CN114316930A - High-temperature-resistant modified nano cobalt oxide plugging agent and oil-based drilling fluid - Google Patents
High-temperature-resistant modified nano cobalt oxide plugging agent and oil-based drilling fluid Download PDFInfo
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Abstract
The invention discloses a high-temperature-resistant modified nano cobalt oxide plugging agent and an oil-based drilling fluid, and belongs to the technical field of oil and gas field drilling. The blocking agent used by the oil-based drilling fluid is a high-temperature-resistant modified nano cobalt oxide blocking agent which is prepared by a step method, and the synthetic raw materials comprise nano cobalt oxyhydroxide (10-40nm), a silane coupling agent, a polyphenyl ring compound containing olefinic bonds, an alkenyl phenyl silane compound, a long-chain ester compound containing olefinic bonds, a cross-linking agent and an initiator. The high-temperature-resistant modified nano cobalt oxide plugging agent provided by the invention has the particle size distribution of 69-432nm, can effectively plug nano cracks, and enhances the stability of a well wall. In addition, compared with the similar plugging agent, the performance of the plugging agent is obviously improved, and the plugging agent has the advantage of high temperature resistance and can be used in deep wells and ultra-deep wells. The plugging agent can be directly added into oil-based drilling fluid, so that the drilling fluid can be prevented from invading stratum, well collapse accidents are prevented, and the stability of a well wall is enhanced.
Description
Technical Field
The invention relates to the technical field of oil and gas field drilling, in particular to a high-temperature-resistant modified nano cobalt oxide plugging agent and an oil-based drilling fluid
Background
In the process of developing petroleum and natural gas resources, borehole wall instability is always one of the common and difficult-to-solve problems in the drilling process. In the process of drilling, drilling fluid easily enters a stratum along tiny pores under the action of pressure difference, and propagates in the tiny cracks to cause crack expansion, so that the stability of a well wall is poor. The instability of the well wall not only can consume the drilling time and lose the drilling fluid, but also can cause a series of complex conditions such as drill sticking, well collapse and the like, even cause the abandonment of the well hole and cause great economic loss. Therefore, how to effectively block the crack becomes the key point of the study of scholars and experts in the field. In addition, for some hard brittle and fractured formations with bedding and nano-pore development, invasion of oil-based drilling fluid filtrate can contribute to formation instability. In addition, the transmission of hydraulic pressure through the nano-pores can also cause wellbore wall instability, and therefore, the plugging of the nano-pores by the oil-based drilling fluid must be enhanced.
At present, the plugging agent of the oil-based drilling fluid is few in types, the used plugging materials are mostly bridge plugs with only hydrophilic performance while drilling leakage-proof materials, the adaptability in the oil-based drilling fluid is poor, and the particle size matching capability is insufficient. Simultaneously, the change of pit shaft pressure can arouse the change of aperture size, and aperture dynamic deformation can lead to the fact the destruction to the shutoff layer, and the shutoff layer that inelastic plugging agent formed can not adapt to the aperture and warp, and this will influence the shutoff effect, compares in conventional rigid plugging agent, and elastic plugging agent can adapt to the aperture better and warp, and the shutoff effect is stable. The oil-based drilling fluid has the advantages of high temperature resistance, salt and calcium corrosion resistance, contribution to well wall stability, good lubricating property, small damage degree to an oil-gas layer and the like. Therefore, a plugging material suitable for the oil-based drilling fluid, namely a high-temperature-resistant modified nano cobalt oxide plugging agent, is researched. The lipophilic long chain is grafted on the basis of the modified nano cobalt oxide, so that the dispersing capacity and the adsorption capacity of the modified nano cobalt oxide can be improved, and the modified nano cobalt oxide can be well dispersed in the oil-based drilling fluid to improve the plugging performance of the oil-based drilling fluid in a nano pore; meanwhile, a filter membrane can be formed on the surface of the rock stratum, so that the invasion of liquid is reduced. The introduction of a plurality of benzene ring structures can improve the high-temperature resistance of the blocking agent.
Disclosure of Invention
Aiming at the problem of borehole wall instability caused by the fact that the conventional plugging agent cannot effectively plug nano cracks in the shale at present, the invention provides the high-temperature-resistant modified nano cobalt oxide plugging agent, the particle size of which is nano, and the high-temperature-resistant modified nano cobalt oxide plugging agent can effectively plug nano cracks in a shale stratum, so that the aim of stabilizing the borehole wall is fulfilled. And develops a high-temperature-resistant modified nano cobalt oxide plugging agent for the oil-based drilling fluid applicable to the shale stratum.
In order to achieve the purpose, the technical scheme of the invention is as follows: a high-temperature resistant modified nano cobalt oxide plugging agent. The raw materials of the high-temperature-resistant modified nano cobalt oxide blocking agent comprise nano cobalt oxyhydroxide (10-40nm), a silane coupling agent, a polycyclic compound containing olefinic bonds, an alkenyl phenylsilane compound, a long-chain ester compound containing olefinic bonds, a cross-linking agent and an initiator, and the preparation steps of the high-temperature-resistant modified nano cobalt oxide blocking agent are as follows:
s1, drying the nano cobalt oxyhydroxide in a vacuum drying oven at 55-65 ℃ for 10-12h, weighing 2-4g of nano cobalt oxyhydroxide, adding 250-500ml of absolute ethyl alcohol, performing ultrasonic dispersion for 20-30min, then dropwise adding 6-12g of silane coupling agent while stirring, adjusting the pH to 3, performing magnetic stirring reaction for 12h at 60 ℃, washing for 3-5 times by using the absolute ethyl alcohol and pure water, and finally drying and grinding to obtain the silane coupling agent modified nano cobalt oxide;
s2, adding 0.1-0.12mol of modified nano cobalt oxide into a reactor, adding ultrapure water for ultrasonic dispersion for 10-15min, putting the dispersion liquid into the reactor, introducing nitrogen for 20-30min, adding 0.025-0.1mol of polycyclic compound containing olefinic bond, 0.04-0.12mol of alkenylphenylsilane compound, 0.05-0.13mol of long-chain ester compound containing olefinic bond and 0.02mol of cross-linking agent, stirring and reacting for 4-5h at 70-80 ℃, adding initiator ammonium persulfate, stirring and reacting for 8-12h at 70-80 ℃, cooling the system to 20-25 ℃ after the reaction is finished, washing the prepared sample to be neutral by distilled water, drying at 60-70 ℃ in a drying oven, obtaining the high-temperature-resistant modified nano cobalt oxide blocking agent after drying, grinding the dried sample, and sealing and storing.
The silane coupling agent is one of 3- (methacryloyloxy) propyl trimethoxy silane, acryloxymethyl trimethoxy silane and methacryloxymethyl triethoxy silane.
The polycyclic compound containing olefinic bonds is one of 2, 4, 6-triphenyl-1-hexene, 1-vinyl-4- [ tri (4-vinyl phenyl) methyl ] benzene and 1, 1, 4, 4-tolyl-1, 3-butadiene.
The alkenyl phenylsilane compound is one of (tri-2-propylene-1-silyl) -benzene, triphenyl allylsilane and vinyl triphenyl silane.
The long-chain ester compound containing the polyene bond is one of 1, 10-decanediol diacrylate, neopentyl glycol diacrylate, ethylene glycol dimethacrylate and 2-butene-1, 4-dimethacrylate.
The cross-linking agent is N, N-methylene bisacrylamide.
The invention also aims to provide an oil-based drilling fluid, which is added with the high-temperature-resistant modified nano cobalt oxide plugging agent.
The drilling fluid comprises the following components in parts by weight: 250 parts of 200-organic-material white oil, 3-4 parts of a main emulsifier, 9-10 parts of an auxiliary emulsifier, 3-4 parts of a wetting agent, 0.5-1 part of a shear promoter, 7-8 parts of organic soil, 24-26 parts of calcium oxide, 28-32 parts of a fluid loss additive, 500 parts of barite powder and 5-15 parts of a high-temperature-resistant modified nano cobalt oxide plugging agent.
The particle size range of the high-temperature-resistant modified nano cobalt oxide plugging agent prepared by the invention is between 69 and 432nm, and the high-temperature-resistant modified nano cobalt oxide plugging agent can enter tiny cracks of a shale well wall, so that the tiny and nano-scale cracks are effectively plugged, and the effect of stabilizing the well wall is achieved; and a benzene ring structure is introduced into the blocking agent, so that the blocking agent has better high-temperature resistance. The oil-based drilling fluid used in the invention has good performances in the aspects of rheological property, stability, plugging property and the like under the condition of shale formation.
Drawings
FIG. 1 is a particle size distribution diagram of the high temperature resistant modified nano cobalt oxide plugging agent in the first example;
FIG. 2 is a particle size distribution diagram of the high temperature resistant modified nano cobalt oxide plugging agent in example two;
FIG. 3 is a particle size distribution diagram of the high temperature resistant modified nano cobalt oxide plugging agent in example three.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the following embodiments of the present invention, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the 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.
In the present examples, the parts are all parts by weight unless otherwise specified.
Synthesis of high-temperature-resistant modified nano cobalt oxide plugging agent
Example 1:
s1, placing the nano cobalt oxyhydroxide in a 65 ℃ vacuum drying oven for drying for 12h, accurately weighing 2g of nano cobalt oxyhydroxide, adding 250ml of absolute ethyl alcohol, carrying out ultrasonic dispersion for 20min, then dropwise adding 6g of 3- (methacryloyloxy) propyl trimethoxy silane while stirring, adjusting the pH to about 3, carrying out magnetic stirring reaction for 12h at the temperature of 60 ℃, washing for 4 times by using absolute ethyl alcohol and pure water, and finally drying and grinding to obtain the silane coupling agent modified nano cobalt oxide;
s2, adding 0.12mol of modified nano cobalt oxide into a reactor, adding ultrapure water for ultrasonic dispersion for 10min, putting a dispersion liquid into the reactor, introducing nitrogen for 20min, adding 0.01mol of 2, 4, 6-triphenyl-1-hexene, 0.04mol of (tri-2-propen-1-ylsilyl) -benzene, 0.05mol of 1, 10-decanediol diacrylate and 0.02mol of N, N-methylene bisacrylamide, stirring and reacting for 4h at 80 ℃, adding an initiator ammonium persulfate, stirring and reacting for 12h at 80 ℃, cooling the system to 25 ℃ after the reaction is finished, washing the prepared sample to be neutral by using distilled water, drying at 70 ℃ in a drying box, obtaining a high-temperature resistant modified nano cobalt oxide sealing agent after drying, grinding the dried sample, and sealing and storing.
Example 2:
s1, placing the nano cobalt oxyhydroxide in a 65 ℃ vacuum drying oven for drying for 10h, accurately weighing 2g of nano cobalt oxyhydroxide, adding 500ml of absolute ethyl alcohol, ultrasonically dispersing for 30min, then dropwise adding 6g of acryloxymethyl trimethoxy silane while stirring, adjusting the pH to about 3, magnetically stirring and reacting for 12h at the temperature of 60 ℃, washing for 3-5 times by using the absolute ethyl alcohol and pure water, and finally drying and grinding to obtain the silane coupling agent modified nano cobalt oxide;
s2, adding 0.1mol of modified nano cobalt oxide into a reactor, adding ultrapure water for ultrasonic dispersion for 15min, taking a dispersion liquid, placing the dispersion liquid into the reactor, introducing nitrogen for 30min, adding 0.025mol of 1-vinyl-4- [ tri (4-vinylphenyl) methyl ] benzene, 0.12mol of triphenylallylsilane, 0.05mol of neopentyl glycol diacrylate and 0.02mol of N, N-methylene bisacrylamide, stirring and reacting for 5h at 80 ℃, adding an initiator ammonium persulfate, stirring and reacting for 10h at 80 ℃, cooling the system to 25 ℃ after the reaction is finished, washing the prepared sample to be neutral by using distilled water, drying at 70 ℃ in a drying box, obtaining a high-temperature-resistant modified nano cobalt oxide blocking agent after drying, grinding the dried sample, and sealing and storing.
Example 3:
s1, placing the nano cobalt oxyhydroxide in a vacuum drying oven at 60 ℃ for drying for 12h, accurately weighing 4g of nano cobalt oxyhydroxide, adding 500ml of absolute ethyl alcohol, ultrasonically dispersing for 30min, then dropwise adding 12g of methacryloxymethyl triethoxysilane while stirring, adjusting the pH to about 3, magnetically stirring and reacting for 12h at 60 ℃, washing for 5 times by using absolute ethyl alcohol and pure water, and finally drying and grinding to obtain silane coupling agent modified nano cobalt oxide;
s2, adding 0.12mol of modified nano cobalt oxide into a reactor, adding ultrapure water for ultrasonic dispersion for 15min, putting a dispersion liquid into the reactor, introducing nitrogen for 30min, adding 0.05mol of 1, 1, 4, 4-tolyl-1, 3-butadiene, 0.04-0.12mol of vinyl triphenylsilane, 0.05mol of ethylene glycol dimethacrylate and 0.02mol of N, N-methylene bisacrylamide, stirring and reacting for 5h at 80 ℃, adding an initiator ammonium persulfate, stirring and reacting for 12h at 70 ℃, cooling the system to 25 ℃ after the reaction is finished, washing the prepared sample to be neutral by using distilled water, drying in a drying box at 70 ℃, obtaining a high-temperature-resistant modified nano cobalt oxide blocking agent after drying, grinding the dried sample, and sealing and storing.
Secondly, preparing the oil-based drilling fluid:
the invention is mainly illustrated by the following application mode of a specific formula to resist the high-temperature modified nano cobalt oxide plugging agent. The specific formula is based on 225 parts by mass of base oil and comprises the following components: 3# white oil, a main emulsifier TYDFF-301, an auxiliary emulsifier TYDFF-401, a wetting agent TYDFF-501, a cutting extraction agent TYDFF-701, organic soil TYDFF-601, a filtrate reducer TYDFF-101, 30% of a calcium chloride solution, calcium oxide TYDFF-801, barite powder and a high-temperature-resistant modified nano cobalt oxide plugging agent.
The concrete preparation process is as follows
225mL of 3# white oil is simply taken, added into a 1000mL stirring cup, then added with 3.75g of main emulsifier TYDDF-301, 10.00g of auxiliary emulsifier TYDDF-401, 3.25g of wetting agent TYDDF-501 and 0.75g of cutting agent TYDDF-701, stirred at 12000r/min at a high speed for 10min, then added with 7.50g of organic soil TYDDF-601, stirred at 12000r/min at a high speed for 10min, slowly added with 25mL of calcium chloride aqueous solution (the calcium chloride has a mass percent concentration of 30 percent), and stirred at a high speed for 20 min; adding 7.5g of calcium oxide TYDF-801 and 15g of fluid loss additive TYDF-101, stirring at high speed for 20min, adding 500g of barite, stirring at high speed for 30min to obtain base slurry of oil-based drilling fluid with density of 2g/cm3。
4 parts of the same base slurry is prepared according to the slurry preparation, and 0 part by weight, 3 parts by weight, 6 parts by weight and 9 parts by weight of the high-temperature resistant modified nano cobalt oxide plugging agent are respectively added to prepare 4 parts of drilling fluid with different addition amounts of the high-temperature resistant modified nano cobalt oxide plugging agent. In order to further illustrate the effects of the high-temperature-resistant modified nano cobalt oxide plugging agent and the oil-based drilling fluid, the high-temperature-resistant modified nano cobalt oxide plugging agent prepared in the examples 1, 2 and 3 and the oil-based drilling fluid were subjected to performance tests.
Third, performance test
1. Particle size test of high-temperature-resistant modified nano cobalt oxide plugging agent
The particle size of the high temperature resistant modified nano cobalt oxide plugging agent prepared in example 1 is shown in fig. 1, the particle size of the high temperature resistant modified nano cobalt oxide plugging agent prepared in example 2 is shown in fig. 2, and the particle size of the high temperature resistant modified nano cobalt oxide plugging agent prepared in example 3 is shown in fig. 3. As can be seen from the figures 1, 2 and 3, the particle size range of the high-temperature-resistant modified nano cobalt oxide plugging agent is between 69 and 432nm, and the high-temperature-resistant modified nano cobalt oxide plugging agent can effectively plug the nano cracks of the shale.
2. Plugging experiment of artificial rock core
The method comprises the steps of simulating a micro-crack stratum and a nano-crack stratum of the stratum by using an artificial rock core, measuring the average flow of a drilling fluid system in the artificial rock core, and calculating the permeability K of the artificial rock core which is Q [ mu ] L/(A [ delta ] P) before and after adding the high-temperature resistant modified nano cobalt oxide with different mass fractions by using a Darcy formula, so that the blocking rate of the high-temperature resistant modified nano cobalt oxide on the artificial rock core is calculated, and the blocking performance of the artificial rock core is evaluated. Table 1 shows a table of the plugging effect of the high temperature resistant modified nano cobalt oxide on the artificial core. The plugging rate is (initial permeability-permeability after plugging)/initial permeability x 100%.
The results shown in table 1 show that, compared with the base slurry without the high temperature resistant modified nano cobalt oxide plugging agent, the plugging rate of the core is increased after the high temperature resistant modified nano cobalt oxide is added in different proportions, which indicates that the high temperature resistant modified nano cobalt oxide plugging agent can effectively plug the micropore gap and further prevent the drilling fluid from entering the core. The plugging effect is better along with the increase of the addition of the high-temperature-resistant modified nano cobalt oxide plugging agent, and when the addition of the high-temperature-resistant modified nano cobalt oxide plugging agent is 3%, the plugging effect is best, and the plugging rates of the rock core are respectively 89.12%, 89.06% and 90.72%, which shows that the high-temperature-resistant modified nano cobalt oxide plugging agent can effectively plug the microcracks, so that the drilling fluid is prevented from entering the rock core.
Table 1 drilling fluid plugging core plugging experiment recording table
Note: the core length was 5cm and the diameter 2.5 cm.
3. Drilling fluid rheological property and water loss wall-building property test
Part 2 of the oil and gas industry drilling fluid field test according to standard GB/T16783.2-2012: oil-based drilling fluid, the rheological property and water loss wall building property of the drilling fluid before and after aging of the drilling fluid prepared in the step (a), are respectively tested, and the results are recorded in table 2.
From the results shown in table 2, it can be seen that, compared with the drilling fluid without adding the high temperature resistant modified nano cobalt oxide plugging agent, when the addition amount of the high temperature resistant modified nano cobalt oxide plugging agent in the drilling fluid is 9 parts by mass, the performance of the drilling fluid is not significantly affected, which indicates that the drilling fluid plugging agent has good compatibility. And the oil-based drilling fluid has higher rock carrying capacity under lower viscosity, and meanwhile, the flushing effect on the well wall is smaller, so that the oil-based drilling fluid has good rheological property. In addition, compared with the performance of the base slurry, the high-temperature and high-pressure filtration loss of the oil-based drilling fluid in all the embodiments is reduced, which shows that the high-temperature-resistant modified nano cobalt oxide plugging agent has good rheological property and water loss wall-building property, can effectively reduce the high-temperature and high-pressure filtration loss of the drilling fluid, can provide good plugging property even in a high-temperature environment, effectively prevents filtrate from entering a stratum and improves the stability of a well wall.
TABLE 2 drilling fluid Performance Table
Injecting AV-apparent viscosity with unit of mPa.s; PV-plastic viscosity in mPa · s; YP-dynamic shear force with unit of Pa; API I normal temperature medium pressure filtration loss, the unit is mL; HTHP-high temperature high pressure fluid loss in mL.
Although the present invention has been described with reference to a preferred embodiment, it should be understood that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (9)
1. The synthesis of the high-temperature-resistant modified nano cobalt oxide plugging agent and the oil-based drilling fluid are characterized in that the high-temperature-resistant modified nano cobalt oxide plugging agent is prepared from the following raw materials of nano cobalt oxyhydroxide (10-40nm), a silane coupling agent, a polyphenyl ring compound containing olefinic bonds, an alkenyl phenyl silane compound, a long-chain ester compound containing olefinic bonds, a crosslinking agent and an initiator by the following steps:
s1, drying the nano cobalt oxyhydroxide in a vacuum drying oven at 55-65 ℃ for 10-12h, weighing 2-4g of nano cobalt oxyhydroxide, adding 250-500ml of absolute ethyl alcohol, performing ultrasonic dispersion for 20-30min, then dropwise adding 6-12g of silane coupling agent while stirring, adjusting the pH to about 3, performing magnetic stirring reaction for 12h at 60 ℃, washing for 3-5 times by using the absolute ethyl alcohol and pure water, and finally drying and grinding to obtain the silane coupling agent modified nano cobalt oxide;
s2, adding 0.1-0.12mol of modified nano cobalt oxide into a reactor, adding ultrapure water for ultrasonic dispersion for 10-15min, putting the dispersion liquid into the reactor, introducing nitrogen for 20-30min, adding 0.025-0.1mol of polycyclic compound containing olefinic bond, 0.04-0.12mol of alkenylphenylsilane compound, 0.05-0.13mol of long-chain ester compound containing olefinic bond and 0.02mol of cross-linking agent, stirring and reacting for 4-5h at 70-80 ℃, adding initiator ammonium persulfate, stirring and reacting for 8-12h at 70-80 ℃, cooling the system to 20-25 ℃ after the reaction is finished, washing the prepared sample to be neutral by distilled water, drying at 60-70 ℃ in a drying oven, obtaining the high-temperature-resistant modified nano cobalt oxide blocking agent after drying, grinding the dried sample, and sealing and storing.
2. The high temperature resistant modified nano cobalt oxide blocking agent according to claim 1, wherein the silane coupling agent is one of 3- (methacryloyloxy) propyltrimethoxysilane, acryloxymethyltrimethoxysilane, and methacryloxymethyltriethoxysilane.
3. The high temperature resistant modified nano cobalt oxide blocking agent according to claim 1, characterized in that the olefinic bond-containing polycyclic compound is one of 2, 4, 6-triphenyl-1-hexene, 1-vinyl-4- [ tris (4-vinylphenyl) methyl ] benzene, 1, 4, 4-tolyl-1, 3-butadiene.
4. The high temperature resistant modified nano cobalt oxide blocking agent according to claim 1, wherein the alkenylphenylsilane compound is one of (tri-2-propen-1-ylsilyl) -benzene, triphenylallylsilane, and vinyltriphenylsilane.
5. The high temperature resistant modified nano cobalt oxide blocking agent according to claim 1, characterized in that the long chain ester compound containing multiple olefinic bonds is one of 1, 10-decanediol diacrylate, neopentyl glycol diacrylate, ethylene glycol dimethacrylate, 2-butene-1, 4-dimethacrylate.
6. The high temperature resistant modified nano cobalt oxide plugging agent according to claim 1, characterized in that the cross-linking agent is N, N-methylene bisacrylamide.
7. An oil-based drilling fluid, which is characterized in that the high-temperature-resistant modified nano cobalt oxide plugging agent as claimed in any one of claims 1 to 6 is added into the drilling fluid.
8. The oil-based drilling fluid of claim 7, wherein the drilling fluid comprises the following components in parts by weight: 250 parts of white oil 200-.
9. The oil-based drilling fluid of claim 8, wherein the white oil is # 3 white oil, the primary emulsifier is TYODF-301, the secondary emulsifier is TYODF-401, the wetting agent is TYODF-501, the shear enhancing agent is TYODF-701, the organic soil is TYODF-601, the calcium oxide is TYODF-801, the fluid loss additive is TYODF-101, the weighting agent is barite powder, the blocking agent is a high temperature resistant modified nano cobalt oxide blocking agent, and the component code is from kyuxi hua wei science and technology limited.
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