CN114350329B - High-temperature-resistant intercalation modified nano titanium carbide composite plugging agent and oil-based drilling fluid - Google Patents
High-temperature-resistant intercalation modified nano titanium carbide composite plugging agent and oil-based drilling fluid Download PDFInfo
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Abstract
The invention discloses a high-temperature-resistant intercalation modified nano titanium carbide composite plugging agent and oil-based drilling fluid. The high-temperature resistant intercalation modified nano titanium carbide composite plugging agent comprises nano titanium carbide (50 nm), p-dodecyl styrene, a hexadecyl acrylate compound, a vinyl naphthene compound, an intercalating agent, a crosslinking agent and an initiator; the drilling fluid comprises the high-temperature-resistant intercalation modified nano titanium carbide composite plugging agent. The high-temperature-resistant intercalation modified nano titanium carbide composite plugging agent is used as a nano plugging agent, has the particle size distribution of 90-330nm, and can effectively plug nano-sized pores in a shale well wall, so that the well wall can be effectively stabilized and collapse can be prevented, and meanwhile, the preparation method is reliable in principle and has a wide market prospect; the oil-based drilling fluid used by the invention has good rheological property, stability, plugging property and other properties under the condition of the shale stratum.
Description
Technical Field
The invention relates to the technical field of drilling of oil and gas fields, in particular to synthesis of a high-temperature-resistant intercalation modified nano titanium carbide composite plugging agent and oil-based drilling fluid containing the plugging agent.
Background
The oil-based drilling fluid is drilling fluid taking oil as a continuous phase, and compared with the water-based drilling fluid, the oil-based drilling fluid has the advantages of high temperature resistance, salt and calcium invasion resistance, contribution to well wall stability, better lubricity, less damage degree to oil and gas layers and the like, achieves excellent effects in various complex stratum at present, and has wider application prospect.
In recent years, the exploitation force of Chinese unconventional oil gas is continuously increased, and the drilling difficulty is continuously increased. Although oil-based drilling fluid is widely used in shale gas development, the problem of instability of the well wall caused by liquid phase pressure transmission cannot be effectively solved, and accidents of drilling and instrument clamping occur. How to improve the plugging effect of the oil-based drilling fluid, reduce the filtration loss of the drilling fluid, improve the stability of the well wall, is a difficult point and a concern in the research field of the oil-based drilling fluid, and is the development of the plugging agent of the oil-based drilling fluid. The existing plugging agent has good plugging effect on shale stratum with cracks or bedding development in the aspect of plugging nanoscale pores, but the plugging effect is needed to be further improved in the aspect of plugging nanoscale pores. Therefore, aiming at the problem of unstable well wall caused by the fact that nanoscale pores in shale cannot be effectively blocked, the synthesis of the blocking agent with nanoscale to improve the blocking effect of the oil-based drilling fluid is a good choice.
Disclosure of Invention
Aiming at the problem of instability of the well wall caused by the fact that the conventional plugging agent cannot effectively plug nano-pore seams in the shale at present, the invention provides the high-temperature-resistant intercalation modified nano-titanium carbide composite plugging agent, the particle size of which is nano-scale, and the nano-pore seams in the shale stratum can be effectively plugged, so that the aim of stabilizing the well wall is fulfilled.
In order to achieve the above purpose, the technical scheme of the invention is as follows: the raw materials of the high-temperature-resistant intercalation modified nano titanium carbide composite plugging agent are nano titanium carbide (50 nm), p-dodecyl styrene, a hexadecyl acrylate compound, a vinyl naphthene compound, an intercalation agent, a crosslinking agent and an initiator, and the preparation steps of the high-temperature-resistant intercalation modified nano titanium carbide composite plugging agent are as follows:
vacuum drying nanometer titanium carbide at 60-70 deg.c, adding nanometer titanium carbide into deionized water dispersion for ultrasonic dispersion, adding intercalation agent while stirring, reaction at 40-50 deg.c, cooling to room temperature, centrifuging, ultrasonic dispersion, suction filtering, washing to obtain intercalation modified nanometer titanium carbide, ultrasonic dispersion of the obtained intercalation modified nanometer titanium carbide with deionized water, introducing nitrogen gas for 20-30min, adding co-monomer p-dodecyl styrene, cetyl acrylate compound and vinyl naphthene compound into the reactor, regulating pH value of the system to 6.5-7.5 with 20-25% concentration NaOH water solution, heating to 60-70 deg.c, adding crosslinking agent and initiator for reaction for 4-5 hr, cooling to room temperature, washing the prepared sample with distilled water to neutrality, vacuum drying at 50-60 deg.c, and grinding to obtain the high temperature resisting intercalation modified nanometer titanium carbide composite plugging agent.
The intercalation agent is one of tetramethyl ammonium hydroxide (TMAH) and dimethyl sulfoxide (DMSO);
the hexadecyl acrylate compound is one of hexadecyl acrylate and hexadecyl methacrylate;
the vinyl cycloalkane compound is one of vinyl cyclopentane, vinyl cyclohexane and vinyl cyclooctane;
the cross-linking agent is one of N, N-Methylene Bisacrylamide (MBA) and dicyclopentadiene acrylic acid ester (DCPA);
the initiator is one of ammonium persulfate and potassium persulfate;
the molar mass ratio of the intercalation modified nano titanium carbide to the dodecyl styrene, the hexadecyl acrylate compound and the vinyl naphthene compound is 2:2:1:3;
the adding amount of the cross-linking agent is 1% -3% of the total weight of the four monomers, namely intercalation modified nano titanium carbide, p-dodecyl styrene, cetyl acrylate compounds and vinyl naphthenes compounds;
the addition amount of the initiator is 1-3% of the total weight of the four monomers of the intercalation modified nano titanium carbide, methyl-dodecyl styrene, hexadecyl acrylate compounds and vinyl naphthene compounds.
The invention further aims to provide an oil-based drilling fluid, which is added with the first high-temperature-resistant intercalation modified nano titanium carbide composite plugging agent.
The drilling fluid comprises the following components in parts by weight: 225-227 parts of 3# white oil, 3.6-3.8 parts of main emulsifier TYODF-301, 9.8-10.2 parts of auxiliary emulsifier TYODF-401, 3.2-3.3 parts of wetting agent TYODF-501, 0.7-0.8 part of cutting agent TYODF-701, 7-8 parts of organic soil TYODF-601, 14.5-15.5 parts of filtrate reducer TYODF-101, 24-26 parts of 25-35% calcium chloride solution, 7.3-7.7 parts of calcium oxide TYODF-801, 1.25-3.75 parts of high-temperature resistant intercalation modified nano titanium carbide composite plugging agent, 250-600 parts of barite powder and 1.5-2.2g/cm < 3 >.
The invention has the following beneficial effects:
the particle size of the high-temperature-resistant intercalation modified nano titanium carbide composite plugging agent prepared by the invention is distributed between 90 and 330nm, so that the nano-pore seams in the shale stratum can be effectively plugged, and the effect of stabilizing the well wall is achieved; the oil-based drilling fluid used by the invention has good rheological property, stability, plugging property and other properties under the condition of the shale stratum.
Drawings
FIG. 1 is a graph showing the particle size distribution of a modified nano titanium carbide composite plugging agent with high temperature intercalation resistance in the first embodiment;
FIG. 2 is a graph showing the particle size distribution of a modified nano titanium carbide composite plugging agent with high temperature intercalation resistance in a second embodiment.
Detailed Description
The technical solutions of the present invention will be clearly and completely described in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
In this example, unless otherwise specified, the parts are parts by weight.
1. Synthesizing the high-temperature resistant intercalation modified nano titanium carbide composite plugging agent:
example 1:
vacuum drying 0.60g of nano titanium carbide at 65 ℃, adding the dried nano titanium carbide into 50ml of deionized water dispersion liquid for ultrasonic dispersion for 30min, then dropwise adding 10% dimethyl sulfoxide for 30ml while stirring, then placing the mixture at 45 ℃ for reaction, cooling to room temperature, centrifugally separating, performing ultrasonic dispersion, suction filtration and washing to obtain intercalation modified nano titanium carbide, then placing the obtained intercalation modified nano titanium carbide into a reactor for ultrasonic dispersion by 60ml of deionized water, introducing nitrogen for 20-30min, adding 2.72g of p-dodecyl styrene, 1.48g of hexadecyl acrylate and 1.44g of vinyl cyclopentane into the reactor, regulating the pH value of the system to 6.5 by using 22% NaOH aqueous solution, heating to 60 ℃, then adding 0.13g of dicyclopentadiene acrylic ester and 0.13g of potassium persulfate for reaction for 4h, cooling to room temperature after the reaction is finished, washing the prepared sample to neutrality by distilled water, then placing the sample into a 55 ℃ for vacuum drying, and carrying out high temperature anti-baking on the sample to obtain the intercalation modified nano titanium carbide composite plugging agent.
Example 2:
vacuum drying 0.90g of nano titanium carbide at 65 ℃, adding the dried nano titanium carbide into 75ml of deionized water dispersion liquid for ultrasonic dispersion for 30min, then dropwise adding 10% dimethyl sulfoxide for 45ml while stirring, then placing the mixture at 45 ℃ for reaction, cooling to room temperature, centrifugally separating, performing ultrasonic dispersion, suction filtration and washing to obtain intercalation modified nano titanium carbide, then placing the obtained intercalation modified nano titanium carbide into a reactor for ultrasonic dispersion by 90ml of deionized water, introducing nitrogen for 20-30min, adding 4.08g of p-dodecyl styrene, 2.32g of hexadecyl methacrylate and 2.48g of vinyl cyclohexane into the reactor, adjusting the pH value of the system to 6.5 by using 22% NaOH aqueous solution, heating to 60 ℃, adding 0.20g of dicyclopentadiene acrylate and 0.20g of potassium persulfate for reaction for 4h, cooling to room temperature after the reaction is finished, washing the prepared sample to neutrality by distilled water, placing the obtained sample into a 55 ℃ for vacuum drying, and grinding the dried sample to obtain the high-temperature-resistant nano titanium carbide composite plugging agent.
2. Preparing oil-based drilling fluid:
the invention mainly describes an application mode of the high-temperature intercalation-resistant modified nano titanium carbide composite plugging agent by using the following specific formula. The specific base stock formulation based on 225 parts by weight of base oil is: 225 parts of 3# white oil+3.75 parts of main emulsifier TYODF-301+10.00 parts of auxiliary emulsifier TYODF-401+3.25 parts of wetting agent TYODF-501+0.75 part of cutting agent TYODF-701+7.50 parts of organic soil TYODF-601+25 parts of 30% calcium chloride solution+7.5 parts of calcium oxide TYODF-801+15 parts of filtrate reducer TYODF-101+500 parts of barite powder.
The specific preparation process is as follows
Taking 225mL of 3# white oil, adding the white oil into a 1000mL stirring cup, adding 3.75g of a main emulsifier TYODF-301, 10.00g of a auxiliary emulsifier TYODF-401,3.25g of a wetting agent TYODF-501 and 0.75g of a cutting agent TYODF-701, stirring at a high speed of 12000r/min for 10min, adding 7.50g of organic soil TYODF-601, stirring at a high speed of 12000r/min for 10min, slowly adding 25mL of a calcium chloride aqueous solution (the mass percentage concentration of calcium chloride is 30%), and stirring at a high speed for 20min; adding 7.5g of calcium oxide TYODF-801 and 15g of filtrate reducer TYODF-101, stirring at high speed for 20min, and continuously adding 500g of barite, stirring at high speed for 30min to obtain base slurry of oil-based drilling fluid, wherein the density of the prepared drilling fluid is 2.0g/cm 3 。
4 parts of the same base slurry is prepared according to the slurry preparation, wherein 1.25g, 2.5g and 3.75g of the high-temperature-resistant intercalation modified nano titanium carbide composite plugging agent are respectively added into 3 parts of the base slurry, and different oil-based drilling fluids with the plugging agent ranging from 0.5% to 1.5% can be prepared, and in order to further illustrate the effects of the high-temperature-resistant intercalation modified nano titanium carbide composite plugging agent and the oil-based drilling fluid, the high-temperature-resistant intercalation modified nano titanium carbide composite plugging agent and the oil-based drilling fluid prepared in the embodiment 1 and the embodiment 2 are subjected to performance test.
1. Particle size test of high-temperature-resistant intercalation modified nano titanium carbide composite plugging agent
The particle size test of the high temperature intercalation modified nano titanium carbide composite plugging agent is carried out by using a BI-200SM type laser scatterometer produced by Bruce Hai instruments, america, and the particle size test results of the high temperature intercalation modified nano titanium carbide composite plugging agent prepared in the two examples are shown in figures 1 and 2 respectively. The high-temperature resistant intercalation modified nano titanium carbide composite plugging agent has a plurality of different nano-sizes from 90-330nm, has wide particle size distribution, and can be used for plugging different nano-pore seams.
2. Drilling fluid plugging performance test
The method comprises the steps of simulating a stratum nano-pore stratum by using an artificial rock core, measuring the average flow of a drilling fluid system in the artificial rock core, calculating the permeability of the artificial rock core before and after adding the high-temperature-resistant intercalation modified nano-titanium carbide composite plugging agent by a Darcy formula, and calculating the plugging rate of the high-temperature-resistant intercalation modified nano-titanium carbide composite plugging agent on the artificial rock core, so that the plugging performance of the artificial rock core is evaluated, and the plugging effect of the high-temperature-resistant intercalation modified nano-titanium carbide composite plugging agent on the artificial rock core is shown in Table 1. As shown in Table 1, the high temperature resistant intercalation modified nano titanium carbide composite plugging agent can effectively reduce the permeability of the artificial rock core, has good plugging effect, and when the addition amount of the high temperature resistant intercalation modified nano titanium carbide composite plugging agent is 0.5%, the permeability of the rock core is respectively reduced by 86.0% and 86.3%, and the plugging effect is better along with the increase of the addition amount of the high temperature resistant intercalation modified nano titanium carbide composite plugging agent, and when the addition amount exceeds 0.5%, the permeability is still reduced, but the reduction is hardly obvious, so that the optimal addition amount of the high temperature resistant intercalation modified nano titanium carbide composite plugging agent is 0.5%.
Table 1 artificial core plugging test chart
| Name of the name | Artificial core permeability/10 -3 mD | Plugging rate% |
| Base slurry | 6.79 | / |
| Base stock +0.5% example 1 | 0.95 | 86.0 |
| Base stock +0.5% example 2 | 0.93 | 86.3 |
| Base stock +1% example 1 | 0.88 | 87.0 |
| Base stock +1% example 2 | 0.87 | 87.2 |
| Base stock +1.5% example 1 | 0.82 | 87.9 |
| Base stock +1.5% example 2 | 0.81 | 88.1 |
The length of the core is 5cm, and the diameter is 2.5cm.
3. Drilling fluid rheological property and fluid loss test
According to the preparation of the base slurry of the oil-based drilling fluid, according to the standard GB/T16783.2-2012, oil-based drilling fluid, part 2 of field test of oil and gas industry drilling fluid, the oil-based drilling fluid prepared by the high-temperature resistant intercalation modified nano titanium carbide composite plugging agent prepared in the embodiment 1-2 is compared with the base slurry, and the performance test of the oil-based drilling fluid before and after aging is carried out under the same condition, and the results are shown in the table 2 and the table 3. The results shown in table 2 and table 3 show that the oil-based drilling fluid prepared by the high-temperature-resistant intercalation modified nano titanium carbide composite plugging agent prepared in example 1 and example 2 has good rheological property and little change in performance before and after aging, and the oil-based drilling fluid is characterized by higher rock carrying capacity and temperature resistance under lower viscosity. In addition, the API and the high-temperature high-pressure fluid loss are lower, and the demulsification voltage is larger, so that the drilling fluid prepared by the high-temperature intercalation modified nano titanium carbide composite plugging agent synthesized by the invention has better performance.
TABLE 2 Table 2 recording rheological Properties and fluid loss Properties of drilling fluids before aging
TABLE 3 Table of rheological Properties and fluid loss Properties of drilling fluids after aging
AV-apparent viscosity in mPa.s; PV-plastic viscosity in mPa.s; yp—dynamic shear force in Pa; API-normal temperature medium pressure filtration loss, unit is mL; HTHP-high temperature high pressure fluid loss in mL; ES-demulsification voltage in V.
The present invention is not limited to the above-mentioned embodiments, but is intended to be limited to the following embodiments, and any modifications, equivalents and modifications can be made to the above-mentioned embodiments without departing from the scope of the invention.
Claims (7)
1. The high-temperature-resistant intercalation modified nano titanium carbide composite plugging agent is characterized in that the raw materials of the high-temperature-resistant intercalation modified nano titanium carbide composite plugging agent are nano titanium carbide of 50nm, p-dodecyl styrene, cetyl acrylate compounds, vinyl naphthenes compounds, an intercalating agent, a cross-linking agent and an initiator; the preparation method comprises the following steps:
s1, intercalation modified nano titanium carbide: vacuum drying nano titanium carbide at 60-70 ℃, adding the dried nano titanium carbide into a dispersion liquid of deionized water for ultrasonic dispersion, then dropwise adding an intercalation agent while stirring, then reacting at 40-50 ℃, cooling to room temperature, centrifugally separating, performing ultrasonic dispersion, suction filtering and washing to obtain intercalation modified nano titanium carbide;
s2, firstly, performing ultrasonic dispersion on the intercalated modified nano titanium carbide obtained in the step S1 by using deionized water, placing a dispersion liquid in a reactor, introducing nitrogen for 20-30min, adding a comonomer of p-dodecyl styrene, a hexadecyl acrylate compound and a vinyl naphthene compound in the reactor, adjusting the pH value of a system to be between 6.5 and 7.5 by using a 20-25% NaOH aqueous solution, heating to 60-70 ℃, adding a cross-linking agent and an initiator for reacting for 4-5h, cooling to room temperature after the reaction is finished, washing the prepared sample to be neutral by using distilled water, then placing the sample in a condition of 50-60 ℃ for vacuum drying, and grinding the dried sample to obtain the high-temperature-resistant intercalated modified nano titanium carbide composite plugging agent with 90-330 nm;
the molar mass ratio of the intercalation modified nano titanium carbide to the dodecyl styrene, the hexadecyl acrylate compound and the vinyl naphthene compound is 2:2:1:3;
the adding amount of the cross-linking agent is 1% -3% of the total weight of the four monomers, namely intercalation modified nano titanium carbide, p-dodecyl styrene, cetyl acrylate compounds and vinyl naphthenes compounds;
the addition amount of the initiator is 1% -3% of the total weight of the four monomers of intercalation modified nano titanium carbide, dodecyl styrene, hexadecyl acrylate compounds and vinyl naphthene compounds;
the hexadecyl acrylate compound is one of hexadecyl acrylate and hexadecyl methacrylate;
the vinyl cycloalkane compound is one of vinyl cyclopentane, vinyl cyclohexane and vinyl cyclooctane.
2. The high temperature resistant intercalation modified nano titanium carbide composite plugging agent according to claim 1, wherein the intercalation agent is one of tetramethylammonium hydroxide (TMAOH) and dimethyl sulfoxide (DMSO).
3. The high temperature resistant intercalation modified nano titanium carbide composite plugging agent according to claim 1, wherein the cross-linking agent is one of N, N-Methylenebisacrylamide (MBA) and dicyclopentadiene acrylic acid ester (DCPA); the initiator is one of ammonium persulfate and potassium persulfate.
4. An oil-based drilling fluid, which is characterized in that the high-temperature-resistant intercalation modified nano titanium carbide composite plugging agent in accordance with claim 1 is added into the drilling fluid.
5. The oil-based drilling fluid of claim 4, wherein the drilling fluid comprises the following components: base oil, main emulsifier, auxiliary emulsifier, wetting agent, cutting agent, organic soil, filtrate reducer, water phase, calcium oxide, weighting agent and plugging agent.
6. The oil-based drilling fluid according to claim 5, wherein the base oil is 3# white oil, the main emulsifier is TYODF-301, the auxiliary emulsifier is TYODF-401, the wetting agent is TYODF-501, the cutting agent is TYODF-701, the organic soil is TYODF-601, the fluid loss additive is TYODF-101, the aqueous phase is 30% calcium chloride solution, the calcium oxide is TYODF-801, the weighting agent is a barite powder, the plugging agent is the high temperature resistant intercalated modified nano titanium carbide composite plugging agent of claim 1, and the main emulsifier, auxiliary emulsifier, wetting agent, cutting agent, organic soil, fluid loss additive, and calcium oxide are derived from the company of decubitus oil.
7. The oil-based drilling fluid according to claim 6, wherein the composition of the drilling fluid is as follows in parts by weight: 225-227 parts of 3# white oil, 3.6-3.8 parts of main emulsifier TYODF-301, 9.8-10.2 parts of auxiliary emulsifier TYODF-401, 3.2-3.3 parts of wetting agent TYODF-501, 0.7-0.8 part of cutting agent TYODF-701, 7-8 parts of organic soil TYODF-601, 14.5-15.5 parts of filtrate reducer TYODF-101, 24-26 parts of 30% calcium chloride solution, 7.3-7.7 parts of calcium oxide TYODF-801, 1.25-3.75 parts of high temperature-resistant intercalation modified nano titanium carbide composite plugging agent, 250-600 parts of barite powder and 1.5-2.2g/cm of drilling fluid density 3 。
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