CN111234785A - Nano plugging agent for water-based drilling fluid, preparation method of nano plugging agent and water-based drilling fluid - Google Patents
Nano plugging agent for water-based drilling fluid, preparation method of nano plugging agent and water-based drilling fluid Download PDFInfo
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- CN111234785A CN111234785A CN202010195708.2A CN202010195708A CN111234785A CN 111234785 A CN111234785 A CN 111234785A CN 202010195708 A CN202010195708 A CN 202010195708A CN 111234785 A CN111234785 A CN 111234785A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- 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
- C09K8/02—Well-drilling compositions
- C09K8/03—Specific additives for general use in well-drilling compositions
- C09K8/032—Inorganic additives
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- 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
- C09K8/02—Well-drilling compositions
- C09K8/04—Aqueous well-drilling compositions
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- 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
- 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
Abstract
The invention provides a nano plugging agent for water-based drilling fluid, a preparation method thereof and the water-based drilling fluid, wherein the preparation method of the nano plugging agent for the water-based drilling fluid comprises the following steps: heating melamine or urea to 400-550 ℃ at a heating rate of not higher than 5 ℃/min in air or protective atmosphere, preserving heat for not less than 2 hours to obtain carbon nitride, and grinding the carbon nitride to obtain flaky carbon nitride powder; mixing the flaky carbon nitride powder with water or an organic solution according to a mass-volume ratio of 1-5: 1 and the unit is mg/mL, mixing and carrying out ultrasonic dispersion, filtering and drying to obtain the flaky nano plugging agent. The nano plugging agent has the advantages of high hardness, strong rigidity, good chemical stability, good stability in a high-temperature environment in the pit, easy access to micropores and microcracks of a stratum, plugging formation by stacking and the like.
Description
Technical Field
The invention belongs to the technical field of functional nano materials for oil and gas field drilling, and particularly relates to a nano plugging agent for water-based drilling fluid, a preparation method of the nano plugging agent and the water-based drilling fluid.
Background
In recent years, the water-based drilling fluid has the advantages of safety, environmental protection, low cost and the like, and becomes a research hotspot of the shale gas drilling fluid technology. Due to strong bedding property and low permeability of the shale stratum, a large number of micro cracks (the width of the cracks is between 50nm and 40 mu m) exist in the shale stratum, and the micro cracks can generate a strong self-absorption phenomenon after being contacted with fluid, so that the micro cracks are expanded and communicated, the borehole wall instability is caused, and the popularization and application of the water-based drilling fluid in shale gas exploitation are seriously restricted.
The conventional plugging materials are distributed in a micron-scale mode, cannot be effectively matched with the nano-scale microcracks of the shale stratum, and are difficult to realize effective plugging, so that well wall blocks fall off and instability occurs in the drilling process of the shale gas horizontal well. Therefore, the research and development of the nanoscale plugging agent matched with the shale stratum and the effective plugging of the nanoscale cracks are of great significance for keeping the well wall stable and reducing the underground complex accident rate.
Disclosure of Invention
The present invention aims to address at least one of the above-mentioned deficiencies of the prior art. For example, one of the purposes of the invention is to provide a preparation method of a nanoscale plugging agent which can be matched with the fracture of a shale formation.
In order to achieve the above object, one aspect of the present invention provides a method for preparing a nano plugging agent for a water-based drilling fluid. The preparation method comprises the following steps: heating melamine or urea to 400-550 ℃ at a heating rate of not higher than 5 ℃/min in air or protective atmosphere, preserving heat for not less than 2 hours to obtain carbon nitride, and grinding the carbon nitride to obtain flaky carbon nitride powder; and mixing the flaky carbon nitride powder and the organic solution according to a mass-volume ratio of 1-5: 1 and the unit is mg/mL, mixing and carrying out ultrasonic dispersion, filtering and drying to obtain the flaky nano plugging agent.
In an exemplary embodiment of an aspect of the present invention, the nano blocking agent may have a length of 200nm to 2000nm, a width of 200nm to 2000nm, and a thickness of 5nm to 15 nm.
In an exemplary embodiment of an aspect of the present invention, the nano blocking agent may have a length of 900nm to 1500nm, a width of 900nm to 1500nm, and a thickness of 8 nm to 12 nm.
In one exemplary embodiment of an aspect of the present invention, the protective atmosphere may be argon or helium.
In one exemplary embodiment of an aspect of the present invention, the organic solution may be an ethanol or acetone solution.
In an exemplary embodiment of an aspect of the present invention, the ultrasonic intensity may be 30 to 40 KHz.
The invention also provides a nano plugging agent. The nano plugging agent can be prepared by the preparation method.
Another object of the present invention is to provide a water-based drilling fluid suitable for drilling in micro-fractured formations.
In another aspect of the invention, a water-based drilling fluid is provided. The water-based drilling fluid can comprise the nano plugging agent prepared by the preparation method.
In an exemplary embodiment of another aspect of the present invention, the volume-to-mass ratio of the drilling fluid to the nano plugging agent may be 1: 5 to 30 and the unit is L/g.
Compared with the prior art, the beneficial effects of the invention can comprise at least one of the following:
(1) the nano plugging agent has high hardness, strong rigidity and good chemical stability, and can keep good stability in a high-temperature environment in a well;
(2) the nano plugging agent prepared by the method is in a sheet shape, is easier to enter micropores and microcracks of a stratum, and forms plugging by stacking;
(3) the preparation method of the nano plugging agent provided by the invention is simple and feasible, is easy to realize large-scale production, and has rich raw material sources and lower cost.
Drawings
Fig. 1 shows a scanning electron microscope image of a nano plugging agent prepared by a preparation method according to an exemplary embodiment of the invention;
fig. 2 shows an atomic force microscope image of a nano plugging agent prepared according to a preparation method of an exemplary embodiment of the present invention.
Detailed Description
Hereinafter, the nano plugging agent for water-based drilling fluid and the preparation method thereof and the water-based drilling fluid of the present invention will be described in detail with reference to the accompanying drawings and exemplary embodiments.
In one exemplary embodiment of the invention, the preparation method of the nano plugging agent for the water-based drilling fluid comprises the following steps: heating melamine or urea to 400-550 ℃ at a heating rate of not higher than 5 ℃/min in air or protective atmosphere, preserving heat for not less than 2h to obtain carbon nitride, and grinding the carbon nitride to obtain flaky carbon nitride powder. Specifically, raw materials for preparing carbon nitride from melamine or urea and the like are added into an alumina crucible, the alumina crucible is covered with a cover and put into a muffle furnace to be heated at a heating rate of not higher than 5 ℃/min under the air atmosphere or protective atmosphere, and when the temperature reaches 400-500 ℃, the heating is stopped and the current temperature is kept for not less than 2 hours, so that the required carbon nitride material (such as powder or solid particles) is prepared. The protective atmosphere may be argon or helium. The resulting carbon nitride material was cooled to room temperature and ground into flaky carbon nitride powder. However, the present invention is not limited thereto, and other means such as a tube-type resistance furnace may be used for heating.
In the embodiment, the mass volume ratio of the flaky carbon nitride powder to water or organic solution is 1-5: 1 and the unit is mg/mL, mixing and carrying out ultrasonic dispersion, filtering and drying to obtain the flaky nano plugging agent. Specifically, the ground flaky carbon nitride powder and water or an organic solvent are added into a beaker according to the mass-volume ratio of 1-5: 1 (for example, 3:1) and the unit of mg/mL to be mixed to obtain a mixed solution, then the carbon nitride powder in the mixed solution is completely dispersed by ultrasonic, and the flaky nano plugging agent is obtained by filtering and drying. Here, the water may be deionized water, and the organic solution may be an ethanol or acetone solution. The ultrasonic intensity can be 30-40 KHz. However, the present invention is not limited thereto, and other dispersion methods are also possible.
Fig. 1 shows a scanning electron microscope image of a nano plugging agent prepared by a preparation method according to an exemplary embodiment of the invention. Fig. 2 shows an atomic force microscope image of the nano-blocking agent prepared by the preparation method according to an exemplary embodiment of the present invention.
In the present exemplary embodiment, the nano blocking agent may have a length of 200nm to 2000nm, a width of 200nm to 2000nm, and a thickness of 5nm to 15 nm. Further, the length of the nano plugging agent can be 900 nm-1500 nm, the width can be 900 nm-1500 nm, and the thickness can be 8-12 nm. Specifically, the prepared nano plugging agent is in a sheet or sheet-like structure, so that the nano plugging agent can enter micro pores and micro cracks of a stratum more easily, and is retained and stacked in irregular cracks to form effective plugging. As shown in FIG. 1 and FIG. 2, it can be seen from FIG. 1 that the prepared nano plugging agent is in the form of a sheet, and the length and width of the nano plugging agent are between 200nm and 2000 nm. As can be seen from FIG. 2, the thickness of the nano blocking agent is about 10 nm. Wherein the microscope model is H-800, the accelerating voltage is 175KV, the magnification is 50000, and the camera length is 800 mm.
In order to better understand the above exemplary embodiments of the present invention, they are further described below with reference to specific examples.
Example 1
20g of melamine were added to an alumina crucible and the lid was closed. And (3) putting the crucible into a muffle furnace, heating at the speed of 2 ℃/min in the air atmosphere, stopping heating after the temperature reaches 500 ℃, and preserving heat for 3h to obtain the carbon nitride material. After cooling to room temperature, the prepared carbon nitride material is ground into flaky carbon nitride powder.
Adding ground carbon nitride powder into a 500mL beaker, mixing with 300mL deionized water, ultrasonically dispersing for 10h, filtering and drying to obtain flaky nano carbon nitride powder, namely 9.62g of nano plugging agent, and characterizing the nano plugging agent by a scanning electron microscope, wherein the length of the nano plugging agent is 900-1300 nm, the width of the nano plugging agent is 900-1300 nm, and the thickness of the nano plugging agent is 8-12 nm.
Example two
Example 2
20g of urea was added to the alumina crucible and the lid was closed. And (3) putting the crucible into a muffle furnace, heating at the speed of 2 ℃/min in the air atmosphere, stopping heating after the temperature reaches 500 ℃, and preserving the heat for 4h to obtain the carbon nitride material. After cooling to room temperature, the prepared carbon nitride material was ground into flaky carbon nitride powder.
Adding ground carbon nitride powder into a 500mL beaker, mixing with 300mL of ethanol solution, ultrasonically dispersing for 10h, filtering and drying to obtain flaky nano carbon nitride powder, namely 1.87g of nano plugging agent, and characterizing the nano plugging agent by a scanning electron microscope, wherein the length of the nano plugging agent is 1000-1500 nm, the width of the nano plugging agent is 1000-1500 nm, and the thickness of the nano plugging agent is 8-12 nm.
In order to evaluate the plugging effect of the nano plugging agent with different addition amounts, table 1 shows the plugging performance of the nano plugging agent and the polymer nano microsphere plugging agent prepared in examples 1 and 2 in the drilling fluid, which are evaluated by adopting a filter cake permeability experiment.
First, a mud cake is prepared.
Slowly adding 3.0g of filtrate reducer Redu-1 into 200mL of bentonite slurry with the concentration of 4%, continuously stirring at a high speed for 20min, adding 1.0g of PAC-LV, then stirring at a high speed for 20min, then adding 4.0g of sulfonated asphalt soltex, then stirring at a high speed for 10min, then adding 200g of API barite and 25g of calcium carbonate with 1250 meshes while stirring at a high speed, then stirring at a high speed for 30min, adding a high-temperature high-pressure water loss instrument, losing water for 30min under the conditions of normal temperature and 3.5MPa, and pouring out the drilling fluid in the high-temperature high-pressure water loss instrument to obtain a mud cake.
The blocking agent was then tested for blocking performance.
The prepared mud cake is used as a filter medium, clear water, nano plugging agents (example one and example two) with different addition amounts and aqueous solution of the polymer nano microsphere plugging agent are added into a high-temperature high-pressure water loss instrument, and the filtration loss is measured for 30min at normal temperature. After the determination is finished, pouring out the liquid, taking out the mud cakes, determining the filtration loss for 60min at normal temperature by using clear water, and calculating the permeability of the mud cakes in each experimental group. Tests were conducted for different additive concentrations of each blocking agent, and the results are shown in table 1. The plugging performance of the plugging agent, namely the calculation formula of the filter cake permeability, is as follows:
wherein: k-cake permeability, mD; vf-fluid loss, mL; mu-viscosity of the filtrate, mPas-1(ii) a h-filter cake thickness, mm; a-area of filter cake, cm2(ii) a Delta P-osmotic pressure difference, kg-cm-2(ii) a t-time, s. And (3) related parameters: a22.90 cm2;μ=0.89mPa·s-1(25℃);ΔP=35kg·cm-2;t=3600 s。
TABLE 1 influence of different addition amounts of nano-plugging agent on mud cake permeability
Wherein 0.0 percent of clear water without the addition of the plugging agent, and 0.5 to 2 percent of the clear water represents that 0.5 to 2g of the plugging agent is added into 100g of water.
As can be seen from table 1, as the addition amounts of the nano plugging agent and the polymer nano microsphere plugging agent of the first example and the second example increase (from 0.0% to 2.0%), the permeability of the mud cake decreases gradually, and the permeability of the mud cake with the nano plugging agent of the first example and the second example is lower than that of the mud cake with the polymer nano microsphere plugging agent at the same addition amount (for example, 2.0%).
In another aspect of the invention, a nano plugging agent is provided. The nano plugging agent can be prepared by adopting the preparation method of the nano plugging agent for the water-based drilling fluid as described in each example above.
In yet another aspect of the present invention, a water-based drilling fluid is provided. The water-based drilling fluid can comprise the nano plugging agent prepared by the preparation method. For example, the volume-to-mass ratio of the drilling fluid to the nano plugging agent may be 1: 5 to 30 and the unit is L/kg. Namely, 5-30 g of nano plugging agent is added into each liter of drilling fluid.
In summary, the beneficial effects of the invention can include at least one of the following:
(1) the nano plugging agent has high hardness, strong rigidity and good chemical stability, and can keep good stability in a high-temperature environment in a well;
(2) the nano plugging agent is in a nano-scale sheet shape, the length and the width of the nano plugging agent are between 200nm and 2000nm, the thickness of the nano plugging agent is between 5nm and 15nm, and the larger length and width dimension is matched with the stronger rigidity of carbon nitride, so that plugging materials are easier to be retained in irregular cracks and stacked to form plugging after entering the cracks;
(4) the preparation method of the nano plugging agent provided by the invention is simple and feasible, is easy to realize large-scale production, and has rich raw material sources and lower cost.
Although the present invention has been described above in connection with the exemplary embodiments and the accompanying drawings, it will be apparent to those of ordinary skill in the art that various modifications may be made to the above-described embodiments without departing from the spirit and scope of the claims.
Claims (9)
1. The preparation method of the nano plugging agent for the water-based drilling fluid is characterized by comprising the following steps of:
heating melamine or urea to 400-550 ℃ at a heating rate of not higher than 5 ℃/min in air or protective atmosphere, preserving heat for not less than 2 hours to obtain carbon nitride, and grinding the carbon nitride to obtain flaky carbon nitride powder;
mixing the flaky carbon nitride powder with water or an organic solution according to a mass-volume ratio of 1-5: 1 and the unit is mg/mL, mixing and carrying out ultrasonic dispersion, filtering and drying to obtain the flaky nano plugging agent.
2. The preparation method of the nano plugging agent for the water-based drilling fluid, according to claim 1, is characterized in that the length of the nano plugging agent is 200nm to 2000nm, the width of the nano plugging agent is 200nm to 2000nm, and the thickness of the nano plugging agent is 5nm to 15 nm.
3. The preparation method of the nano plugging agent for the water-based drilling fluid, according to claim 1, is characterized in that the length of the nano plugging agent is 900nm to 1500nm, the width of the nano plugging agent is 900nm to 1500nm, and the thickness of the nano plugging agent is 8 nm to 12 nm.
4. The method for preparing the nano plugging agent for the water-based drilling fluid according to claim 1, wherein the protective atmosphere is argon or helium.
5. The preparation method of the nano plugging agent for the water-based drilling fluid, according to claim 1, wherein the organic solution is ethanol or acetone solution.
6. The preparation method of the nano plugging agent for the water-based drilling fluid, according to claim 1, is characterized in that the ultrasonic intensity is 30-40 KHz.
7. The nano plugging agent for the water-based drilling fluid is characterized by being prepared by the preparation method of any one of claims 1 to 6.
8. A water-based drilling fluid, which is characterized by comprising the nano plugging agent prepared by the preparation method of any one of claims 1 to 6.
9. The water-based drilling fluid according to claim 8, wherein the volume mass ratio of the drilling fluid to the nano plugging agent is 1: 5 to 30 and the unit is L/g.
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US20150176363A1 (en) * | 2013-12-24 | 2015-06-25 | Baker Hughes Incorporated | Swellable downhole structures including carbon nitride materials, and methods of forming and using such structures |
CN104401948A (en) * | 2014-11-17 | 2015-03-11 | 长安大学 | Preparation method for single-layer graphite-type carbon nitride nanosheet solution |
CN106634890A (en) * | 2016-12-18 | 2017-05-10 | 西南石油大学 | Boron-nitride-nanosheet-modified water-base drilling fluid |
CN109810678A (en) * | 2017-11-20 | 2019-05-28 | 中石化石油工程技术服务有限公司 | Mud shale stratum sealing agent and preparation method of the drilling fluid based on nanofiber composite |
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