perforating well section is shattered, so that in a free section of the casing, a sealing section and a production interval are perforated due to corrosion, in addition, special and complex geological conditions, a salt-gypsum layer develops, the motion of a crust causes the deformation of the casing, the damage causes the slurry and water to be discharged from a stratum, and long-term water injection development, especially pressurized water injection, the damage phenomenon of the oil-water well casing is very common, the problem of well condition deterioration is increasingly prominent, and the normal production of the oil-gas well is seriously influenced. At present, the problem of bad perforation of a casing pipe caused by corrosion and other reasons of an oil-water well is solved, and gel materials are mainly adopted for plugging. The conventional gel plugging technology has a good effect in field application, but has some disadvantages that a cross-linking action domain line in a polymer system is difficult to form a continuous space grid structure, so that the strength of the gel plugging agent is not high, and the pressure-bearing capacity is weak; the gel polymer is easily influenced by external temperature and the like, so that the gelling time and the gelling strength of the plugging agent are difficult to regulate and control in site construction.
Disclosure of Invention
The invention aims to provide a high-pressure-bearing plugging agent for an oil production casing and a processing technology thereof.
In order to achieve the purpose, the invention provides the following technical scheme: the high pressure-bearing plugging agent for the oil extraction casing comprises the following raw material components; 48-60 parts of MOFs-modified epoxy resin, 23-27 parts of solid particles, 17-21 parts of curing agent, 13-17 parts of coupling agent and 0.7-1.2 parts of curing regulator.
The MOFs-modified epoxy resin is prepared by carrying out multi-stage reaction on bisphenol A epoxy resin, nano silicon nitride, an acrylate monomer, methacrylic acid, acrylonitrile, hydroxyl-terminated butadiene-acrylonitrile rubber powder and an MOFs material; the MOFs material is one or more of Ni-MOF, Co-MOF and Fe-MOF. The solid particles are formed by mixing bentonite and attapulgite, and the mass ratio of the bentonite to the attapulgite is 3: 1.
The curing agent is a polyamide or modified amine type curing agent. The coupling agent is at least one of 3-glycidoxypropyltrimethoxysilane, propyltrimethoxysilane, trimethoxysilane, triethoxysilane, phenyltriethoxysilane, phenyltrimethoxysilane and diphenyldimethoxysilane; the curing accelerator is at least one of 2-methylimidazole, 2-ethyl-4-methylimidazole, 2-phenylimidazole and tris- (dimethylaminomethyl) phenol. The acrylate monomer is any one of methyl acrylate, ethyl acrylate, butyl acrylate and octyl acrylate.
The curing agent is polyamide or modified amine curing agent, which is dissolved with the modified epoxy resin, and the curing time is adjustable through the dosage of the curing agent, so that the plugging agent is not cured in the sinking process, is smoothly settled to a leakage part and is rapidly cured at high temperature.
The solid granular bentonite and attapulgite have good dispersibility, and are added into a plugging agent system to mainly play a role in adjusting density and viscosity.
A processing technology of a high pressure-bearing plugging agent for an oil extraction casing comprises the following steps: (1) preparing MOFs-modified epoxy resin, and (2) mixing and stirring to obtain a finished product of the high-pressure-bearing plugging agent for the oil production casing.
A processing technology of a high pressure-bearing plugging agent for an oil extraction casing comprises the following steps; (1) preparing MOFs-modified epoxy resin: dissolving an acrylate monomer, methacrylic acid and acrylonitrile in an acetone solution, adding dimethyl azodiisobutyrate, maintaining the pressure with nitrogen, reacting for 2.5-3h, cooling, and drying in vacuum to obtain a substance A; dissolving nano silicon nitride in an acetone solution, adding the substance A, stirring, reacting for 2-2.5h, and drying in vacuum to obtain a substance B;
ultrasonically dispersing the substance B and the hydroxyl-terminated butadiene-acrylonitrile rubber powder in an acetone solution, reacting for 25-30min, filtering, and drying to obtain a substance C; dissolving bisphenol A epoxy resin and allyl glycidyl ether in absolute ethyl alcohol to form epoxy resin solution; dissolving the substance C and the propyl trimethoxy silane in a xylene solvent to form a solution D; dropwise adding the solution D into an epoxy resin solution, reacting for 3.5-4h, cooling, filtering, and drying in vacuum to obtain modified epoxy resin; adding deionized water and MOFs materials, and carrying out ultrasonic dispersion for 2-3 h; thus obtaining the MOFs-modified epoxy resin.
The nano silicon nitride is a molecular material with higher strength, high thermal stability, salt and alkali resistance and cold and hot shock resistance, and in a plugging agent system, the hydroxyl groups on the surface of the nano silicon carbide are easy to combine with each other to generate hydrolysis and generate an agglomeration phenomenon, so that the nano silicon nitride has poor compatibility with the system; according to the technical scheme, a high molecular polymer is formed by graft polymerization of an acrylate monomer, methacrylic acid and acrylonitrile; the nano silicon nitride is used as a modifier for surface treatment of the nano silicon nitride; the hydroxyl and the amino on the surface of the nano silicon nitride molecule react with-CN, thereby avoiding the agglomeration phenomenon of the nano silicon nitride molecule caused by the self hydroxyl reaction and improving the dispersion effect of the silicon nitride in the system. The compatibility of the nano silicon nitride with-CN introduced to the surface and the hydroxyl-terminated butadiene-acrylonitrile rubber is enhanced, and a polymer of the hydroxyl-terminated butadiene-acrylonitrile rubber coated with the nano silicon nitride is obtained through reaction treatment; the polymer has the advantages of high strength, excellent thermal stability and rubber toughness of nano silicon nitride, and good dispersion effect with a system. The bisphenol A epoxy resin is modified by using the modified bisphenol A epoxy resin as a modifier, and under the action of a silane coupling agent, the ring opening of the epoxy resin and a branched chain structure formed by rubber and nano silicon nitride form a space network structure. When bearing pressure, the space network structure has good elasticity, and can play a role in quick buffering. The rubber molecules can absorb water and slowly expand, so that the elasticity and the strength of the molecules are further improved, and the effect of water-swelling sealing can be achieved. The modified epoxy resin and the MOFs material with a porous structure act to form an interpenetrating network structure, so that the toughness and strength of molecules are further improved; in addition, the MOFs material can protect metal in acidic and alkaline solutions, and reduce surface metal corrosion. Therefore, when the plugging agent prepared from the MOFs-modified epoxy resin is applied to an oil extraction casing, the solid phase has the characteristics of higher mechanical strength, high pressure bearing, thermal stability and corrosion resistance.
(2) Mixing and stirring to prepare a finished product of the high-pressure-bearing plugging agent for the oil production casing; uniformly mixing the MOFs-modified epoxy resin prepared in the step (1), 23-27 parts of solid particles and 13-17 parts of coupling agent, dispersing at a high speed, adding 17-21 parts of curing agent and 0.7-1.2 parts of curing regulator, filtering, drying and grinding to prepare the high-pressure-bearing plugging agent for the oil production casing.
A processing technology of a high pressure-bearing plugging agent for an oil extraction casing is characterized in that; the preparation method comprises the following steps of (1) MOFs-modified epoxy resin: taking an acrylate monomer, methacrylic acid and acrylonitrile in a mass ratio of 75:5: 10; dissolving in acetone solution, adding dimethyl azodiisobutyrate at the temperature of 8-10 ℃, maintaining the pressure with nitrogen, heating to 48-52 ℃, reacting for 2.5-3h, cooling, and vacuum drying to obtain a substance A; dissolving nano silicon nitride in an acetone solution, adding the substance A, stirring, reacting at the temperature of 105-115 ℃ for 2-2.5h, and performing vacuum drying to obtain a substance B;
ultrasonically dispersing the substance B and the hydroxyl-terminated butadiene-acrylonitrile rubber powder in an acetone solution, reacting at 48-52 ℃ for 25-30min, filtering, and drying to obtain a substance C; dissolving bisphenol A epoxy resin and allyl glycidyl ether in absolute ethyl alcohol, and heating to 63-70 ℃ to form epoxy resin solution; dissolving the substance C and the propyl trimethoxy silane in a xylene solvent to form a solution D; dropwise adding the solution D into an epoxy resin solution, reacting for 3.5-4h at the temperature of 185-190 ℃, cooling, filtering, and drying in vacuum to obtain modified epoxy resin; (ii) a Adding deionized water and MOFs materials, wherein the mass ratio of the deionized water to the modified epoxy resin is 1:1, and ultrasonically dispersing for 2-3 h; preparing MOFs-modified epoxy resin;
(2) mixing and stirring to prepare a finished product of the high-pressure-bearing plugging agent for the oil production casing; uniformly mixing the MOFs-modified epoxy resin prepared in the step (1), solid particles and a coupling agent, dispersing at a high speed at the rotating speed of 2500-.
The obtained plugging agent is mixed with cement sand slurry, pumped into an oil production casing and solidified to play a plugging effect.
Compared with the prior art, the invention has the beneficial effects that: the modified epoxy resin with rubber flexibility and high mechanical strength, saline-alkali resistance and thermal stability of silicon nitride is prepared by carrying out multi-stage reaction on bisphenol A epoxy resin, nano silicon nitride, an acrylate monomer, methacrylic acid, acrylonitrile and hydroxyl-terminated butadiene-acrylonitrile rubber powder; the modified epoxy resin is reacted with MOFs material to form MOFs-modified epoxy resin. The composite material is crosslinked and ground with a curing agent, a crosslinking agent and solid particles to form plugging agent powder, the plugging agent can quickly form an interpenetrating space network structure, has higher mechanical strength, strong bearing capacity, high thermal stability, saline and alkaline resistance, corrosion resistance and can slowly expand when meeting water to enhance the sealing property; the plugging agent acts in the oil extraction casing pipe, can effectively plug leakage layers such as pores, cracks and the like, prevents leakage by extrusion, and reduces corrosion of the oil extraction casing pipe.
The specific implementation mode is as follows:
the technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
A high pressure-bearing plugging agent for an oil extraction casing comprises the following raw material components; 48 parts of MOFs-modified epoxy resin, 23 parts of solid particles, 17 parts of curing agent, 13 parts of coupling agent and 0.7 part of curing regulator.
The solid particles are formed by mixing bentonite and attapulgite, and the mass ratio of the bentonite to the attapulgite is 3: 1.
A processing technology of a high-pressure-bearing plugging agent for an oil production casing comprises the following steps (1) of MOFs-modified epoxy resin: taking an acrylate monomer, methacrylic acid and acrylonitrile in a mass ratio of 75:5: 10; dissolving in acetone solution, adding dimethyl azodiisobutyrate at the temperature of 8 ℃, heating to 48 ℃, reacting for 2.5h, cooling, and drying in vacuum to obtain a substance A; dissolving nano silicon nitride in an acetone solution, adding the substance A, stirring, reacting for 2 hours at the temperature of 105 ℃, and performing vacuum drying to obtain a substance B;
ultrasonically dispersing the substance B and the hydroxyl-terminated butadiene-acrylonitrile rubber powder in an acetone solution, reacting for 25min at the temperature of 48 ℃, filtering and drying to obtain a substance C;
dissolving bisphenol A epoxy resin and allyl glycidyl ether in absolute ethyl alcohol, and heating to 63 ℃ to form epoxy resin solution; dissolving the substance C and the propyl trimethoxy silane in a xylene solvent to form a solution D; dropwise adding the solution D into an epoxy resin solution, reacting for 3.5h at 185 ℃, cooling, filtering, and drying in vacuum to obtain modified epoxy resin; adding deionized water and MOFs materials, and carrying out ultrasonic dispersion for 2 hours; preparing MOFs-modified epoxy resin;
(2) mixing and stirring to prepare a finished product of the high-pressure-bearing plugging agent for the oil production casing; uniformly mixing the MOFs-modified epoxy resin prepared in the step (1), solid particles and a coupling agent, dispersing at a high speed at the rotating speed of 2500r/min, adding a curing agent and a curing regulator, filtering, drying and grinding to prepare the high-pressure-bearing plugging agent for the oil production casing.
Example 2
A high pressure-bearing plugging agent for an oil extraction casing comprises the following raw material components; 51 parts of MOFs-modified epoxy resin, 25 parts of solid particles, 20 parts of curing agent, 14 parts of coupling agent and 1.0 part of curing regulator.
The solid particles are formed by mixing bentonite and attapulgite, and the mass ratio of the bentonite to the attapulgite is 3: 1.
A processing technology of a high-pressure-bearing plugging agent for an oil production casing comprises the following steps (1) of MOFs-modified epoxy resin: taking an acrylate monomer, methacrylic acid and acrylonitrile in a mass ratio of 75:5: 10; dissolving in acetone solution, adding dimethyl azodiisobutyrate at the temperature of 9 ℃, heating to 51 ℃, reacting for 2.7h, cooling, and drying in vacuum to obtain a substance A; dissolving nano silicon nitride in an acetone solution, adding the substance A, stirring, reacting for 2.2 hours at the temperature of 112 ℃, and drying in vacuum to obtain a substance B;
ultrasonically dispersing the substance B and the hydroxyl-terminated butadiene-acrylonitrile rubber powder in an acetone solution, reacting at 50 ℃ for 27min, filtering and drying to obtain a substance C;
dissolving bisphenol A epoxy resin and allyl glycidyl ether in absolute ethyl alcohol, and heating to 66 ℃ to form epoxy resin solution; dissolving the substance C and the propyl trimethoxy silane in a xylene solvent to form a solution D; dropwise adding the solution D into an epoxy resin solution, reacting for 3.7h at the temperature of 188 ℃, cooling, filtering, and drying in vacuum to obtain modified epoxy resin; adding deionized water and MOFs materials, and carrying out ultrasonic dispersion for 2.5 h; preparing MOFs-modified epoxy resin;
(2) mixing and stirring to prepare a finished product of the high-pressure-bearing plugging agent for the oil production casing; uniformly mixing the MOFs-modified epoxy resin prepared in the step (1), solid particles and a coupling agent, dispersing at a high speed at the rotating speed of 2750r/min, adding a curing agent and a curing regulator, filtering, drying and grinding to prepare the high-pressure-bearing plugging agent for the oil production casing.
Example 3
A high pressure-bearing plugging agent for an oil extraction casing comprises the following raw material components; 60 parts of MOFs-modified epoxy resin, 27 parts of solid particles, 21 parts of curing agent, 17 parts of coupling agent and 1.2 parts of curing regulator.
The solid particles are formed by mixing bentonite and attapulgite, and the mass ratio of the bentonite to the attapulgite is 3: 1.
A processing technology of a high-pressure-bearing plugging agent for an oil production casing comprises the following steps (1) of MOFs-modified epoxy resin: taking an acrylate monomer, methacrylic acid and acrylonitrile in a mass ratio of 75:5: 10; dissolving in acetone solution, adding dimethyl azodiisobutyrate at 10 ℃, heating to 52 ℃, reacting for 3h, cooling, and vacuum drying to obtain a substance A; dissolving nano silicon nitride in an acetone solution, adding the substance A, stirring, reacting at 115 ℃ for 2.5 hours, and drying in vacuum to obtain a substance B;
ultrasonically dispersing the substance B and the hydroxyl-terminated butadiene-acrylonitrile rubber powder in an acetone solution, reacting at 52 ℃ for 30min, filtering and drying to obtain a substance C;
dissolving bisphenol A epoxy resin and allyl glycidyl ether in absolute ethyl alcohol, and heating to 70 ℃ to form epoxy resin solution; dissolving the substance C and the propyl trimethoxy silane in a xylene solvent to form a solution D; dropwise adding the solution D into an epoxy resin solution, reacting for 4 hours at the temperature of 190 ℃, cooling, filtering, and drying in vacuum to obtain modified epoxy resin; adding deionized water and MOFs materials, and dispersing for 3 hours by ultrasonic waves; preparing MOFs-modified epoxy resin;
(2) mixing and stirring to prepare a finished product of the high-pressure-bearing plugging agent for the oil production casing; uniformly mixing the MOFs-modified epoxy resin prepared in the step (1), solid particles and a coupling agent, dispersing at a high speed at a rotating speed of 3000r/min, adding a curing agent and a curing regulator, filtering, drying and grinding to prepare the high-pressure-bearing plugging agent for the oil production casing.
Comparative example 1
A high pressure-bearing plugging agent for an oil extraction casing comprises the following raw material components; 60 parts of modified epoxy resin, 27 parts of solid particles, 21 parts of curing agent, 17 parts of coupling agent and 1.2 parts of curing regulator.
The solid particles are formed by mixing bentonite and attapulgite, and the mass ratio of the bentonite to the attapulgite is 3: 1.
A processing technology of a high-pressure-bearing plugging agent for an oil extraction casing comprises the following steps of (1) modifying epoxy resin: taking an acrylate monomer, methacrylic acid and acrylonitrile in a mass ratio of 75:5: 10; dissolving in acetone solution, adding dimethyl azodiisobutyrate at 10 ℃, heating to 52 ℃, reacting for 3h, cooling, and vacuum drying to obtain a substance A; dissolving nano silicon nitride in an acetone solution, adding the substance A, stirring, reacting at 115 ℃ for 2.5 hours, and drying in vacuum to obtain a substance B;
ultrasonically dispersing the substance B and the hydroxyl-terminated butadiene-acrylonitrile rubber powder in an acetone solution, reacting at 52 ℃ for 30min, filtering and drying to obtain a substance C;
dissolving bisphenol A epoxy resin and allyl glycidyl ether in absolute ethyl alcohol, and heating to 70 ℃ to form epoxy resin solution; dissolving the substance C and the propyl trimethoxy silane in a xylene solvent to form a solution D; dropwise adding the solution D into an epoxy resin solution, reacting for 4 hours at the temperature of 190 ℃, cooling, filtering, and drying in vacuum to obtain modified epoxy resin;
(2) mixing and stirring to prepare a finished product of the high-pressure-bearing plugging agent for the oil production casing; uniformly mixing the modified epoxy resin, the solid particles and the coupling agent, dispersing at a high speed, adding a curing agent and a curing regulator at a rotating speed of 3000r/min, filtering, drying and grinding to obtain the high-pressure-bearing plugging agent for the oil production casing.
Comparative example 2
A high pressure-bearing plugging agent for an oil extraction casing comprises the following raw material components; 60 parts of MOFs-epoxy resin, 27 parts of solid particles, 21 parts of curing agent, 17 parts of coupling agent and 1.2 parts of curing regulator.
The solid particles are formed by mixing bentonite and attapulgite, and the mass ratio of the bentonite to the attapulgite is 3: 1.
A processing technology of a high pressure-bearing plugging agent for an oil production casing comprises the following steps (1) of MOFs-epoxy resin: taking epoxy resin, adding deionized water and MOFs materials, and ultrasonically dispersing for 3 hours; preparing MOFs-epoxy resin;
(2) mixing and stirring to prepare a finished product of the high-pressure-bearing plugging agent for the oil production casing; uniformly mixing the MOFs-epoxy resin prepared in the step (1), solid particles and a coupling agent, dispersing at a high speed at a rotating speed of 3000r/min, adding a curing agent and a curing regulator, filtering, drying and grinding to prepare the high-pressure-bearing plugging agent for the oil production casing.
Comparative example 2
A high pressure-bearing plugging agent for an oil extraction casing comprises the following raw material components; 60 parts of modified epoxy resin, 27 parts of solid particles, 21 parts of curing agent, 17 parts of coupling agent and 1.2 parts of curing regulator.
The solid particles are formed by mixing bentonite and attapulgite, and the mass ratio of the bentonite to the attapulgite is 3: 1.
A processing technology of a high-pressure-bearing plugging agent for an oil extraction casing comprises the following steps of (1) modifying epoxy resin: taking an acrylate monomer, methacrylic acid and acrylonitrile in a mass ratio of 75:5: 10; dissolving in acetone solution, adding dimethyl azodiisobutyrate at 10 ℃, heating to 52 ℃, reacting for 3h, cooling, and vacuum drying to obtain a substance A; dissolving nano silicon nitride in an acetone solution, adding the substance A, stirring, reacting at 115 ℃ for 2.5 hours, and drying in vacuum to obtain a substance B;
ultrasonically dispersing the substance B and the hydroxyl-terminated butadiene-acrylonitrile rubber powder in an acetone solution, reacting at 52 ℃ for 30min, filtering and drying to obtain a substance C;
dissolving bisphenol A epoxy resin and allyl glycidyl ether in absolute ethyl alcohol, and heating to 70 ℃ to form epoxy resin solution; dissolving the substance C and the propyl trimethoxy silane in a xylene solvent to form a solution D; dropwise adding the solution D into an epoxy resin solution, reacting for 4 hours at the temperature of 190 ℃, cooling, filtering, and drying in vacuum to obtain modified epoxy resin;
(2) mixing and stirring to prepare a finished product of the high-pressure-bearing plugging agent for the oil production casing; uniformly mixing the modified epoxy resin, the solid particles and the coupling agent, dispersing at a high speed, adding a curing agent and a curing regulator at a rotating speed of 3000r/min, filtering, drying and grinding to obtain the high-pressure-bearing plugging agent for the oil production casing.
Comparative example 3
A high pressure-bearing plugging agent for an oil extraction casing comprises the following raw material components; 60 parts of epoxy resin, 27 parts of solid particles, 21 parts of curing agent, 17 parts of coupling agent and 1.2 parts of curing regulator.
The solid particles are formed by mixing bentonite and attapulgite, and the mass ratio of the bentonite to the attapulgite is 3: 1.
A processing technology of a high pressure-bearing plugging agent for an oil extraction casing comprises the following steps
Uniformly mixing epoxy resin, solid particles and a coupling agent, dispersing at a high speed of 3000r/min, adding a curing agent and a curing regulator, filtering, drying and grinding to obtain the high-pressure-bearing plugging agent for the oil production casing.
Comparative analysis of experiments
In order to more intuitively prove the beneficial effects of the technical scheme of the invention, a comparison experiment is carried out on the technical scheme of the invention and the prior art; the embodiment 1-3 is the technical scheme of the invention;
comparative example 1 uses a modified epoxy resin without the MOFs material and the other steps are the same as example 3.
In comparative example 2, a MOFs-epoxy resin was used, which is different from the MOFs-epoxy resin in example 3; the other steps are the same as in example 3;
in comparative example 3, epoxy resin was used without the MOFs material, and the other steps were the same as in example 3.
Pressure bearing capacity experiment: preparing 6 groups of same cement sand slurry; sealing and maintaining for 24 h; plugging agent powders prepared in examples 1 to 3 and comparative examples 1 to 3 were added thereto, respectively; stirring uniformly, heating to 75 ℃, and carrying out curing reaction; cutting out a 8 mm-12 mm wedge-shaped test piece from each group of the obtained cured materials; the pressure bearing capacity of the wedge-shaped test piece is measured by using a high-temperature high-pressure leak stoppage instrument, and the test data are shown in the following table 1;
| example 1 | Example 2 | Example 3 | Comparative example 1 | Comparative example 2 | Comparative example 3 | |
| Pressure bearing value Mpa | 8.5 | 8.5 | 8.7 | 4.4 | 4.0 | 2.8 |
TABLE 1
As can be seen from the data in Table 1, the bearing values of examples 1 to 3 are greater than those of comparative examples 1 to 3; the pressure bearing value of the comparative example 1 is larger than that of the comparative example 3, which shows that the mechanical strength and the toughness of the epoxy resin modified by the nano silicon nitride and the hydroxyl-terminated butadiene-acrylonitrile rubber powder are superior to those of the common epoxy resin; and the pressure bearing value of the comparative example 2 is larger than that of the comparative example 3, which shows that the MOFs can enhance the pressure bearing capacity of the plugging agent. In conclusion, the plugging agent prepared by the invention has excellent pressure bearing capacity of the cured substance formed by plugging.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Claims (10)
1. The high-pressure-bearing plugging agent for the oil extraction casing is characterized by comprising the following components in parts by weight: the high-pressure-bearing leak stopping agent for the oil recovery casing comprises the following raw material components; 48-60 parts of MOFs-modified epoxy resin, 23-27 parts of solid particles, 17-21 parts of curing agent, 13-17 parts of coupling agent and 0.7-1.2 parts of curing regulator.
2. The high pressure-bearing plugging agent for the oil production casing according to claim 1, which is characterized in that: the MOFs-modified epoxy resin is mainly prepared by carrying out multi-stage reaction on bisphenol A epoxy resin, nano silicon nitride, an acrylate monomer, methacrylic acid, acrylonitrile, hydroxyl-terminated butadiene-acrylonitrile rubber powder and an MOFs material; the MOFs material is one or more of Ni-MOF, Co-MOF and Fe-MOF.
3. The high pressure-bearing plugging agent for the oil production casing according to claim 1, which is characterized in that: the solid particles are formed by mixing bentonite and attapulgite, and the mass ratio of the bentonite to the attapulgite is 3: 1.
4. The high pressure-bearing plugging agent for the oil production casing according to claim 1, which is characterized in that: the curing agent is a polyamide or modified amine type curing agent.
5. The high pressure-bearing plugging agent for the oil production casing according to claim 1, wherein; the coupling agent is at least one of 3-glycidoxypropyltrimethoxysilane, propyltrimethoxysilane, trimethoxysilane, triethoxysilane, phenyltriethoxysilane, phenyltrimethoxysilane and diphenyldimethoxysilane;
the curing accelerator is at least one of 2-methylimidazole, 2-ethyl-4-methylimidazole, 2-phenylimidazole and tris- (dimethylaminomethyl) phenol.
6. The high pressure-bearing plugging agent for the oil production casing according to claim 2, which is characterized in that: the acrylate monomer is any one of methyl acrylate, ethyl acrylate, butyl acrylate and octyl acrylate.
7. A processing technology of a high pressure-bearing plugging agent for an oil extraction casing is characterized by comprising the following steps;
(1) preparing MOFs-modified epoxy resin;
(2) mixing and stirring to prepare the finished product of the high-pressure-bearing plugging agent for the oil production casing.
8. The processing technology of the high pressure-bearing plugging agent for the oil production casing according to claim 7 is characterized by comprising the following steps;
(1) dissolving an acrylate monomer, methacrylic acid and acrylonitrile in an acetone solution, adding dimethyl azodiisobutyrate, maintaining the pressure with nitrogen, reacting for 2.5-3h, cooling, and drying in vacuum to obtain a substance A; dissolving nano silicon nitride in an acetone solution, adding the substance A, stirring, reacting for 2-2.5h, and drying in vacuum to obtain a substance B;
ultrasonically dispersing the substance B and the hydroxyl-terminated butadiene-acrylonitrile rubber powder in an acetone solution, reacting for 25-30min, filtering, and drying to obtain a substance C;
dissolving bisphenol A epoxy resin and allyl glycidyl ether in absolute ethyl alcohol to form epoxy resin solution; dissolving the substance C and the propyl trimethoxy silane in a xylene solvent to form a solution D; dropwise adding the solution D into an epoxy resin solution, reacting for 3.5-4h, cooling, filtering, and drying in vacuum to obtain modified epoxy resin; adding deionized water and MOFs materials, and carrying out ultrasonic dispersion for 2-3 h; preparing MOFs-modified epoxy resin;
(2) uniformly mixing MOFs-modified epoxy resin, solid particles and a coupling agent, dispersing at a high speed, adding a curing agent and a curing regulator, filtering, drying and grinding to obtain the high-pressure-bearing plugging agent for the oil production casing.
9. The processing technology of the high pressure-bearing plugging agent for the oil production casing according to claim 8, characterized in that; comprises the following steps of (a) carrying out,
(1) taking an acrylate monomer, methacrylic acid and acrylonitrile in a mass ratio of 75:5: 10; dissolving in acetone solution, adding dimethyl azodiisobutyrate at 8-10 deg.C, heating to 48-52 deg.C, reacting for 2.5-3h, cooling, and vacuum drying to obtain substance A; dissolving nano silicon nitride in an acetone solution, adding the substance A, stirring, reacting at the temperature of 105-115 ℃ for 2-2.5h, and performing vacuum drying to obtain a substance B;
ultrasonically dispersing the substance B and the hydroxyl-terminated butadiene-acrylonitrile rubber powder in an acetone solution, reacting at 48-52 ℃ for 25-30min, filtering, and drying to obtain a substance C;
dissolving bisphenol A epoxy resin and allyl glycidyl ether in absolute ethyl alcohol, and heating to 63-70 ℃ to form epoxy resin solution; dissolving the substance C and the propyl trimethoxy silane in a xylene solvent to form a solution D; dropwise adding the solution D into an epoxy resin solution, reacting for 3.5-4h at the temperature of 185-190 ℃, cooling, filtering, and drying in vacuum to obtain modified epoxy resin; adding deionized water and MOFs materials, and carrying out ultrasonic dispersion for 2-3 h; preparing MOFs-modified epoxy resin;
(2) uniformly mixing the MOFs-modified epoxy resin prepared in the step (1), solid particles and a coupling agent, dispersing at a high speed at the rotating speed of 2500-.
10. The processing technology of the high pressure-bearing plugging agent for the oil production casing according to the claims 7-9, characterized in that; the obtained plugging agent is mixed with cement sand slurry, pumped into an oil production casing and solidified to play a plugging effect.
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